[go: up one dir, main page]

WO2017176085A1 - Aluminum precursor synthesization system and aluminum precursor preparation method using same - Google Patents

Aluminum precursor synthesization system and aluminum precursor preparation method using same Download PDF

Info

Publication number
WO2017176085A1
WO2017176085A1 PCT/KR2017/003812 KR2017003812W WO2017176085A1 WO 2017176085 A1 WO2017176085 A1 WO 2017176085A1 KR 2017003812 W KR2017003812 W KR 2017003812W WO 2017176085 A1 WO2017176085 A1 WO 2017176085A1
Authority
WO
WIPO (PCT)
Prior art keywords
reactor
inert gas
aluminum precursor
pressure
product
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/KR2017/003812
Other languages
French (fr)
Korean (ko)
Inventor
이혜문
정수호
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Korea Institute of Machinery and Materials KIMM
Original Assignee
Korea Institute of Machinery and Materials KIMM
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Korea Institute of Machinery and Materials KIMM filed Critical Korea Institute of Machinery and Materials KIMM
Priority to KR1020187032171A priority Critical patent/KR20180125601A/en
Publication of WO2017176085A1 publication Critical patent/WO2017176085A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/001—Controlling catalytic processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
    • C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
    • C07F5/06—Aluminium compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
    • C07F5/06—Aluminium compounds
    • C07F5/069—Aluminium compounds without C-aluminium linkages

Definitions

  • the present invention relates to an aluminum precursor synthesis system and a method for manufacturing an aluminum precursor using the same, and more particularly, a pressure control unit connected to an associated reactor for preparing an aluminum precursor, and the like to control the pressure of the internal reactor.
  • a pressure control unit connected to an associated reactor for preparing an aluminum precursor, and the like to control the pressure of the internal reactor.
  • Aluminum has a specific resistance of about 2.65 u ⁇ / cm, which is the fourth most conductive after silver, copper, and gold, and has a low work function. It is an environmental-energy that requires ohmic contact such as solar cells and OLEDs. It can be utilized as a cathode material of the device.
  • aluminum has such a high oxidation characteristic that it is impossible to manufacture metal ink such as gold or silver, so that where an aluminum thin film is needed as an electrode or wiring, it is not a simple wet process through ink, but a vacuum thermal evaporation method, Relatively complex processes such as sputter coating and vacuum deposition processes have been used, with high loss of raw materials.
  • an aluminum precursor ink was developed, and a process of manufacturing an aluminum film through a simple wet process in a low temperature atmosphere of 150 ° C. or lower has been developed. There was a difficulty in manufacturing.
  • the present inventors have developed an aluminum precursor ink in the form of an organo-metal and a method of manufacturing an aluminum electrode using the same, but this is also a raw material for producing an aluminum precursor ink in the form of an organo-metal. Materials and solvents were difficult to handle, requiring a new manufacturing system capable of mass production efficiently and safely.
  • Another object of the present invention is to provide a method for producing an aluminum precursor using the aluminum precursor synthesis system according to the present invention.
  • the present invention to solve the above problems
  • a raw material supply unit supplying a raw material into the reactor
  • a reaction solvent supply unit supplying a reaction solvent into the reactor
  • An inert gas supply unit supplying an inert gas to the reactor and the reaction solvent supply unit;
  • a pressure control unit connected to the reactor and the product storage unit to control pressure; It supplies an aluminum precursor synthesis system comprising a.
  • the raw material supply unit In the aluminum precursor synthesis system according to the invention, the raw material supply unit, the sealed housing; One or a plurality of raw material storage units accommodated in the housing and storing raw materials; And a raw material supply line connecting the raw material storage unit and the reactor and supplying the raw material to the reactor.
  • the reaction solvent supply unit a reaction solvent storage unit for receiving the reaction solvent; It consists of; a reaction solvent supply line for supplying the reaction solvent to the reactor.
  • the reaction solvent supply is because the inert gas is injected into the reaction solvent reservoir to supply the reaction solvent to the reactor at the pressure of the inert gas, the reaction solvent supply line is the reaction The terminal is connected in the solvent reservoir in a state immersed in the reaction solvent.
  • the inert gas supply unit In the aluminum precursor synthesis system according to the present invention, the inert gas supply unit, the inert gas storage unit; A first inert gas supply line connecting the inert gas storage unit and the reaction solvent storage unit to supply the inert gas to the reaction solvent storage unit; And a second inert gas supply line connecting the inert gas storage unit and the reactor to supply the inert gas to the reactor. And a third inert gas supply line connecting the inert gas storage unit and the source material supply unit to supply the inert gas to the source material supply unit.
  • the end of the first inert gas supply line is connected without contact with the reaction solvent contained in the reaction solvent reservoir, and the end of the second inert gas supply line is in the reactor. It is connected without contacting the reactants, characterized in that the third inert gas supply line end is connected to the raw material in a non-contact state in the raw material supply.
  • the product storage unit In the aluminum precursor synthesis system according to the invention, the product storage unit, the product storage chamber for receiving the product flowing out of the reactor; A first product discharge line connecting between said product storage chamber and said reactor; Characterized in that consists of.
  • the first product outlet line is connected to the bottom of the reactor, or is withdrawn from the top of the reactor, characterized in that the end is precipitated in the product inside the reactor.
  • the pressure control unit the pressure control chamber for receiving a medium for pressure control and exposure to the outside environment;
  • a vacuum pump A first pressure regulation line connecting the pressure regulation chamber and the vacuum pump;
  • a second pressure regulating line connecting between the product storage chamber and the pressure control unit to regulate pressure in the product storage chamber;
  • a third pressure regulating line connected between the reactor and the pressure controller to regulate pressure in the reactor. Characterized in that it comprises a.
  • one end of the second pressure regulation line is connected to the submerged state in the medium for the pressure regulation
  • the end of the third pressure regulation line is the medium for the pressure regulation It is characterized in that connected in the state immersed in.
  • the pressure control medium is characterized in that the silicone oil.
  • the second pressure regulating line and the third pressure regulating line are connected by a three-way valve to operate integrally.
  • the reactor includes a heating unit; A pressure measuring unit (not shown) for measuring the pressure inside the reactor; And a pH measuring unit (not shown) for measuring the pH of the reactant.
  • Aluminum precursor synthesis system the reactor; A raw material supply unit supplying a raw material into the reactor; A reaction solvent supply unit supplying a reaction solvent into the reactor; An inert gas supply unit supplying an inert gas to the reactor and the reaction solvent supply unit; A product storage unit in which the product generated from the reactor is discharged and stored; And a pressure control unit connected to the reactor and the product storage unit to control the pressure.
  • the present invention also provides
  • Transferring the product to a product reservoir It provides an aluminum precursor manufacturing method using an aluminum precursor synthesis system according to the present invention comprising a.
  • the inert gas in the injecting the inert gas into the reactor, the inert gas to the second inert gas supply line by inducing a reduced pressure in the reactor by the pressure control unit and the third pressure control line. Is injected into the reactor, and the inert gas injected into the reactor moves to the product reservoir and the pressure controller.
  • the present invention also includes the step of injecting the inert gas into the reactor, the reactor, the first product discharge line connecting the reactor and the product reservoir, and the second pressure control line connecting the product reservoir and the pressure control chamber, And controlling the first pressure control line connected to the vacuum pump through an opening / closing means that can be controlled by those skilled in the art such as a valve, thereby inducing a reduced pressure in the reactor and continuously injecting an inert gas into the reactor according to the pressure difference. do.
  • the step of injecting the inert gas into the reactor thereby controls the atmosphere inside the reaction system to the inert gas, and includes the meaning of removing impurities in the reactor before inducing the present reaction.
  • the inert gas in the injecting the inert gas into the reactor, the inert gas is injected by inducing a reduced pressure in the reactor, but the method of inducing the reduced pressure in the reactor is not particularly limited.
  • inert gas is injected into the reaction solvent storage through the first inert gas supply line, by the air pressure of the injected inert gas
  • the reaction solvent is characterized in that the injection into the reactor.
  • the third pressure control line connecting the reactor and the pressure control chamber, and the first pressure control connected to the pressure control chamber
  • the opening and closing means that can be adjusted by other persons skilled in the art, such as a valve through the line, induces a reduced pressure in the reactor to supply an inert gas to the raw material supply unit through the third inert gas supply line according to the pressure difference It characterized in that the injection into the reactor.
  • a solvent supply unit, a raw material supply unit, etc. are integrally connected to the reactor, and by adjusting the pressure difference in the system using the pressure control unit, raw materials, which have been difficult to handle in the past, The reaction solvent and the like can be systematically supplied, and as a result, mass production of the aluminum precursor ink in the form of an organic metal is possible.
  • 1 to 8 show an aluminum precursor synthesis system according to an embodiment of the present invention.
  • FIG. 1 shows an aluminum precursor synthesis system according to the present invention.
  • the aluminum precursor synthesis system comprises a reactor (100); A raw material supply unit 200 for supplying a raw material into the reactor; A reaction solvent supply unit 300 supplying a reaction solvent into the reactor; An inert gas supply unit 400 supplying an inert gas to the reactor and the reaction solvent supply unit; A product storage part 500 in which the product generated from the reactor is leaked out and stored; And a pressure control unit 600 connected to the reactor and the product storage unit to control pressure. It includes.
  • the reactor 100 the heating unit 110; A pressure measuring unit (not shown) for measuring the pressure inside the reactor; And a pH measurement unit (not shown) for measuring the pH of the reactant.
  • the heating unit 110 for maintaining the temperature inside the reactor at a constant temperature is a heat transfer medium heated in a separate heating unit as shown in FIGS. It is possible to circulate around the reactor, a direct heating method such as a heating mantle, and others can freely choose.
  • the reactor is not particularly limited as long as it is a reactor used in organic synthesis.
  • the aluminum precursor synthesis system according to the present invention induces a reduced pressure inside the reactor by the pressure control unit 600 connected to the reactor, it is preferable to include a pressure measuring unit for measuring the pressure inside the reactor.
  • the raw material supply unit 200 the sealed housing 210; One or a plurality of raw material storage units 220, 230, and 240 accommodated in the housing and storing raw materials for synthesizing an aluminum precursor; And a raw material supply line (L2) connecting the raw material storage unit and the reactor to supply the raw material to the reactor. It includes.
  • the method of controlling the input amount of the raw material is a method for detecting the change in volume by the input amount of the raw material in the beaker or the mass cylinder and the mass according to the input material input by using a load cell such as a scale Raw material inputs can be controlled by detecting changes.
  • the reaction solvent supply unit 300 a reaction solvent storage unit 310 for receiving a reaction solvent;
  • a reaction solvent supply line (L3) for supplying the reaction solvent to the reactor; It consists of.
  • the aluminum precursor produced by the aluminum precursor synthesis system according to the present invention includes all possible aluminum precursors apparent to those skilled in the art, and is not limited to the embodiments of the present invention.
  • the aluminum precursor synthesized by the aluminum precursor synthesis system according to the present invention comprises substituted and / or unsubstituted aluminum hydride compounds.
  • the aluminum metal precursor comprises AlH 3 .
  • the aluminum metal precursor may comprise one or more organic side chains (eg, alkyl-substituted aluminum hydrides such as isobutylaluminum hydride, dimethylaluminum hydride, etc.) and / or trialkyl aluminum species (eg, Aluminum hydride substituted with triisobutyl aluminum).
  • the aluminum metal precursor may further include one or more ligands that complex with substituted and / or unsubstituted aluminum hydride. More specifically, the aluminum precursor may comprise one or two ligands selected from amines, phosphines, ethers and / or other suitable (donor-type) ligands.
  • aluminum hydride as the aluminum precursor may be prepared by a reaction of lithium aluminum hydride (LiAlH 4 ) and AlCl 3 in an ether solvent, and thus the raw material may be lithium aluminum hydride (LiAlH 4). ) And AlCl 3 , and the reaction solvent may include ether.
  • Ether solvent as the reaction solvent may include one or more aliphatic ethers, examples of which are diethyl ether, di-n-propyl ether, di-n-butyl ether, di-isopropyl ether, di-t-butyl ether , Methyl-butyl ether, n-propyl-n-butyl ether, methyl-t-butyl ether, ethyl-t-butyl ether, or mixtures thereof.
  • the raw material may include one or more additives (eg, surfactants, adhesion promoters and / or catalysts) included in the aluminum precursor composition.
  • additives eg, surfactants, adhesion promoters and / or catalysts
  • the reaction solvent is dibutyl sulfide. It may include.
  • the reaction solvent is di Ethyl sulfide may be included.
  • the inert gas supply unit 400 an inert gas storage unit 410 for storing an inert gas to be a raw material;
  • a first inert gas supply line (L4-1) connecting the inert gas storage unit and the reaction solvent storage unit 300 to supply the inert gas to the reaction solvent storage unit;
  • a second inert gas supply line (L4-2) connecting the inert gas storage unit and the reactor (100) to supply the inert gas to the reactor.
  • a third inert gas supply line L4-3 which connects the inert gas storage unit and the source material supply unit to supply the inert gas to the source material supply unit.
  • the terminal contacting the reaction solvent storage of the first inert gas supply line (L4-1) is not in contact with the reaction solvent contained in the reaction solvent storage 310 Connected to the reactor, and the end of the second inert gas supply line (L4-2) contacting the reactor is not in contact with the reactants in the reactor, and the raw material supply part of the third inert gas supply line (L4-3)
  • the contact end is characterized in that connected to the raw material in a state not in contact with the raw material supply.
  • the reaction solvent is pushed into the reactor at a pressure of the inert gas in the reaction solvent reservoir. It is characterized in that the feed into the reactor.
  • the end of the first inert gas supply line (L4-1) is connected without contact with the reaction solvent contained in the reaction solvent storage 310, the reaction solvent of the reaction solvent supply line (L3) It is characterized in that the terminals are connected in a reservoir so as to be immersed in the reaction solvent.
  • the product storage unit 500 In the aluminum precursor synthesis system according to the present invention, the product storage unit 500, the product storage chamber for receiving the product flowing out of the reactor (510); A first product discharge line (L5) connecting between said product storage chamber and said reactor; Characterized in that consists of.
  • the product storage chamber 510 may be manufactured in a cartridge type and installed in a detachable state from the aluminum precursor synthesis system according to the present invention.
  • the product reservoir 500 in the aluminum precursor synthesis system according to the present invention, can be arranged in a reactor without a separate chamber, or may be disposed in a separate chamber (not shown). Do.
  • the pressure control unit 600 includes a pressure control chamber 610 for receiving a medium for controlling pressure in the reaction system and blocking direct contact of reactants and products with the external environment; Vacuum pump 620; A first pressure regulating line (L6-1) connecting the pressure regulating chamber and the vacuum pump; A second pressure regulating line (L6-2) connected between the product storage chamber and the pressure controller to regulate the pressure in the product storage chamber; And a third pressure regulating line (L6-3) connected between the reactor and the pressure controller to adjust the pressure in the reactor. Characterized in that it comprises a.
  • the aluminum precursor synthesis system does not include a separate driving means, and includes a pressure control unit 600 connected to the reactor 100 and the product storage unit 500, and the product storage chamber ( 500) and the raw material supply unit 200 by controlling the pressure to move the reactants, reaction solvents, raw materials difficult to handle due to the pressure difference, and also serves as a buffer to accommodate the product generated when it is leaked to the outside Done.
  • a pressure control unit 600 connected to the reactor 100 and the product storage unit 500, and the product storage chamber ( 500) and the raw material supply unit 200 by controlling the pressure to move the reactants, reaction solvents, raw materials difficult to handle due to the pressure difference, and also serves as a buffer to accommodate the product generated when it is leaked to the outside Done.
  • one end of the second pressure control line (L6-2) is connected in a state immersed in the medium for the pressure control
  • the third pressure control line (L6-3) ) End is connected to the state immersed in the pressure control medium
  • the vacuum pump 620 is first induced a pressure reduction inside the pressure control chamber, and then induces a pressure reduction inside the reactor connected to the pressure control chamber So that even if the reactant in the reactor or the reactant in the product storage chamber overflows, it is collected into the medium for pressure regulation once contained in the pressure control chamber.
  • the pressure control medium contained in the pressure control chamber may be freely selected by those skilled in the art from non-aqueous solutions such as alkane series, aromatic series, ether series, oil series, and the like. Is preferably a silicone oil.
  • FIG. 2 shows an aluminum precursor synthesis system according to another embodiment of the present invention.
  • the second pressure regulating line L6-2 and the third pressure regulating line L6-3 are connected to each other by a three-way valve to operate integrally.
  • the aluminum precursor synthesis system according to the present invention is connected to the reactor and the product reservoir, and includes a filter 700 including a filter 710 for filtering a product generated from the reactor. It may further include.
  • the filtering unit is to filter the raw material and precipitate remaining in the product generated and transported in the reactor.
  • the filtering unit is to filter the raw material and precipitate remaining in the product generated and transported in the reactor.
  • AlCl 3 and LiAlH 4 as a raw material with dibutyl sulfide as a solvent
  • LiCl is generated in addition to the aluminum precursor, and the by-products generated outside the product are filtered by the filter 710, Only the aluminum precursor is stored in the product reservoir.
  • the filter used in the filtering unit may be made of a material that does not react with the aluminum precursor, more specifically, a cellulose-based filter, polyester, poly Polymer-based filters such as propylene and polystyrene can be used.
  • the aluminum precursor synthesis system according to the present invention includes a second product discharge line L7-1 connecting the reactor 100 and the filter 710; And a third product discharge line L7-2 connecting the filter 710 and the product reservoir. It characterized in that it further comprises.
  • the end of the third product discharge line (L7-2) is connected in the state immersed in the pressure regulator.
  • the second pressure regulating line (L6-2) and the third pressure regulating line (L6-3) is connected by a three-way valve to operate integrally Characterized in that.
  • 5 to 8 show an aluminum precursor synthesis system according to another embodiment of the present invention.
  • a first product discharge line L5 connecting between the reactor 100 and the product storage chamber 500 may be drawn out to the top of the reactor 100.
  • the second product discharge line L7-1 ′ connecting between the reactor 100 and the filtering unit 700 is drawn out to the top of the reactor 100, The end of the second product discharge line L7-1 'can be immersed in the product inside the reactor.
  • the aluminum precursor synthesis system is the reactor; A raw material supply unit supplying a raw material into the reactor; A reaction solvent supply unit supplying a reaction solvent into the reactor; An inert gas supply unit supplying an inert gas to the reactor and the reaction solvent supply unit; A product storage unit in which the product generated from the reactor is discharged and stored; It is possible to further include a housing (800) containing both; and a pressure control unit connected to the reactor and the product reservoir to control the pressure.
  • Transferring the product to a product reservoir includes.
  • a pressure in the reactor 100 may be induced by the pump 620 and the first pressure regulating line L6-1.
  • the inert gas stored in the inert gas storage unit 410 is supplied to the reaction solvent storage unit 300 through the first inert gas supply line L4-1, and the supplied inert
  • the reaction solvent is supplied into the reactor 100 through the reaction solvent supply line L3 by the pressure of the gas.
  • a pressure in the reactor 100 may be induced by the pump 620 and the first pressure regulating line L6-1.
  • the third pressure control line (L6-3) and the vacuum pump 620, the first pressure control line connecting between the pressure control chamber 610 and the reactor 100 to supply the raw material by inducing a reduced pressure inside the reactor (L6-1) may induce a reduced pressure in the reactor (100).
  • the inert gas may be injected into the raw material storage unit 200 through the third inert gas supply line L4-3 to supply the raw material by pushing the raw material into the reactor 100.
  • the reaction solvent and raw materials sequentially introduced into the reactor by induction of the reduced pressure in the reactor are stirred while controlling the temperature and pH in the reactor to produce a product, and the resulting product is a first product discharge line (L5).
  • the pressure control chamber 610 a vacuum pump for receiving a medium for pressure regulation in order to induce a reduced pressure in the product storage unit 500 to be smoothly stored in the product storage unit 510 by the pressure difference ( 620, the first pressure regulating line L6-1 and the second pressure regulating line L6-2 may induce a reduced pressure in the product reservoir 500.
  • the filter unit 700 further includes the product generated from the reactor 100 is introduced into the filter unit 700 through the second product discharge line L7-1 and then filtered by the filter. It is moved to the product storage unit 500 through the third product discharge line (L7-2).
  • control line L6-2 may induce reduced pressure in product reservoir 500.
  • the second pressure regulating line L6-2 and the third pressure regulating line L6-3 may be connected and used by a three-way valve.
  • the aluminum precursor synthesis system according to the present invention may further include a separate control means (not shown) for integrally controlling the opening and closing of the valve according to such sequential step adjustment and step performance.
  • a separate control means (not shown) for integrally controlling the opening and closing of the valve according to such sequential step adjustment and step performance. Can be.
  • a solvent supply unit, a raw material supply unit, etc. are integrally connected to the reactor, and by adjusting the pressure difference in the system using the pressure control unit, raw materials, which have been difficult to handle in the past, The reaction solvent and the like can be systematically supplied, and as a result, mass production of the aluminum precursor ink in the form of an organic metal is possible.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)

Abstract

The present invention relates to an aluminum precursor synthesization system and an aluminum precursor preparation method using the same and, more specifically, to a novel aluminum precursor synthesization system and an aluminum precursor preparation method using the same, the system enabling a solvent supply part, a raw material supply part and the like to be integrally connected to a reactor and a difference in the internal pressure of the system to be regulated by using a pressure control part, and thus raw materials, a reaction solvent, and the like, which were conventionally difficult to handle, can be systematically supplied, thereby resultantly enabling the production of an organo-metal aluminum precursor ink.

Description

알루미늄 전구체 합성 시스템 및 이를 이용한 알루미늄 전구체 제조방법Aluminum precursor synthesis system and manufacturing method of aluminum precursor using the same

본 발명은 알루미늄 전구체 합성 시스템 및 이를 이용한 알루미늄 전구체 제조방법에 관한 것으로서, 더욱 상세하게는 알루미늄 전구체 제조를 위한 관련 반응기 등이 일체적으로 연결되고, 내부 반응기의 압력을 조절하기 위하여 연결되는 압력 제어부를 포함하여, 시스템 반응기 내부 압력 차이를 유도하여 별도의 구동 수단 없이 취급이 어려운 원료물질, 반응 용매 등을 반응기로 공급하여 반응을 수행하는 것이 가능하게 된 새로운 알루미늄 전구체 합성 시스템 및 이를 이용한 알루미늄 전구체 제조방법에 관한 것이다. The present invention relates to an aluminum precursor synthesis system and a method for manufacturing an aluminum precursor using the same, and more particularly, a pressure control unit connected to an associated reactor for preparing an aluminum precursor, and the like to control the pressure of the internal reactor. Including a new aluminum precursor synthesis system and a method for manufacturing an aluminum precursor using the same, which makes it possible to induce a pressure difference inside the system reactor to supply a raw material, a reaction solvent, and the like, which are difficult to handle without a separate driving means, to perform the reaction. It is about.

알루미늄은 약 2.65 uΩ/cm의 비저항을 지니고 있어 은, 구리, 금에 이어 4번째로 전기전도성이 좋으며 일함수 또한, 낮은 금속으로 태양전지 및 OLED 등 오믹접촉(ohmic contact)을 요구하는 환경-에너지 소자의 음극(cathode) 소재로 활용될 수 있다. Aluminum has a specific resistance of about 2.65 uΩ / cm, which is the fourth most conductive after silver, copper, and gold, and has a low work function. It is an environmental-energy that requires ohmic contact such as solar cells and OLEDs. It can be utilized as a cathode material of the device.

그러나, 알루미늄은 이와 같이 산화특성이 매우 높아 금 또는 은과 같이 금속잉크 제조가 불가능하여, 알루미늄 박막을 전극 또는 배선으로 필요로 하는 곳에는 잉크를 통한 간단한 습식공정이 아니라 진공상태의 열 증발법, 스퍼터(sputter) 코팅과 진공증착 공정 등의 비교적 복잡하고 원료소재의 손실이 큰 공정이 활용되어 왔다. However, aluminum has such a high oxidation characteristic that it is impossible to manufacture metal ink such as gold or silver, so that where an aluminum thin film is needed as an electrode or wiring, it is not a simple wet process through ink, but a vacuum thermal evaporation method, Relatively complex processes such as sputter coating and vacuum deposition processes have been used, with high loss of raw materials.

이러한 종래 알루미늄 잉크 제조 공정의 문제점을 해결하기 위해 알루미늄 전구체 잉크가 개발되어 150℃ 이하의 저온 분위기에서 간단한 습식공정을 통해 알루미늄 필름을 제조하는 공정이 개발되었으나, 이러한 공정에서도 알루미늄 전구체 잉크의 안정화가 확보되지 않아 제조에 어려움이 있었다. In order to solve the problems of the conventional aluminum ink manufacturing process, an aluminum precursor ink was developed, and a process of manufacturing an aluminum film through a simple wet process in a low temperature atmosphere of 150 ° C. or lower has been developed. There was a difficulty in manufacturing.

이에 따라 본 발명자들은 유기금속(organo-metal) 형태인 알루미늄 전구체 잉크 및 이를 이용하여 알루미늄 전극을 제조하는 방법을 개발하였으나, 이 역시 유기금속(organo-metal) 형태인 알루미늄 전구체 잉크를 제조하기 위한 원료 물질 및 용매 등이 취급이 어려워, 효율적이고, 안전적으로 대량 생산이 가능한 새로운 제조 시스템이 필요한 상황이었다.Accordingly, the present inventors have developed an aluminum precursor ink in the form of an organo-metal and a method of manufacturing an aluminum electrode using the same, but this is also a raw material for producing an aluminum precursor ink in the form of an organo-metal. Materials and solvents were difficult to handle, requiring a new manufacturing system capable of mass production efficiently and safely.

본 발명은 상기와 같은 종래 기술의 문제점을 해결하기 위하여 취급이 어려운 원료 물질 및 용매 등을 용이하게 공급할 수 있게 되어, 결과적으로 유기 금속 형태의 알루미늄 전구체 잉크의 양산이 가능하도록 하는 새로운 구조의 알루미늄 전구체 합성 시스템을 제공하는 것을 목적으로 한다. In order to solve the above problems of the prior art, it is possible to easily supply raw materials, solvents, and the like, which are difficult to handle, and consequently, aluminum precursors having a new structure which enables mass production of aluminum precursor ink in the form of organometallic. It is an object to provide a synthesis system.

본 발명은 또한, 본 발명에 의한 알루미늄 전구체 합성 시스템을 이용한 알루미늄 전구체 제조방법을 제공하는 것을 목적으로 한다. Another object of the present invention is to provide a method for producing an aluminum precursor using the aluminum precursor synthesis system according to the present invention.

본 발명은 상기와 같은 과제를 해결하기 위하여 The present invention to solve the above problems

반응기; Reactor;

상기 반응기 내로 원료 물질을 공급하는 원료물질 공급부;A raw material supply unit supplying a raw material into the reactor;

상기 반응기 내로 반응 용매를 공급하는 반응용매 공급부;A reaction solvent supply unit supplying a reaction solvent into the reactor;

상기 반응기 및 반응용매 공급부로 비활성 가스를 공급하는 비활성 가스 공급부; An inert gas supply unit supplying an inert gas to the reactor and the reaction solvent supply unit;

상기 반응기로부터 생성되는 생성물이 유출되어 저장되는 생성물 저장부; 및A product storage unit in which the product generated from the reactor is discharged and stored; And

상기 반응기 및 상기 생성물 저장부와 연결되어 압력을 제어하는 압력 제어부; 를 포함하는 알루미늄 전구체 합성 시스템을 공급한다. A pressure control unit connected to the reactor and the product storage unit to control pressure; It supplies an aluminum precursor synthesis system comprising a.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 원료물질 공급부는, 밀폐된 하우징; 상기 하우징 내에 수용되며, 원료물질을 저장하는 1개 또는 복수개의 원료물질 저장부; 및 상기 원료물질 저장부와 상기 반응기를 연결하며, 상기 원료물질을 상기 반응기로 공급하는 원료물질 공급라인;을 포함한다. In the aluminum precursor synthesis system according to the invention, the raw material supply unit, the sealed housing; One or a plurality of raw material storage units accommodated in the housing and storing raw materials; And a raw material supply line connecting the raw material storage unit and the reactor and supplying the raw material to the reactor.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 반응용매 공급부는, 반응용매를 수용하는 반응용매 저장부; 상기 반응용매를 상기 반응기로 공급하는 반응용매 공급라인;로 구성된다. In the aluminum precursor synthesis system according to the present invention, the reaction solvent supply unit, a reaction solvent storage unit for receiving the reaction solvent; It consists of; a reaction solvent supply line for supplying the reaction solvent to the reactor.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 반응용매 공급은 상기 반응 용매 저장부 내부로 비활성 가스가 주입되어 비활성 가스의 압력으로 반응 용매를 반응기로 공급하기 때문에, 상기 반응용매 공급라인은 상기 반응용매 저장부 내에서 말단이 반응 용매 내에 침지된 상태로 연결되는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the present invention, the reaction solvent supply is because the inert gas is injected into the reaction solvent reservoir to supply the reaction solvent to the reactor at the pressure of the inert gas, the reaction solvent supply line is the reaction The terminal is connected in the solvent reservoir in a state immersed in the reaction solvent.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 비활성 가스 공급부는, 비활성 가스 저장부; 상기 비활성 가스 저장부와 상기 반응용매 저장부를 연결하여 상기 비활성 가스를 상기 반응용매 저장부로 공급하는 제 1 비활성 가스 공급라인; 및 상기 비활성 가스 저장부와 상기 반응기를 연결하여 상기 비활성 가스를 상기 반응기로 공급하는 제 2 비활성 가스 공급라인; 상기 비활성 가스 저장부와 상기 원료물질 공급부를 연결하여 상기 비활성가스를 상기 원료물질 공급부로 공급하는 제 3 비활성 가스 공급라인으로 구성되는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the present invention, the inert gas supply unit, the inert gas storage unit; A first inert gas supply line connecting the inert gas storage unit and the reaction solvent storage unit to supply the inert gas to the reaction solvent storage unit; And a second inert gas supply line connecting the inert gas storage unit and the reactor to supply the inert gas to the reactor. And a third inert gas supply line connecting the inert gas storage unit and the source material supply unit to supply the inert gas to the source material supply unit.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 제 1 비활성 가스 공급라인 말단은 상기 반응 용매 저장부 내에 수용된 상기 반응 용매에 접촉하지 않은 상태로 연결되고, 상기 제 2 비활성 가스 공급라인 말단은 반응기 내에 반응물에 접촉하지 않은 상태로 연결되고, 상기 제 3 비활성 가스 공급라인 말단은 원료물질 공급부 내에 원료물질에 비접촉 상태로 연결되는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the present invention, the end of the first inert gas supply line is connected without contact with the reaction solvent contained in the reaction solvent reservoir, and the end of the second inert gas supply line is in the reactor. It is connected without contacting the reactants, characterized in that the third inert gas supply line end is connected to the raw material in a non-contact state in the raw material supply.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 생성물 저장부는, 반응기로부터 유출되는 생성물을 수용하는 생성물 저장 챔버; 상기 생성물 저장 챔버와 상기 반응기 사이를 연결하는 제 1 생성물 배출 라인; 으로 구성되는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the invention, the product storage unit, the product storage chamber for receiving the product flowing out of the reactor; A first product discharge line connecting between said product storage chamber and said reactor; Characterized in that consists of.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 제 1 생성물 배출 라인은 상기 반응기 하부와 연결되거나, 반응기 상부로부터 인출되어 말단이 상기 반응기 내부의 생성물에 침전되는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the invention, the first product outlet line is connected to the bottom of the reactor, or is withdrawn from the top of the reactor, characterized in that the end is precipitated in the product inside the reactor.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 압력 제어부는, 압력 조절 및 외부환경 노출 방지를 위한 매체를 수용하는 압력 조절 챔버; 진공 펌프; 상기 압력 조절 챔버와 상기 진공 펌프를 연결시키는 제 1 압력 조절 라인; 상기 생성물 저장 챔버와 상기 압력 제어부 사이를 연결하여 상기 생성물 저장 챔버 내의 압력을 조절하는 제 2 압력 조절 라인; 및 상기 반응기와 상기 압력 제어부 사이를 연결하여 상기 반응기 내의 압력을 조절하는 제 3 압력 조절 라인; 을 포함하는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the present invention, the pressure control unit, the pressure control chamber for receiving a medium for pressure control and exposure to the outside environment; A vacuum pump; A first pressure regulation line connecting the pressure regulation chamber and the vacuum pump; A second pressure regulating line connecting between the product storage chamber and the pressure control unit to regulate pressure in the product storage chamber; And a third pressure regulating line connected between the reactor and the pressure controller to regulate pressure in the reactor. Characterized in that it comprises a.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 제 2 압력 조절 라인의 일 말단은 상기 압력 조절을 위한 매체 내에 침지된 상태로 연결되고, 상기 제 3 압력 조절 라인의 말단은 상기 압력 조절을 위한 매체 내에 침지된 상태로 연결되는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the present invention, one end of the second pressure regulation line is connected to the submerged state in the medium for the pressure regulation, the end of the third pressure regulation line is the medium for the pressure regulation It is characterized in that connected in the state immersed in.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 압력 조절을 위한 매체는 실리콘 오일인 것을 특징으로 한다. In the aluminum precursor synthesis system according to the present invention, the pressure control medium is characterized in that the silicone oil.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 제 2 압력 조절 라인 및 제 3 압력 조절 라인은 3 방향밸브로 연결되어 일체적으로 작동하는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the present invention, the second pressure regulating line and the third pressure regulating line are connected by a three-way valve to operate integrally.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 반응기는, 가열부; 상기 반응기 내부 압력을 측정하기 위한 압력 측정부(미도시); 및 상기 반응물의 pH를 측정하기 위한 pH 측정부(미도시);를 포함하는 것을 특징으로 한다.In the aluminum precursor synthesis system according to the present invention, the reactor includes a heating unit; A pressure measuring unit (not shown) for measuring the pressure inside the reactor; And a pH measuring unit (not shown) for measuring the pH of the reactant.

본 발명에 의한 알루미늄 전구체 합성 시스템은 상기 반응기; 상기 반응기 내로 원료 물질을 공급하는 원료물질 공급부; 상기 반응기 내로 반응 용매를 공급하는 반응용매 공급부; 상기 반응기 및 상기 반응용매 공급부로 비활성 가스를 공급하는 비활성 가스 공급부; 상기 반응기로부터 생성되는 생성물이 유출되어 저장되는 생성물 저장부; 및 상기 반응기 및 상기 생성물 저장부와 연결되어 압력을 제어하는 압력 제어부;를 모두 수용하는 하우징을 더 포함하는 것이 가능하다. Aluminum precursor synthesis system according to the invention the reactor; A raw material supply unit supplying a raw material into the reactor; A reaction solvent supply unit supplying a reaction solvent into the reactor; An inert gas supply unit supplying an inert gas to the reactor and the reaction solvent supply unit; A product storage unit in which the product generated from the reactor is discharged and stored; And a pressure control unit connected to the reactor and the product storage unit to control the pressure.

본 발명은 또한, The present invention also provides

비활성 가스를 반응기로 주입하는 단계;Injecting an inert gas into the reactor;

반응용매를 반응기로 주입하는 단계;Injecting a reaction solvent into the reactor;

원료물질을 반응기로 주입하는 단계;Injecting the raw material into the reactor;

반응기 내로 주입된 반응용매 및 원료물질을 교반하고, 반응온도를 제어하여 생성물을 생성하는 단계; Stirring the reaction solvent and the raw material injected into the reactor, and controlling the reaction temperature to generate a product;

상기 생성물을 생성물 저장부로 이송시키는 단계; 를 포함하는 본 발명에 의한 알루미늄 전구체 합성 시스템을 이용한 알루미늄 전구체 제조방법을 제공한다. Transferring the product to a product reservoir; It provides an aluminum precursor manufacturing method using an aluminum precursor synthesis system according to the present invention comprising a.

본 발명에 의한 알루미늄 전구체 제조방법에 있어서, 상기 비활성 가스를 반응기 내로 주입하는 단계에서는, 상기 압력제어부 및 제 3 압력 조절 라인에 의해 반응기 내부의 감압을 유도하여 상기 제 2 비활성 가스 공급라인으로 비활성 가스를 반응기 내로 주입하고, 상기 반응기 내로 주입된 비활성 가스가 생성물 저장부 및 압력 제어부로 이동하도록 하는 것을 특징으로 한다. In the method of manufacturing an aluminum precursor according to the present invention, in the injecting the inert gas into the reactor, the inert gas to the second inert gas supply line by inducing a reduced pressure in the reactor by the pressure control unit and the third pressure control line. Is injected into the reactor, and the inert gas injected into the reactor moves to the product reservoir and the pressure controller.

본 발명은 또한, 상기 비활성 가스를 반응기 내로 주입하는 단계에서는, 상기 반응기, 상기 반응기와 생성물 저장조를 연결하는 제 1 생성물 배출라인, 및 상기 생성물 저장조와 압력조절챔버를 연결하는 제 2 압력조절라인, 및 진공 펌프와 연결된 제 1 압력조절라인을, 밸브 등 기타 당업자가 조절할 수 있는 개폐 수단을 통하여 조절함으로써, 반응기 내부의 감압을 유도하여 압력차에 따라 비활성 가스를 반응기 내로 지속적으로 주입하는 것을 특징으로 한다. The present invention also includes the step of injecting the inert gas into the reactor, the reactor, the first product discharge line connecting the reactor and the product reservoir, and the second pressure control line connecting the product reservoir and the pressure control chamber, And controlling the first pressure control line connected to the vacuum pump through an opening / closing means that can be controlled by those skilled in the art such as a valve, thereby inducing a reduced pressure in the reactor and continuously injecting an inert gas into the reactor according to the pressure difference. do.

본 발명에 의한 알루미늄 전구체 제조방법에 있어서, 상기 비활성 가스를 반응기 내로 주입하는 단계는 이에 의하여 반응시스템 내부 분위기를 비활성 가스로 조절하고, 본 반응을 유도하기 전 반응기 내부의 불순물 제거의 의미도 포함한다. In the method of manufacturing an aluminum precursor according to the present invention, the step of injecting the inert gas into the reactor thereby controls the atmosphere inside the reaction system to the inert gas, and includes the meaning of removing impurities in the reactor before inducing the present reaction. .

이와 같이 본 발명에 의한 알루미늄 전구체 제조방법에 있어서, 상기 비활성 가스를 반응기 내로 주입하는 단계에서는 반응기 내부의 감압을 유도하여 비활성 가스를 주입하되, 반응기 내부의 감압을 유도하는 방법은 특별히 제한되지 않는다. As described above, in the method of manufacturing the aluminum precursor according to the present invention, in the injecting the inert gas into the reactor, the inert gas is injected by inducing a reduced pressure in the reactor, but the method of inducing the reduced pressure in the reactor is not particularly limited.

본 발명에 의한 알루미늄 전구체 제조방법에 있어서, 상기 반응용매를 반응기 내로 주입하는 단계에서는, 상기 제 1 비활성 가스 공급 라인을 통하여 비활성 가스를 반응 용매 저장부로 주입하고, 상기 주입된 비활성 가스의 공기압에 의해 상기 반응 용매가 상기 반응기로 주입되는 것을 특징으로 한다. In the method of manufacturing an aluminum precursor according to the present invention, in the step of injecting the reaction solvent into the reactor, inert gas is injected into the reaction solvent storage through the first inert gas supply line, by the air pressure of the injected inert gas The reaction solvent is characterized in that the injection into the reactor.

본 발명에 의한 알루미늄 전구체 제조방법에 있어서, 상기 반응용매를 반응기 내로 주입하는 단계에서는, 상기 압력제어부 및 제 3 압력 조절 라인에 의해 반응기 내부의 감압을 유도하는 것을 특징으로 한다. In the method of manufacturing an aluminum precursor according to the present invention, in the step of injecting the reaction solvent into the reactor, it is characterized in that the pressure control unit and the third pressure control line to induce a reduced pressure inside the reactor.

본 발명에 의한 알루미늄 전구체 제조방법에 있어서, 상기 원료물질을 반응기로 주입하는 단계에서는, 상기 압력제어부 및 제 3 압력 조절 라인에 의해 반응기 내부의 감압을 유도하여 상기 원료물질을 반응기로 주입하는 것을 특징으로 한다. In the method of manufacturing an aluminum precursor according to the present invention, in the step of injecting the raw material into the reactor, by inducing a reduced pressure inside the reactor by the pressure control unit and the third pressure control line to inject the raw material into the reactor. It is done.

본 발명에 의한 알루미늄 전구체 제조방법에 있어서, 상기 원료물질을 반응기로 주입하는 단계에서는, 상기 반응기와 압력조절챔버를 연결하는 제 3 압력조절라인, 및 상기 압력조절챔버에 연결되어 있는 제 1 압력조절라인을 통하여 밸브 등 기타 당업자가 조절할 수 있는 개폐 수단을 통하여 조절함으로써, 반응기 내부의 감압을 유도하여 압력차에 따라 상기 제 3 비활성 가스공급라인을 통해 원료물질 공급부에 비활성 가스를 공급하여 상기 원료물질을 반응기로 주입하는 것을 특징으로 한다. In the method of manufacturing an aluminum precursor according to the present invention, in the step of injecting the raw material into the reactor, the third pressure control line connecting the reactor and the pressure control chamber, and the first pressure control connected to the pressure control chamber By controlling the opening and closing means that can be adjusted by other persons skilled in the art, such as a valve through the line, induces a reduced pressure in the reactor to supply an inert gas to the raw material supply unit through the third inert gas supply line according to the pressure difference It characterized in that the injection into the reactor.

본 발명에 의한 알루미늄 전구체 제조방법에 있어서, 상기 생성물을 생성물 저장부로 이송시키는 단계에서는, 상기 압력제어부 및 제 2 압력 조절 라인에 의해 반응기 및 생성물 저장부 내부의 감압을 유도하여 상기 생성물을 생성물 저장부로 이송하는 것을 특징으로 한다. In the method of manufacturing an aluminum precursor according to the present invention, in the step of transferring the product to the product storage unit, by inducing a reduced pressure in the reactor and the product storage unit by the pressure control unit and the second pressure control line to the product storage unit. Characterized in that the transfer.

본 발명의 알루미늄 전구체 합성 시스템 및 이를 이용한 알루미늄 전구체 제조방법은 용매 공급부, 원료 물질 공급부 등이 반응기와 일체적으로 연결되고, 압력 제어부를 이용한 시스템 내부 압력 차이를 조절하여, 종래 취급이 어려웠던 원료물질, 반응 용매등을 체계적으로 공급 가능하게 되고, 이에 따라 결과적으로 유기 금속 형태의 알루미늄 전구체 잉크의 양산이 가능하도록 한다. In the aluminum precursor synthesis system of the present invention and a method for manufacturing an aluminum precursor using the same, a solvent supply unit, a raw material supply unit, etc. are integrally connected to the reactor, and by adjusting the pressure difference in the system using the pressure control unit, raw materials, which have been difficult to handle in the past, The reaction solvent and the like can be systematically supplied, and as a result, mass production of the aluminum precursor ink in the form of an organic metal is possible.

도 1 내지 도 8은 본 발명의 실시예에 의한 알루미늄 전구체 합성 시스템을 나타낸다.1 to 8 show an aluminum precursor synthesis system according to an embodiment of the present invention.

이하에서는 본 발명을 도면 및 실시예에 의하여 더욱 상세히 설명한다. 그러나, 본 발명이 이하의 설명에 의하여 한정되는 것은 아니다. Hereinafter, the present invention will be described in more detail with reference to the drawings and examples. However, the present invention is not limited by the following description.

본 명세서에서 사용된 용어는 실시예들을 설명하기 위한 것이며 본 발명을 제한하고자 하는 것은 아니다. 본 명세서에서, 단수형은 문구에서 특별히 언급하지 않는 한 복수형도 포함한다. 명세서에서 사용되는 "포함한다(comprises)" 및/또는 "포함하는(comprising)"은 언급된 구성요소, 단계, 동작 및/또는 소자는 하나 이상의 다른 구성요소, 단계, 동작 및/또는 소자의 존재 또는 추가를 배제하지 않는다.The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In this specification, the singular also includes the plural unless specifically stated otherwise in the phrase. As used herein, “comprises” and / or “comprising” refers to the presence of one or more other components, steps, operations and / or elements. Or does not exclude additions.

도 1에 본 발명에 의한 알루미늄 전구체 합성 시스템을 나타내었다. 1 shows an aluminum precursor synthesis system according to the present invention.

도 1에서 보는 바와 같이 본 발명에 의한 알루미늄 전구체 합성 시스템은 반응기(100); 상기 반응기 내로 원료 물질을 공급하는 원료물질 공급부(200); 상기 반응기 내로 반응 용매를 공급하는 반응용매 공급부(300); 상기 반응기 및 반응용매 공급부로 비활성 가스를 공급하는 비활성 가스 공급부(400); 상기 반응기로부터 생성되는 생성물이 유출되어 저장되는 생성물 저장부(500); 및 상기 반응기 및 상기 생성물 저장부와 연결되어 압력을 제어하는 압력 제어부(600); 를 포함한다. As shown in Figure 1, the aluminum precursor synthesis system according to the present invention comprises a reactor (100); A raw material supply unit 200 for supplying a raw material into the reactor; A reaction solvent supply unit 300 supplying a reaction solvent into the reactor; An inert gas supply unit 400 supplying an inert gas to the reactor and the reaction solvent supply unit; A product storage part 500 in which the product generated from the reactor is leaked out and stored; And a pressure control unit 600 connected to the reactor and the product storage unit to control pressure. It includes.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 반응기(100)는, 가열부(110); 상기 반응기 내부 압력을 측정하기 위한 압력 측정부(미도시); 및 상기 반응물의 pH를 측정하기 위한 pH 측정부(미도시);를 포함하는 것이 가능하다. In the aluminum precursor synthesis system according to the present invention, the reactor 100, the heating unit 110; A pressure measuring unit (not shown) for measuring the pressure inside the reactor; And a pH measurement unit (not shown) for measuring the pH of the reactant.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 반응기 내부의 온도를 일정 온도로 유지하기 위한 가열부(110)는 도 1 내지 도 4에 도시된 바와 같이 별도의 가열부에서 가열된 열 전달 매체를 반응기 주변으로 순환시키는 방식, 가열 mantle과 같은 직접 가열 방식이 가능하며, 그외 당업자가 자유롭게 선택할 수 있다. In the aluminum precursor synthesis system according to the present invention, the heating unit 110 for maintaining the temperature inside the reactor at a constant temperature is a heat transfer medium heated in a separate heating unit as shown in FIGS. It is possible to circulate around the reactor, a direct heating method such as a heating mantle, and others can freely choose.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 반응기는 유기 합성시 사용되는 반응기라면 특별히 제한되지 않는다. In the aluminum precursor synthesis system according to the present invention, the reactor is not particularly limited as long as it is a reactor used in organic synthesis.

본 발명에 의한 알루미늄 전구체 합성 시스템은 상기 반응기와 연결되는 압력 제어부(600)에 의해 반응기 내부의 감압이 유도되므로, 상기 반응기 내부의 압력을 측정하기 위한 압력 측정부를 포함하는 것이 바람직하다. Since the aluminum precursor synthesis system according to the present invention induces a reduced pressure inside the reactor by the pressure control unit 600 connected to the reactor, it is preferable to include a pressure measuring unit for measuring the pressure inside the reactor.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 원료물질 공급부(200)는, 밀폐된 하우징(210); 상기 하우징 내에 수용되며, 알루미늄 전구체 합성을 위한 원료물질을 저장하는 1개 또는 복수개의 원료물질 저장부(220, 230, 240); 및 상기 원료물질 저장부와 상기 반응기를 연결하며, 상기 원료물질을 상기 반응기로 공급하는 원료물질 공급라인(L2); 을 포함한다. In the aluminum precursor synthesis system according to the present invention, the raw material supply unit 200, the sealed housing 210; One or a plurality of raw material storage units 220, 230, and 240 accommodated in the housing and storing raw materials for synthesizing an aluminum precursor; And a raw material supply line (L2) connecting the raw material storage unit and the reactor to supply the raw material to the reactor. It includes.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 복수개의 원료 물질의 투입량을 개별적으로 조절할 수 있는 조절 장치를 더 포함하는 것이 가능하다. 본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 원료물질 투입량 조절방법은 비이커 또는 매스실린더에 원료물질을 넣고 투입량에 의한 부피변화를 감지하는 방법과 저울 등의 load cell을 이용하여 원료물질 투입량에 따른 질량변화 감지 등을 통해 원료물질 투입량을 조절할 수 있다.In the aluminum precursor synthesis system according to the present invention, it is possible to further include a control device that can individually adjust the input amount of the plurality of raw materials. In the aluminum precursor synthesis system according to the present invention, the method of controlling the input amount of the raw material is a method for detecting the change in volume by the input amount of the raw material in the beaker or the mass cylinder and the mass according to the input material input by using a load cell such as a scale Raw material inputs can be controlled by detecting changes.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 반응용매 공급부(300)는, 반응용매를 수용하는 반응용매 저장부(310); 상기 반응용매를 상기 반응기로 공급하는 반응용매 공급라인(L3); 로 구성된다. In the aluminum precursor synthesis system according to the present invention, the reaction solvent supply unit 300, a reaction solvent storage unit 310 for receiving a reaction solvent; A reaction solvent supply line (L3) for supplying the reaction solvent to the reactor; It consists of.

본 발명에 의한 알루미늄 전구체 합성 시스템에 의하여 제조되는 알루미늄 전구체는 당업자들에게 자명한 모든 가능한 알루미늄 전구체가 포함되며, 본 발명의 실시예로 제한되지 않는다.The aluminum precursor produced by the aluminum precursor synthesis system according to the present invention includes all possible aluminum precursors apparent to those skilled in the art, and is not limited to the embodiments of the present invention.

본 발명에 의한 알루미늄 전구체 합성 시스템에 의하여 합성되는 상기 알루미늄 전구체는 치환된 및/또는 치환되지 않은 알루미늄 수소화물 화합물들을 포함한다. 예를 들어, 한 실시예에서, 알루미늄 금속 전구체는 AlH3를 포함한다. 다른 실시예들에서, 알루미늄 금속 전구체는 하나 이상의 유기 측쇄(예를 들어, 아이소뷰틸알루미늄 수소화물, 다이메틸알루미늄 수소화물 등과 같은 알킬-치환 알루미늄 수소화물) 및/또는 트라이알킬 알루미늄 종(예를 들어, 트라이아이소뷰틸 알루미늄)으로 치환된 알루미늄 수소화물을 포함한다. The aluminum precursor synthesized by the aluminum precursor synthesis system according to the present invention comprises substituted and / or unsubstituted aluminum hydride compounds. For example, in one embodiment, the aluminum metal precursor comprises AlH 3 . In other embodiments, the aluminum metal precursor may comprise one or more organic side chains (eg, alkyl-substituted aluminum hydrides such as isobutylaluminum hydride, dimethylaluminum hydride, etc.) and / or trialkyl aluminum species (eg, Aluminum hydride substituted with triisobutyl aluminum).

다른 실시예들에서, 알루미늄 금속 전구체는 치환된 및/또는 치환되지 않은 알루미늄 수소화물과 착물을 형성하는 하나 이상의 리간드를 더 포함할 수 있다. 더욱 구체적으로, 알루미늄 전구체는 아민, 포스핀, 에터 및/또는 다른 적절한(도너-타입) 리간드로부터 선택된 하나 또는 두 개의 리간드를 포함할 수 있다. In other embodiments, the aluminum metal precursor may further include one or more ligands that complex with substituted and / or unsubstituted aluminum hydride. More specifically, the aluminum precursor may comprise one or two ligands selected from amines, phosphines, ethers and / or other suitable (donor-type) ligands.

일 예로서 상기 알루미늄 전구체로서 알루미늄 수소화물은 에테르 용매 내에서 아래와 같은 리튬알루미늄 수소화물(LiAlH4)과 AlCl3의 반응에 의해 제조될 수 있으며, 이에 따라 상기 원료 물질은 리튬알루미늄 수소화물(LiAlH4)과 AlCl3을 포함하고, 상기 반응 용매는 에테르를 포함할 수 있다. As an example, aluminum hydride as the aluminum precursor may be prepared by a reaction of lithium aluminum hydride (LiAlH 4 ) and AlCl 3 in an ether solvent, and thus the raw material may be lithium aluminum hydride (LiAlH 4). ) And AlCl 3 , and the reaction solvent may include ether.

3 LiAlH4 + AlCl3 → 4 AlH3 + 3 LiCl3 LiAlH 4 + AlCl 3 → 4 AlH 3 + 3 LiCl

상기 반응 용매로서 에테르 용매는 하나 이상의 지방족 에테르를 포함할 수 있고, 이의 예들은 다이에틸 에테르, 다이-n-프로필 에테르, 다이-n-뷰틸 에테르, 다이-아이소프로필 에테르, 다이-t-뷰틸 에테르, 메틸-뷰틸 에테르, n-프로필-n-뷰틸 에테르, 메틸-t-뷰틸 에테르, 에틸-t-뷰틸 에테르, 또는 이의 혼합물을 포함한다.Ether solvent as the reaction solvent may include one or more aliphatic ethers, examples of which are diethyl ether, di-n-propyl ether, di-n-butyl ether, di-isopropyl ether, di-t-butyl ether , Methyl-butyl ether, n-propyl-n-butyl ether, methyl-t-butyl ether, ethyl-t-butyl ether, or mixtures thereof.

상기 원료 물질은 알루미늄 전구체 조성물에 포함되는 하나 이상의 첨가제(예를 들어, 계면활성제, 접착 향상제 및/또는 촉매)를 포함할 수 있다. The raw material may include one or more additives (eg, surfactants, adhesion promoters and / or catalysts) included in the aluminum precursor composition.

본 발명자들에 의해 발명된 AlCl3 및 LiAlH4를 용매인 디부틸설파이드에 첨가하고 혼합하여 하기 반응식과 같이 디부틸설파이드기가 결합된 형태의 알루미늄 전구체와 LiCl이 생성되는 경우 반응 용매는 디부틸설파이드를 포함할 수 있다. When AlCl 3 and LiAlH 4 invented by the present inventors are added to dibutyl sulfide as a solvent and mixed to produce an aluminum precursor and LiCl in the form of a dibutyl sulfide group bonded as shown in the following scheme, the reaction solvent is dibutyl sulfide. It may include.

AlCl3 + 3LiAlH4 + S(C4H9)2 (용매) → 4SAlH3(C4H9)2 + 3LiCl + S(C4H9)2 (용매) → 필터링 → 4SAlH3(C4H9)2 + S(C4H9)2 (용매)AlCl 3 + 3LiAlH 4 + S (C 4 H 9 ) 2 (solvent) → 4SAlH 3 (C 4 H 9 ) 2 + 3LiCl + S (C 4 H 9 ) 2 (solvent) → filtering → 4SAlH 3 (C 4 H 9 ) 2 + S (C 4 H 9 ) 2 (solvent)

본 발명자들에 의해 발명된 공정에 따라 AlCl3 및 LiAlH4를 용매인 디에틸설파이드에 첨가하고 혼합하여 하기 반응식과 같이 디에틸설파이드기가 결합된 형태의 알루미늄 전구체와 LiCl이 생성되는 경우 반응 용매는 디에틸설파이드를 포함할 수 있다. According to the process invented by the inventors, when AlCl 3 and LiAlH 4 are added to diethyl sulfide as a solvent and mixed to produce an aluminum precursor and LiCl in the form of a diethyl sulfide group bonded as shown in the following scheme, the reaction solvent is di Ethyl sulfide may be included.

AlCl3 + 3LiAlH4 + S(C2H5)2 (용매) → 4SAlH3(C2H5)2 + 3LiCl + S(C2H5)2 (용매) → 필터링 → 4SAlH3(C2H5)2 + S(C2H5)2 (용매)AlCl 3 + 3LiAlH 4 + S (C 2 H 5 ) 2 (solvent) → 4SAlH 3 (C 2 H 5 ) 2 + 3LiCl + S (C 2 H 5 ) 2 (solvent) → filtering → 4SAlH 3 (C 2 H 5 ) 2 + S (C 2 H 5 ) 2 (solvent)

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 비활성 가스 공급부(400)는, 원료가 되는 비활성 가스를 저장하는 비활성 가스 저장부(410); 상기 비활성 가스 저장부와 상기 반응용매 저장부(300)를 연결하여 상기 비활성 가스를 상기 반응용매 저장부로 공급하는 제 1 비활성 가스 공급라인(L4-1); 및 상기 비활성 가스 저장부와 상기 반응기(100)를 연결하여 상기 비활성 가스를 상기 반응기로 공급하는 제 2 비활성 가스 공급라인(L4-2); 상기 비활성 가스 저장부와 상기 원료물질 공급부를 연결하여 상기 비활성 가스를 상기 원료물질 공급부로 공급하는 제 3 비활성 가스 공급라인 (L4-3)으로 구성되는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the present invention, the inert gas supply unit 400, an inert gas storage unit 410 for storing an inert gas to be a raw material; A first inert gas supply line (L4-1) connecting the inert gas storage unit and the reaction solvent storage unit 300 to supply the inert gas to the reaction solvent storage unit; And a second inert gas supply line (L4-2) connecting the inert gas storage unit and the reactor (100) to supply the inert gas to the reactor. And a third inert gas supply line L4-3 which connects the inert gas storage unit and the source material supply unit to supply the inert gas to the source material supply unit.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 제 1 비활성 가스 공급라인(L4-1) 의 반응 용매 저장부와 접하는 말단은 상기 반응 용매 저장부(310) 내에 수용된 상기 반응 용매에 접촉하지 않은 상태로 연결되고, 상기 제 2 비활성 가스 공급라인(L4-2)의 반응기와 접하는 말단은 반응기 내에 반응물에 접촉하지 않은 상태로 연결되고, 제 3 비활성 가스 공급라인(L4-3)의 원료물질 공급부와 접하는 말단은 원료소재 공급부 내 원료물질과 접촉하지 않은 상태로 연결되는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the present invention, the terminal contacting the reaction solvent storage of the first inert gas supply line (L4-1) is not in contact with the reaction solvent contained in the reaction solvent storage 310 Connected to the reactor, and the end of the second inert gas supply line (L4-2) contacting the reactor is not in contact with the reactants in the reactor, and the raw material supply part of the third inert gas supply line (L4-3) The contact end is characterized in that connected to the raw material in a state not in contact with the raw material supply.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 비활성 가스가 상기 반응 용매 저장부(310) 내부로 주입되면 상기 반응 용매 저장부 내의 비활성 가스의 압력으로 반응 용매를 반응기로 밀어내는 방식으로 반응 용매를 반응기 내부로 공급하는 것을 특징으로 한다. 이를 위하여 상기 제 1 비활성 가스 공급라인(L4-1) 말단은 상기 반응 용매 저장부(310) 내에 수용된 상기 반응 용매에 접촉하지 않은 상태로 연결되고, 상기 반응용매 공급라인(L3)의 상기 반응용매 저장부 내에서 말단이 반응 용매 내에 침지된 상태로 연결되는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the present invention, when the inert gas is injected into the reaction solvent reservoir 310, the reaction solvent is pushed into the reactor at a pressure of the inert gas in the reaction solvent reservoir. It is characterized in that the feed into the reactor. To this end, the end of the first inert gas supply line (L4-1) is connected without contact with the reaction solvent contained in the reaction solvent storage 310, the reaction solvent of the reaction solvent supply line (L3) It is characterized in that the terminals are connected in a reservoir so as to be immersed in the reaction solvent.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 생성물 저장부(500)는, 반응기로부터 유출되는 생성물을 수용하는 생성물 저장 챔버(510); 상기 생성물 저장 챔버와 상기 반응기 사이를 연결하는 제 1 생성물 배출 라인(L5); 로 구성되는 것을 특징으로 한다. 본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 생성물 저장 챔버(510) 는 카트리지 타입으로 제조되어 본 발명에 의한 알루미늄 전구체 합성 시스템으로부터 분리 가능한 상태로 설치될 수 있다. In the aluminum precursor synthesis system according to the present invention, the product storage unit 500, the product storage chamber for receiving the product flowing out of the reactor (510); A first product discharge line (L5) connecting between said product storage chamber and said reactor; Characterized in that consists of. In the aluminum precursor synthesis system according to the present invention, the product storage chamber 510 may be manufactured in a cartridge type and installed in a detachable state from the aluminum precursor synthesis system according to the present invention.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 생성물 저장부(500)는, 도 1 내지 도 4에서 보는 바와 같이 반응기 내에 별도의 챔버 없이 배치되거나, 별도의 챔버(미도시) 내에 배치되는 것이 가능하다. In the aluminum precursor synthesis system according to the present invention, the product reservoir 500, as shown in Figures 1 to 4 can be arranged in a reactor without a separate chamber, or may be disposed in a separate chamber (not shown). Do.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 압력 제어부(600)는, 반응시스템 내의 압력 조절 및 반응물 및 생성물의 외부환경과의 직접적 접촉 차단을 위한 매체를 수용하는 압력 조절 챔버(610); 진공 펌프(620); 상기 압력 조절 챔버와 상기 진공 펌프를 연결시키는 제 1 압력 조절 라인(L6-1); 상기 생성물 저장 챔버와 상기 압력 제어부 사이를 연결하여 상기 생성물 저장 챔버 내의 압력을 조절하는 제 2 압력 조절 라인(L6-2); 및 상기 반응기와 상기 압력 제어부 사이를 연결하여 상기 반응기 내의 압력을 조절하는 제 3 압력 조절 라인(L6-3); 을 포함하는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the present invention, the pressure control unit 600 includes a pressure control chamber 610 for receiving a medium for controlling pressure in the reaction system and blocking direct contact of reactants and products with the external environment; Vacuum pump 620; A first pressure regulating line (L6-1) connecting the pressure regulating chamber and the vacuum pump; A second pressure regulating line (L6-2) connected between the product storage chamber and the pressure controller to regulate the pressure in the product storage chamber; And a third pressure regulating line (L6-3) connected between the reactor and the pressure controller to adjust the pressure in the reactor. Characterized in that it comprises a.

본 발명에 의한 알루미늄 전구체 합성 시스템은 별도의 구동 수단을 포함하지 않고, 반응기(100) 및 생성물 저장부(500)에 연결된 압력 제어부(600)를 포함하고, 압력 제어부의 동작에 의해 생성물 저장 챔버(500) 및 원료소재 공급부(200) 내의 압력을 조절하여 압력 차이에 의해 취급이 어려운 반응물, 반응 용매, 원료물질을 이동시키고, 또한, 생성되는 생성물이 외부로 유출되는 경우 이를 수용하는 버퍼 역할도 수행하게 된다. The aluminum precursor synthesis system according to the present invention does not include a separate driving means, and includes a pressure control unit 600 connected to the reactor 100 and the product storage unit 500, and the product storage chamber ( 500) and the raw material supply unit 200 by controlling the pressure to move the reactants, reaction solvents, raw materials difficult to handle due to the pressure difference, and also serves as a buffer to accommodate the product generated when it is leaked to the outside Done.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 제 2 압력 조절 라인(L6-2)의 일 말단은 상기 압력 조절을 위한 매체 내에 침지된 상태로 연결되고, 상기 제 3 압력 조절 라인(L6-3)의 말단은 상기 압력 조절을 위한 매체 내에 침지된 상태로 연결되어, 상기 진공 펌프(620)에 의해 먼저 압력 조절 챔버 내부의 감압이 유도되고, 이후 상기 압력 조절 챔버와 연결된 반응기 내부의 감압을 유도하여 반응기 내부의 반응물 또는 생성물 저장 챔버 내의 반응물이 오버플로우 되는 경우에도 일단 압력 조절 챔버 내에 수용된 압력 조절을 위한 매체 내로 포집되도록 하는 것을 특징으로 한다. In the aluminum precursor synthesis system according to the present invention, one end of the second pressure control line (L6-2) is connected in a state immersed in the medium for the pressure control, the third pressure control line (L6-3) ) End is connected to the state immersed in the pressure control medium, the vacuum pump 620 is first induced a pressure reduction inside the pressure control chamber, and then induces a pressure reduction inside the reactor connected to the pressure control chamber So that even if the reactant in the reactor or the reactant in the product storage chamber overflows, it is collected into the medium for pressure regulation once contained in the pressure control chamber.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 압력 조절 챔버 내에 수용되는 압력 조절을 위한 매체는 알칸계열, 방향족 계열, 에테르 계열, 오일 계열 등의 비수용성 용액 중 당업자가 자유롭게 선택할 수 있으며, 구체적으로는 실리콘 오일인 것이 바람직하다. In the aluminum precursor synthesis system according to the present invention, the pressure control medium contained in the pressure control chamber may be freely selected by those skilled in the art from non-aqueous solutions such as alkane series, aromatic series, ether series, oil series, and the like. Is preferably a silicone oil.

도 2에 본 발명의 다른 실시예에 의한 알루미늄 전구체 합성 시스템을 나타내었다. 도 2에서 보는 바와 같이 상기 제 2 압력 조절 라인(L6-2) 및 제 3 압력 조절 라인(L6-3)은 3 방향밸브로 연결되어 일체적으로 작동하는 것을 특징으로 한다. 2 shows an aluminum precursor synthesis system according to another embodiment of the present invention. As shown in FIG. 2, the second pressure regulating line L6-2 and the third pressure regulating line L6-3 are connected to each other by a three-way valve to operate integrally.

도 3 및 도 4 에 본 발명의 다른 실시예에 의한 알루미늄 전구체 합성 시스템을 나타내었다. 도 3 및 도 4 에서 보는 바와 같이 본 발명에 의한 알루미늄 전구체 합성 시스템은 상기 반응기와 상기 생성물 저장부 사이에 연결되어 상기 반응기로부터 생성되는 생성물을 필터링하는 필터(710)를 구비하는 필터링부(700)를 더 포함할 수 있다. 3 and 4 show an aluminum precursor synthesis system according to another embodiment of the present invention. As shown in FIGS. 3 and 4, the aluminum precursor synthesis system according to the present invention is connected to the reactor and the product reservoir, and includes a filter 700 including a filter 710 for filtering a product generated from the reactor. It may further include.

본 발명의 다른 실시예에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 필터링부는 반응기에서 생성되어 이송되는 생성물 내에 잔류하는 원료 물질 및 침전물을 필터링 하게 된다. 일 예로서, 원료물질로서 AlCl3 및 LiAlH4를 용매로서 디부틸설파이드를 사용하여 반응시키는 경우 알루미늄 전구체 외에 LiCl 이 생성되며, 이와 같이 생성물 외에 생성되는 부산물은 상기 필터(710)에 의해 필터링되고, 상기 생성물 저장부에는 알루미늄 전구체만이 저장되게 된다. In the aluminum precursor synthesis system according to another embodiment of the present invention, the filtering unit is to filter the raw material and precipitate remaining in the product generated and transported in the reactor. For example, when reacting AlCl 3 and LiAlH 4 as a raw material with dibutyl sulfide as a solvent, LiCl is generated in addition to the aluminum precursor, and the by-products generated outside the product are filtered by the filter 710, Only the aluminum precursor is stored in the product reservoir.

본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 필터링부에 사용되는 필터는 알루미늄 전구체와 반응하지 않는 재질로 구성된 것을 사용하는 것이 가능하며, 더욱 구체적으로는 셀룰로우즈 계열의 필터, 폴리에스터, 폴리프로필렌, 폴리스티렌 등의 폴리머계열 필터 등을 사용할 수 있다.In the aluminum precursor synthesis system according to the present invention, the filter used in the filtering unit may be made of a material that does not react with the aluminum precursor, more specifically, a cellulose-based filter, polyester, poly Polymer-based filters such as propylene and polystyrene can be used.

도 3 및 도 4 에서 보는 바와 같이 본 발명에 의한 알루미늄 전구체 합성 시스템은 상기 반응기(100)와 필터(710)를 연결하는 제 2 생성물 배출 라인(L7-1); 및 상기 필터(710)와 상기 생성물 저장부를 연결하는 제 3 생성물 배출 라인(L7-2); 을 더 포함하는 것을 특징으로 한다. 본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 제 3 생성물 배출 라인(L7-2)의 말단은 상기 압력 조절부 내에 침지된 상태로 연결된다. 3 and 4, the aluminum precursor synthesis system according to the present invention includes a second product discharge line L7-1 connecting the reactor 100 and the filter 710; And a third product discharge line L7-2 connecting the filter 710 and the product reservoir. It characterized in that it further comprises. In the aluminum precursor synthesis system according to the present invention, the end of the third product discharge line (L7-2) is connected in the state immersed in the pressure regulator.

도 4에서 보는 바와 같이 본 발명에 의한 알루미늄 전구체 합성 시스템에 있어서, 상기 제 2 압력 조절 라인(L6-2) 및 제 3 압력 조절 라인(L6-3)은 3 방향밸브로 연결되어 일체적으로 작동하는 것을 특징으로 한다.In the aluminum precursor synthesis system according to the present invention as shown in Figure 4, the second pressure regulating line (L6-2) and the third pressure regulating line (L6-3) is connected by a three-way valve to operate integrally Characterized in that.

도 5 내지 도 8은 본 발명의 다른 실시예에 의한 알루미늄 전구체 합성 시스템을 나타내었다. 5 to 8 show an aluminum precursor synthesis system according to another embodiment of the present invention.

도 5 및 도 6 에서 보는 바와 같이 상기 반응기(100)와 상기 생성물 저장 챔버(500) 사이를 연결하는 제 1 생성물 배출 라인(L5) 은 상기 반응기(100) 의 상부로 인출되는 것이 가능하다. As shown in FIGS. 5 and 6, a first product discharge line L5 connecting between the reactor 100 and the product storage chamber 500 may be drawn out to the top of the reactor 100.

또한, 도 7 및 도 8 에서 보는 바와 같이 상기 반응기(100)와 상기 필터링부(700) 사이를 연결하는 제 2 생성물 배출 라인(L7-1') 은 상기 반응기(100) 의 상부로 인출되고, 상기 제 2 생성물 배출 라인(L7-1') 의 말단은 반응기 내부의 생성물에 침지되는 것이 가능하다. In addition, as shown in FIG. 7 and FIG. 8, the second product discharge line L7-1 ′ connecting between the reactor 100 and the filtering unit 700 is drawn out to the top of the reactor 100, The end of the second product discharge line L7-1 'can be immersed in the product inside the reactor.

도 1 내지 도 8에서 보는 바와 같이 본 발명에 의한 알루미늄 전구체 합성 시스템은 상기 반응기; 상기 반응기 내로 원료 물질을 공급하는 원료물질 공급부; 상기 반응기 내로 반응 용매를 공급하는 반응용매 공급부; 상기 반응기 및 상기 반응용매 공급부로 비활성 가스를 공급하는 비활성 가스 공급부; 상기 반응기로부터 생성되는 생성물이 유출되어 저장되는 생성물 저장부; 및 상기 반응기 및 상기 생성물 저장부와 연결되어 압력을 제어하는 압력 제어부;를 모두 수용하는 하우징(800)을 더 포함하는 것이 가능하다. 1 to 8, the aluminum precursor synthesis system according to the present invention is the reactor; A raw material supply unit supplying a raw material into the reactor; A reaction solvent supply unit supplying a reaction solvent into the reactor; An inert gas supply unit supplying an inert gas to the reactor and the reaction solvent supply unit; A product storage unit in which the product generated from the reactor is discharged and stored; It is possible to further include a housing (800) containing both; and a pressure control unit connected to the reactor and the product reservoir to control the pressure.

이하에서는 본 발명의 알루미늄 전구체 합성 시스템을 이용한 알루미늄 전구체 제조방법을 설명한다. Hereinafter, an aluminum precursor manufacturing method using the aluminum precursor synthesis system of the present invention will be described.

본 발명에 의한 알루미늄 전구체 합성 시스템을 이용한 알루미늄 전구체 제조방법은 Method for producing an aluminum precursor using the aluminum precursor synthesis system according to the present invention

비활성 가스를 반응기로 주입하는 단계; Injecting an inert gas into the reactor;

반응용매를 반응기로 주입하는 단계; Injecting a reaction solvent into the reactor;

원료물질을 반응기로 주입하는 단계; Injecting the raw material into the reactor;

반응기 내로 주입된 반응용매 및 원료물질을 교반하고, 반응온도를 제어하여 생성물을 생성하는 단계; 및 Stirring the reaction solvent and the raw material injected into the reactor, and controlling the reaction temperature to generate a product; And

상기 생성물을 생성물 저장부로 이송시키는 단계; 를 포함한다. Transferring the product to a product reservoir; It includes.

먼저, 비활성 가스를 반응기로 주입하는 단계에서는 도 1에서 비활성 가스 저장부(410)에 저장되어 있던 비활성 가스가 제 2 비활성 가스 공급라인(L4-2)을 통해서 반응기(100)로 공급되고, 반응기(100)로 공급된 비활성 가스는 생성물 저장부(500) 및 압력 조절부(600)까지 이동하면서 주된 반응을 유도하기 전 반응기 내부의 불순물 제거 및 전체적인 시스템 내부를 비활성 상태로 유지하게 된다. First, in the injecting the inert gas into the reactor inert gas stored in the inert gas storage unit 410 in Figure 1 is supplied to the reactor 100 through the second inert gas supply line (L4-2), the reactor The inert gas supplied to the 100 moves to the product reservoir 500 and the pressure regulator 600 to keep impurities in the reactor and the entire system inert before inducing the main reaction.

이때 반응기 내부를 감압 유도하여 비활성 가스 공급을 원활하게 하기 위해 압력 조절을 위한 매체를 수용하는 압력 조절 챔버(610)와 반응기(100) 사이를 연결하는 제 3 압력 조절 라인(L6-3) 및 진공 펌프(620), 제 1 압력 조절 라인(L6-1)으로 반응기(100) 내의 감압을 유도할 수 있다. 또는 제 1 압력조절라인 (L6-1)을 말단 부분을 외부환경에 노출시킨 후 반응기(100)와 생성물 저장부(510)를 연결하는 라인 (L5)에 설치되어 있는 밸브, 생성물 저장부 (510)와 압력조절챔버(610) 사이를 연결하는 라인 (L6-2)에 설치되어 있는 밸브를 열어, 비활성 가스를 반응기내로 공급 공급하는 방법으로 전 반응기 내부의 불순물 제거 및 전체적인 시스템 내부를 비활성 상태로 유지할 수 있다.At this time, the third pressure control line (L6-3) and the vacuum connecting the pressure control chamber 610 and the reactor 100 for receiving a medium for pressure control to facilitate the inert gas supply by inducing a reduced pressure inside the reactor A pressure in the reactor 100 may be induced by the pump 620 and the first pressure regulating line L6-1. Or a valve installed in the line L5 connecting the reactor 100 and the product reservoir 510 after exposing the first pressure regulating line L6-1 to the external environment, and the product reservoir 510. ) By opening the valve installed in the line (L6-2) connecting the pressure control chamber 610 and supplying the inert gas into the reactor. Can be maintained.

반응용매를 반응기로 주입하는 단계에서는 비활성 가스 저장부(410)에 저장되어 있던 비활성 가스를 제 1 비활성 가스 공급라인(L4-1)을 통해서 반응용매 저장부(300)로 공급하고, 공급된 비활성 가스의 압력에 의해 반응 용매가 반응용매 공급라인(L3)을 통해 반응기(100) 내부로 공급된다. 이때 반응기 내부를 감압 유도하여 반응 용매 공급을 원활하게 하기 위해 압력 조절을 위한 매체를 수용하는 압력 조절 챔버(610)와 반응기(100) 사이를 연결하는 제 3 압력 조절 라인(L6-3) 및 진공 펌프(620), 제 1 압력 조절 라인(L6-1)으로 반응기(100) 내의 감압을 유도할 수 있다. In the step of injecting the reaction solvent into the reactor, the inert gas stored in the inert gas storage unit 410 is supplied to the reaction solvent storage unit 300 through the first inert gas supply line L4-1, and the supplied inert The reaction solvent is supplied into the reactor 100 through the reaction solvent supply line L3 by the pressure of the gas. At this time, the third pressure control line (L6-3) and the vacuum connecting between the pressure control chamber 610 and the reactor 100 for receiving a medium for pressure control to facilitate the reaction solvent supply by inducing a reduced pressure inside the reactor A pressure in the reactor 100 may be induced by the pump 620 and the first pressure regulating line L6-1.

이후 원료물질을 반응기로 주입하는 단계에서는 원료물질 저장부(200)에 저장된 1개 또는 복수개의 원료 물질(220, 230, 240)을 원료물질 공급라인(L2)을 통해서 반응기(100) 내부로 공급된다. 이때 반응기 내부를 감압 유도하여 원료 물질 을 공급하기 위해 압력 조절 챔버(610)와 반응기(100) 사이를 연결하는 제 3 압력 조절 라인(L6-3) 및 진공 펌프(620), 제 1 압력 조절 라인(L6-1)으로 반응기(100) 내의 감압을 유도할 수 있다. 또는 제 3 비활성가스 공급라인(L4-3)을 통해 원료물질 저장부(200)에 비활성가스를 주입하여 원료물질을 반응기(100) 내부로 밀어내는 방식으로 공급하는 것이 가능하다. 이때 제 3 압력조절라인(L6-3)의 밸브를 열고 제 1 압력조절라인(L6-1)의 말단을 외부환경에 노출시켜 반응기(100)의 압력을 원료물질 저장부(200) 압력보다 낮게 유지한다.Thereafter, in the step of injecting the raw material into the reactor, one or a plurality of raw materials 220, 230, and 240 stored in the raw material storage unit 200 are supplied into the reactor 100 through the raw material supply line L2. do. At this time, the third pressure control line (L6-3) and the vacuum pump 620, the first pressure control line connecting between the pressure control chamber 610 and the reactor 100 to supply the raw material by inducing a reduced pressure inside the reactor (L6-1) may induce a reduced pressure in the reactor (100). Alternatively, the inert gas may be injected into the raw material storage unit 200 through the third inert gas supply line L4-3 to supply the raw material by pushing the raw material into the reactor 100. At this time, open the valve of the third pressure control line (L6-3) and expose the end of the first pressure control line (L6-1) to the external environment to lower the pressure of the reactor 100 than the pressure of the raw material storage unit 200 Keep it.

이와 같이 반응기 내부의 감압 유도에 의해 반응기 내부로 순차적으로 유입된 반응 용매 및 원료물질은 반응기 내에서 온도 및 pH가 조절되면서 교반되어 생성물을 생성하게 되고, 생성된 생성물은 제 1 생성물 배출 라인(L5)을 통해서 생성물 저장부(510)에 저장된다. 이때 생성물 저장부(500) 내를 감압 유도하여 압력차에 의해 생성 물질이 원활하게 생성물 저장부(510)에 저장되도록 하기 위해 압력 조절을 위한 매체를 수용하는 압력 조절 챔버(610), 진공 펌프(620), 제 1 압력 조절 라인(L6-1) 및 제 2 압력 조절 라인(L6-2)으로 생성물 저장부(500) 내의 감압을 유도할 수 있다. As such, the reaction solvent and raw materials sequentially introduced into the reactor by induction of the reduced pressure in the reactor are stirred while controlling the temperature and pH in the reactor to produce a product, and the resulting product is a first product discharge line (L5). Is stored in the product storage unit 510 through. At this time, the pressure control chamber 610, a vacuum pump for receiving a medium for pressure regulation in order to induce a reduced pressure in the product storage unit 500 to be smoothly stored in the product storage unit 510 by the pressure difference ( 620, the first pressure regulating line L6-1 and the second pressure regulating line L6-2 may induce a reduced pressure in the product reservoir 500.

도 3에서 보는 바와 같이 필터부(700)를 더 포함하는 경우 반응기(100)로부터 생성된 생성물은 제 2 생성물 배출 라인(L7-1)을 통해 필터부(700)로 유입되어 필터에서 필터링 된 후 제 3 생성물 배출 라인(L7-2)을 통해서 생성물질 저장부(500)로 이동되게 된다. As shown in FIG. 3, when the filter unit 700 further includes the product generated from the reactor 100 is introduced into the filter unit 700 through the second product discharge line L7-1 and then filtered by the filter. It is moved to the product storage unit 500 through the third product discharge line (L7-2).

이때 생성물 저장부(500) 내를 감압 유도하여 생성물을 필터부 및 생성물 저장부로 유출시키기 위해 압력 조절 챔버(610), 진공 펌프(620), 제 1 압력 조절 라인(L6-1) 및 제 2 압력 조절 라인(L6-2)으로 생성물 저장부(500) 내의 감압을 유도할 수 있다. At this time, the pressure regulating chamber 610, the vacuum pump 620, the first pressure regulating line L6-1, and the second pressure in order to induce a reduced pressure in the product reservoir 500 to discharge the product into the filter unit and the product reservoir. Control line L6-2 may induce reduced pressure in product reservoir 500.

도 2 및 도 4에서 보는 바와 같이 제 2 압력 조절 라인(L6-2) 및 제 3 압력 조절 라인(L6-3)은 3 방향밸브로 연결되어 사용될 수 있다. As shown in FIG. 2 and FIG. 4, the second pressure regulating line L6-2 and the third pressure regulating line L6-3 may be connected and used by a three-way valve.

도 1 내지 도 8에서 보는 바와 같이 본 발명에 의한 알루미늄 전구체 합성 시스템은 이와 같은 순차적인 단계 조절 및 단계 수행에 따른 밸브의 개폐를 통합적으로 조절하기 위한 별도의 제어 수단(미도시)을 더 포함할 수 있다. As shown in Figures 1 to 8, the aluminum precursor synthesis system according to the present invention may further include a separate control means (not shown) for integrally controlling the opening and closing of the valve according to such sequential step adjustment and step performance. Can be.

본 발명의 알루미늄 전구체 합성 시스템 및 이를 이용한 알루미늄 전구체 제조방법은 용매 공급부, 원료 물질 공급부 등이 반응기와 일체적으로 연결되고, 압력 제어부를 이용한 시스템 내부 압력 차이를 조절하여, 종래 취급이 어려웠던 원료물질, 반응 용매등을 체계적으로 공급 가능하게 되고, 이에 따라 결과적으로 유기 금속 형태의 알루미늄 전구체 잉크의 양산이 가능하도록 한다. In the aluminum precursor synthesis system of the present invention and a method for manufacturing an aluminum precursor using the same, a solvent supply unit, a raw material supply unit, etc. are integrally connected to the reactor, and by adjusting the pressure difference in the system using the pressure control unit, raw materials, which have been difficult to handle in the past, The reaction solvent and the like can be systematically supplied, and as a result, mass production of the aluminum precursor ink in the form of an organic metal is possible.

Claims (23)

반응기;Reactor; 상기 반응기 내로 원료 물질을 공급하는 원료물질 공급부;A raw material supply unit supplying a raw material into the reactor; 상기 반응기 내로 반응 용매를 공급하는 반응용매 공급부;A reaction solvent supply unit supplying a reaction solvent into the reactor; 상기 반응기 및 상기 반응용매 공급부로 비활성 가스를 공급하는 비활성 가스 공급부; An inert gas supply unit supplying an inert gas to the reactor and the reaction solvent supply unit; 상기 반응기로부터 생성되는 생성물이 유출되어 저장되는 생성물 저장부; 및A product storage unit in which the product generated from the reactor is discharged and stored; And 상기 반응기 및 상기 생성물 저장부와 연결되어 압력을 제어하는 압력 제어부;A pressure control unit connected to the reactor and the product storage unit to control pressure; 를 포함하는 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system comprising a. 제1항에 있어서,The method of claim 1, 원료물질 공급부는,Raw material supply unit, 밀폐된 하우징;Sealed housing; 상기 하우징 내에 수용되며, 원료물질을 저장하는 1개 또는 복수개의 원료물질 저장부; 및One or a plurality of raw material storage units accommodated in the housing and storing raw materials; And 상기 원료물질 저장부와 상기 반응기를 연결하며, 상기 원료물질을 상기 반응기로 공급하는 원료물질 공급라인; 을 포함하는 것인 A raw material supply line connecting the raw material storage unit and the reactor and supplying the raw material to the reactor; To include 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system. 제1항에 있어서,The method of claim 1, 반응용매 공급부는,Reaction solvent supply unit, 반응용매를 수용하는 반응용매 저장부; 및 A reaction solvent storage unit containing a reaction solvent; And 상기 반응용매를 상기 반응기로 공급하는 반응용매 공급라인;으로 구성되는 것인Consists of a reaction solvent supply line for supplying the reaction solvent to the reactor 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system. 제3항에 있어서,The method of claim 3, 상기 반응용매 공급라인은 상기 반응용매 저장부 내에서 말단이 반응 용매 내에 침지된 상태로 연결되는 것인 Wherein the reaction solvent supply line is connected in a state that the end is immersed in the reaction solvent in the reaction solvent reservoir 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system. 제1항에 있어서,The method of claim 1, 상기 비활성 가스 공급부는,The inert gas supply unit, 비활성 가스 저장부;Inert gas storage; 상기 비활성 가스 저장부와 상기 반응용매 저장부를 연결하여 상기 비활성 가스를 상기 반응용매 저장부로 공급하는 제 1 비활성 가스 공급라인; A first inert gas supply line connecting the inert gas storage unit and the reaction solvent storage unit to supply the inert gas to the reaction solvent storage unit; 상기 비활성 가스 저장부와 상기 반응기를 연결하여 상기 비활성 가스를 상기 반응기로 공급하는 제 2 비활성 가스 공급라인; 및A second inert gas supply line connecting the inert gas storage unit and the reactor to supply the inert gas to the reactor; And 상기 비활성 가스 저장부와 상기 원료물질 공급부를 연결하여 상기 비활성가스를 상기 원료물질 공급부로 공급하는 제 3 비활성가스 공급라인으로 구성되는 것인And a third inert gas supply line connecting the inert gas storage unit and the raw material supply unit to supply the inert gas to the raw material supply unit. 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system. 제5항에 있어서,The method of claim 5, 상기 제 1 비활성 가스 공급라인 말단은 반응 용매에 비접촉 상태로 연결되고, An end of the first inert gas supply line is connected to a reaction solvent in a non-contact state, 상기 제 2 비활성 가스 공급라인 말단은 반응기 내에 반응물에 비접촉 상태로 연결되고,The second inert gas supply line end is connected in a non-contact state to the reactants in the reactor, 상기 제 3 비활성 가스 공급라인 말단은 원료물질 공급부 내에 원료물질에 비접촉 상태로 연결되는 것인 End of the third inert gas supply line is connected to the raw material in a non-contact state in the raw material supply portion 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system. 제1항에 있어서,The method of claim 1, 생성물 저장부는Product reservoir 반응기로부터 유출되는 생성물을 수용하는 생성물 저장 챔버;A product storage chamber containing the product exiting the reactor; 상기 생성물 저장 챔버와 상기 반응기 사이를 연결하는 제 1 생성물 배출 라인; 으로 구성되는 것인 A first product discharge line connecting between said product storage chamber and said reactor; Consisting of 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system. 제7항에 있어서,The method of claim 7, wherein 상기 제 1 생성물 배출 라인은 상기 반응기 하부와 연결되거나, 반응기 상부로부터 인출되어 말단이 상기 반응기 내부의 생성물에 침전되는 것인 The first product outlet line is connected to the bottom of the reactor or is withdrawn from the top of the reactor so that the ends are precipitated in the product inside the reactor 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system. 제1항에 있어서,The method of claim 1, 압력 제어부는,Pressure control unit, 압력 조절 및 반응 시스템의 외부환경으로의 노출을 방지하기 위한 매체를 수용하는 압력 조절 챔버; A pressure regulation chamber containing a medium for preventing pressure regulation and exposure of the reaction system to the outside environment; 진공 펌프; A vacuum pump; 상기 압력 조절 챔버와 상기 진공 펌프를 연결시키는 제 1 압력 조절 라인;A first pressure regulation line connecting the pressure regulation chamber and the vacuum pump; 상기 생성물 저장 챔버와 상기 압력 제어부 사이를 연결하여 상기 생성물 저장 챔버 내의 압력을 조절하는 제 2 압력 조절 라인; 및 A second pressure regulating line connecting between the product storage chamber and the pressure control unit to regulate pressure in the product storage chamber; And 상기 반응기와 상기 압력 제어부 사이를 연결하여 상기 반응기 내의 압력을 조절하는 제 3 압력 조절 라인; 을 포함하는 것인 A third pressure regulating line connected between the reactor and the pressure controller to regulate pressure in the reactor; To include 알루미늄 전구체 합성 시스템. Aluminum precursor synthesis system. 제9항에 있어서,The method of claim 9, 상기 제 2 압력 조절 라인의 일 말단은 상기 압력 조절을 위한 매체 내에 침지된 상태로 연결되고, One end of the second pressure regulation line is connected in a state of being immersed in the medium for pressure regulation, 상기 제 3 압력 조절 라인의 일 말단은 상기 압력 조절을 위한 매체 내에 침지된 상태로 연결되는 것인 One end of the third pressure regulation line is connected in a state immersed in the medium for pressure regulation 알루미늄 전구체 합성 시스템. Aluminum precursor synthesis system. 제10항에 있어서,The method of claim 10, 상기 압력 조절을 위한 매체는 실리콘 오일인 것인 The medium for pressure control is silicone oil 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system. 제10항에 있어서, The method of claim 10, 상기 제 2 압력 조절 라인 및 제 3 압력 조절 라인은 3 방향밸브로 연결되는 것인 The second pressure regulating line and the third pressure regulating line are connected to the three-way valve 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system. 제1항에 있어서,The method of claim 1, 상기 반응기는,The reactor, 가열부;Heating section; 상기 반응기 내부 압력을 측정하기 위한 압력 측정부; 및A pressure measuring unit for measuring the pressure inside the reactor; And 상기 반응물의 pH를 측정하기 위한 pH 측정부; 를 포함하는 것인 PH measuring unit for measuring the pH of the reactant; To include 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system. 제1항에 있어서,The method of claim 1, 상기 반응기와 상기 생성물 저장부 사이에 상기 반응기로부터 생성되는 생성물을 필터링하는 필터부를 더 포함하는 것인 It further comprises a filter unit for filtering the product generated from the reactor between the reactor and the product storage unit 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system. 제14항에 있어서,The method of claim 14, 상기 반응기와 상기 필터부를 연결하는 제 2 생성물 배출 라인; 및 A second product discharge line connecting the reactor and the filter portion; And 상기 필터부와 상기 생성물 저장부를 연결하는 제 3 생성물 배출 라인;을 더 포함하는 것인 And a third product discharge line connecting the filter portion and the product reservoir. 알루미늄 전구체 합성 시스템.Aluminum precursor synthesis system. 비활성 가스를 반응기 내로 주입하는 단계;Injecting an inert gas into the reactor; 반응용매를 반응기로 주입하는 단계;Injecting a reaction solvent into the reactor; 원료물질을 반응기로 주입하는 단계;Injecting the raw material into the reactor; 반응기 내로 주입된 반응용매 및 원료물질을 교반하고, 반응온도를 제어하여 생성물을 생성하는 단계; 및 Stirring the reaction solvent and the raw material injected into the reactor, and controlling the reaction temperature to generate a product; And 상기 생성물을 생성물 저장부로 이송시키는 단계; 를 포함하는 Transferring the product to a product reservoir; Containing 제1항에 의한 알루미늄 전구체 합성 시스템을 이용한 알루미늄 전구체 제조방법.Method for producing an aluminum precursor using the aluminum precursor synthesis system according to claim 1. 제16항에 있어서,The method of claim 16, 상기 비활성 가스를 반응기 내로 주입하는 단계에서는,Injecting the inert gas into the reactor, 상기 압력제어부 및 제 3 압력 조절 라인에 의해 반응기 내부의 감압을 유도하여 상기 제 2 비활성 가스 공급라인으로 비활성 가스를 반응기 내로 주입하고, Induce the reduced pressure in the reactor by the pressure control unit and the third pressure control line to inert the inert gas into the reactor to the second inert gas supply line, 상기 반응기 내로 주입된 비활성 가스가 생성물 저장부 및 압력 제어부로 이동하도록 하는 것인 Inert gas injected into the reactor to move to the product reservoir and the pressure control unit 알루미늄 전구체 제조방법.Method for producing aluminum precursor. 제16항에 있어서,The method of claim 16, 상기 비활성 가스를 반응기 내로 주입하는 단계에서는,Injecting the inert gas into the reactor, 상기 반응기와 생성물 저장조를 연결하는 제 1 생성물 배출라인 및 생성물 저장조와 압력조절챔버를 연결하는 제 2 압력조절라인의 밸브를 열고, Opening the valve of the first product discharge line connecting the reactor and the product reservoir and the second pressure control line connecting the product reservoir and the pressure control chamber, 상기 압력조절챔버와 진공펌프를 연결하는 제 1 압력조절라인의 말단을 외부환경에 노출시켜 반응기 내부의 감압을 유도하여,By exposing the end of the first pressure control line connecting the pressure control chamber and the vacuum pump to the external environment to induce a reduced pressure inside the reactor, 상기 비활성 가스를 반응기에 공급하여 비활성 가스가 반응기, 생성물 저장부 및 압력제어부로 이동하도록 하는 것인 Supplying the inert gas to the reactor to move the inert gas to the reactor, the product reservoir and the pressure control unit 알루미늄 전구체 제조방법.Method for producing aluminum precursor. 제16항에 있어서,The method of claim 16, 상기 반응용매를 반응기 내로 주입하는 단계에서는,In the step of injecting the reaction solvent into the reactor, 상기 제 1 비활성 가스 공급 라인을 통하여 비활성 가스를 반응 용매 저장부로 주입하고, Inert gas is injected into the reaction solvent reservoir through the first inert gas supply line, 상기 주입된 비활성 가스의 공기압에 의해 상기 반응 용매가 상기 반응기로 주입되는 것인 The reaction solvent is injected into the reactor by the air pressure of the injected inert gas 알루미늄 전구체 제조방법.Method for producing aluminum precursor. 제19항에 있어서,The method of claim 19, 상기 반응용매를 반응기 내로 주입하는 단계에서는,In the step of injecting the reaction solvent into the reactor, 상기 압력제어부 및 제 3 압력 조절 라인에 의해 반응기 내부의 감압을 유도하는 것인 By inducing the pressure reduction inside the reactor by the pressure control unit and the third pressure control line 알루미늄 전구체 제조방법.Method for producing aluminum precursor. 제16항에 있어서,The method of claim 16, 상기 원료물질을 반응기로 주입하는 단계에서는,In the step of injecting the raw material into the reactor, 상기 압력제어부 및 제 3 압력 조절 라인에 의해 반응기 내부의 감압을 유도하여 상기 원료물질을 반응기로 주입하는 것인 Injecting the raw material into the reactor by inducing a reduced pressure in the reactor by the pressure control unit and the third pressure control line 알루미늄 전구체 제조방법.Method for producing aluminum precursor. 제16항에 있어서,The method of claim 16, 상기 원료물질을 반응기로 주입하는 단계에서는,In the step of injecting the raw material into the reactor, 상기 반응기와 압력조절챔버를 연결하는 제 3 압력조절라인의 밸브를 열어 압력조절챔버에 연결되어 있는 제 1 압력조절라인 말단을 외부환경에 노출시켜 반응기 내부의 감압을 유도하여,Opening the valve of the third pressure control line connecting the reactor and the pressure control chamber to expose the end of the first pressure control line connected to the pressure control chamber to the external environment to induce a reduced pressure inside the reactor, 상기 제 3 비활성 가스공급라인을 통해 원료물질 공급부에 비활성 가스를 공급하여 상기 원료물질을 반응기로 주입하는 것인Injecting the raw material into the reactor by supplying an inert gas to the raw material supply portion through the third inert gas supply line 알루미늄 전구체 제조방법.Method for producing aluminum precursor. 제16항에 있어서,The method of claim 16, 상기 생성물을 생성물 저장부로 이송시키는 단계에서는,In the step of transferring the product to the product reservoir, 상기 압력제어부 및 제 2 압력 조절 라인에 의해 반응기 및 생성물 저장부 내부의 감압을 유도하여 상기 생성물을 생성물 저장부로 이송하는 것인 Inducing pressure reduction in the reactor and the product storage unit by the pressure control unit and the second pressure control line to transfer the product to the product storage unit 알루미늄 전구체 제조방법.Method for producing aluminum precursor.
PCT/KR2017/003812 2016-04-07 2017-04-07 Aluminum precursor synthesization system and aluminum precursor preparation method using same Ceased WO2017176085A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020187032171A KR20180125601A (en) 2016-04-07 2017-04-07 Aluminum precursor synthesis system and method for producing aluminum precursor using the same

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR20160042891 2016-04-07
KR10-2016-0042891 2016-04-07

Publications (1)

Publication Number Publication Date
WO2017176085A1 true WO2017176085A1 (en) 2017-10-12

Family

ID=60000521

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/KR2017/003812 Ceased WO2017176085A1 (en) 2016-04-07 2017-04-07 Aluminum precursor synthesization system and aluminum precursor preparation method using same

Country Status (2)

Country Link
KR (1) KR20180125601A (en)
WO (1) WO2017176085A1 (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000051680A (en) * 1998-06-03 2000-02-22 Lion Corp Method for introducing granular material into liquid in reactor and method for producing alkylene oxide adduct using same
US20010038821A1 (en) * 1999-06-16 2001-11-08 Petrie Mark A. Stabilized aluminum hydride polymorphs, and associated methods of preparation and use
US20050180908A1 (en) * 2004-02-13 2005-08-18 Klingler Kerry M. Method of producing a chemical hydride
JP2008178823A (en) * 2007-01-25 2008-08-07 Dowa Technology Kk Plural fluids reaction method and plural fluids reaction apparatus using it
WO2012063991A1 (en) * 2010-11-11 2012-05-18 한국기계연구원 Method for manufacturing aluminum electrode using wetting process and aluminum electrode manufactured thereby

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000051680A (en) * 1998-06-03 2000-02-22 Lion Corp Method for introducing granular material into liquid in reactor and method for producing alkylene oxide adduct using same
US20010038821A1 (en) * 1999-06-16 2001-11-08 Petrie Mark A. Stabilized aluminum hydride polymorphs, and associated methods of preparation and use
US20050180908A1 (en) * 2004-02-13 2005-08-18 Klingler Kerry M. Method of producing a chemical hydride
JP2008178823A (en) * 2007-01-25 2008-08-07 Dowa Technology Kk Plural fluids reaction method and plural fluids reaction apparatus using it
WO2012063991A1 (en) * 2010-11-11 2012-05-18 한국기계연구원 Method for manufacturing aluminum electrode using wetting process and aluminum electrode manufactured thereby

Also Published As

Publication number Publication date
KR20180125601A (en) 2018-11-23

Similar Documents

Publication Publication Date Title
WO2021096326A1 (en) Method for forming thin film using surface protection material
WO2011129492A1 (en) Gas injection unit and a thin-film vapour-deposition device and method using the same
WO2015016412A1 (en) Mos2 thin film and method for manufacturing same
EP2630278A2 (en) Process for growing silicon carbide single crystal and device for the same
WO2013154250A1 (en) System for producing zinc oxide
WO2011043566A2 (en) Apparatus and method for processing substrate
WO2016167555A1 (en) Substrate processing apparatus
WO2021141324A1 (en) Method for forming thin film using surface protection material
WO2023177265A1 (en) Insulating liquid supply apparatus
WO2017176085A1 (en) Aluminum precursor synthesization system and aluminum precursor preparation method using same
WO2013176443A1 (en) Sublimation purification apparatus and method
WO2019066179A1 (en) Vapor deposition precursor having excellent thermal stability and reactivity and preparing method therefor
WO2014084557A1 (en) Silicon precursor compounds, and method for depositing thin film containing silicon using same
WO2023027505A1 (en) Secondary battery electrode slurry coating device, and electrode slurry coating method using same
WO2013191414A1 (en) Substrate processing apparatus
WO2024151153A1 (en) Method for producing lithium sulfide
WO2019199013A1 (en) Method for preparing lithium bis(fluorosulfonyl)imide salt
WO2015099334A1 (en) Apparatus and method for manufacturing silicon nitride powder
WO2018199665A1 (en) System and method for converting carbon dioxide using liquid-liquid interface and electron donor-acceptor catalyst
WO2024214936A1 (en) Method for producing lithium sulfide
WO2024091016A1 (en) Electrode slurry transfer system and electrode slurry temperature control method using same
WO2024219704A1 (en) Perovskite material mass production method
WO2021054632A1 (en) Compound for release agent and method for producing same
WO2021002590A1 (en) Gas supply device for substrate processing device, and substrate processing device
WO2021141438A1 (en) Chamber cleaning method

Legal Events

Date Code Title Description
NENP Non-entry into the national phase

Ref country code: DE

ENP Entry into the national phase

Ref document number: 20187032171

Country of ref document: KR

Kind code of ref document: A

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 17779385

Country of ref document: EP

Kind code of ref document: A1

122 Ep: pct application non-entry in european phase

Ref document number: 17779385

Country of ref document: EP

Kind code of ref document: A1