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WO2017171690A1 - Procédé de production conjointe des nanopoudres de mono-oxyde de silicium et d'oxyde de zirconium et installation industrielle pour sa mise en oeuvre - Google Patents

Procédé de production conjointe des nanopoudres de mono-oxyde de silicium et d'oxyde de zirconium et installation industrielle pour sa mise en oeuvre Download PDF

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Publication number
WO2017171690A1
WO2017171690A1 PCT/UA2017/000031 UA2017000031W WO2017171690A1 WO 2017171690 A1 WO2017171690 A1 WO 2017171690A1 UA 2017000031 W UA2017000031 W UA 2017000031W WO 2017171690 A1 WO2017171690 A1 WO 2017171690A1
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WO
WIPO (PCT)
Prior art keywords
zirconium oxide
silicon monoxide
silicon
synthesis
nanopowder
Prior art date
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Ceased
Application number
PCT/UA2017/000031
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English (en)
Russian (ru)
Inventor
Андрей ЦЫБА
Александр КАРПЛЮК
Павел КУЗЕМА
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Publication of WO2017171690A1 publication Critical patent/WO2017171690A1/fr
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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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00—Other disintegrating devices or methods
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C01G25/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates

Definitions

  • the invention relates to the field of nanotechnology, namely the production of nanopowders, which are used as raw materials for the manufacture of semiconductor elements, various ceramics, flame retardant coatings, composite materials, catalysts and the like.
  • a known method for the joint production of nanopowders of silicon monoxide and zirconium oxide (publ. US N_ 4755365 (A), CO 1G 25/02), in which zircon and carbon-containing material that does not emit gas at a temperature that is below 1000 ° C, mixed in a certain percentage.
  • the resulting mixture is loaded into a furnace for the synthesis of zirconium oxide and silicon monoxide, in which a non-oxidizing medium and a temperature are maintained in the first stage in the temperature range from 1200 ° C to 1550 ° C and in the second stage from 1550 ° C to 2000 ° C.
  • a zirconium oxide nanopowder is simultaneously synthesized, which is sent to the product acceptance unit, where it is cooled and the silicon monoxide gas that is released.
  • a disadvantage of the known method is that a mixture of zircon and auxiliary material, which has insufficient dispersion and homogenization, is loaded into the synthesis furnace of zirconium oxide and silicon monoxide, which complicates the reaction between them, as a result of which the synthesis of zirconium oxide and silicon monoxide is carried out at elevated temperatures.
  • a known method for the joint production of nanopowders of silicon monoxide and zirconium oxide (publ. US N ° 5096685 (A), B01J 3/00, C01B 33/113, COIF P / 22, COIF 7/38, COIG 25 / O2), selected as the closest analogue in which silicon dioxide, which is bound to zircon, and silicon are mixed in a certain percentage, the resulting mixture is loaded into a synthesis furnace of silicon monoxide and zirconium oxide, in which a non-oxidizing medium and a temperature in the range from 1300 ° C to 2000 are maintained ° C.
  • silicon monoxide gas and zirconia nanopowder are simultaneously synthesized, which are sent to the product acceptance unit, where they are cooled.
  • silicon monoxide gas is deposited to form a silicon monoxide nanopowder.
  • the features by which zircon and silicon are mixed in a certain percentage ratio load the mixture into a synthesis furnace of silicon monoxide and zirconium oxide, in which a non-oxidizing environment and a temperature in the range from 1300 ° C are maintained up to 1600 ° C.
  • silicon monoxide gas and zirconia nanopowder are simultaneously synthesized, which are sent to the product acceptance unit, where they are cooled.
  • silicon monoxide gas is deposited to form a silicon monoxide nanopowder.
  • a disadvantage of the known method is that a mixture of zircon and zircon is loaded into a synthesis furnace of silicon monoxide and zirconium oxide. silicon, which has insufficient dispersion and homogenization, which complicates the reaction between them, as a result of which the synthesis of silicon monoxide and zirconium oxide is carried out at elevated temperatures.
  • the invention is based on the task of improving the known method, in which by technological changes to improve the dispersion and homogenization of a mixture of zircon and silicon, which is loaded into a furnace for the synthesis of silicon monoxide and zirconium oxide, to facilitate the reaction between them, resulting in the synthesis of silicon monoxide and zirconium oxide is carried out at low temperatures.
  • a well-known industrial complex for the joint production of nanopowders of silicon monoxide and zirconium oxide (publ. US JMb 4755365 (A), SOYU 25/02), which contains loaders of zircon and carbon-containing material, a mixer, a furnace for the synthesis of zirconium oxide and silicon monoxide, which linked to a non-oxidative environment maintenance system.
  • the output of this furnace is connected to the input of the product acceptance unit and configured to exit the gas of silicon monoxide.
  • a disadvantage of the known industrial complex is the insufficient conditions for dispersion and homogenization of a mixture of zircon and auxiliary material, which is loaded into a furnace for the synthesis of zirconium oxide and silicon monoxide, which complicates the reaction between them, as a result of which the synthesis of zirconium oxide and silicon monoxide is carried out at elevated temperatures.
  • a well-known industrial complex for the joint production of nanopowders of silicon monoxide and zirconium oxide (publ.
  • US 5096685 (A), B01J 3/00, C01B 33/113, C01F 1 1/22, C01F 7/38, CO 1G 25/02 ), selected as the closest analogue that contains silica and zircon loaders, and a silicon, a mixer, a silica and zirconia synthesis furnace that contains a silica container that is bound to zircon and silicon. This furnace is connected to a system for maintaining a non-oxidizing environment and its output is connected to the input of the product acceptance unit with cooling elements.
  • a disadvantage of the known industrial complex is the insufficient conditions for dispersion and homogenization of a mixture of zircon and silicon, which is loaded into a synthesis furnace of silicon monoxide and zirconium oxide, which complicates the reaction between them, as a result of which the synthesis of silicon monoxide and zirconium oxide is carried out at temperatures.
  • the invention is based on the task of improving a well-known industrial complex, in which, through structural changes, improve the conditions for dispersion and homogenization of a mixture of zircon and silicon, which is loaded into a synthesis furnace of silicon monoxide and zirconium oxide, than to facilitate the reaction between them, resulting in synthesis silicon monoxide and zirconium oxide to conduct at low temperatures.
  • the resulting mixture is loaded into a synthesis furnace of silicon monoxide and zirconium oxide in which a non-oxidizing medium is maintained, a temperature in the range of 1300 ° C.
  • the mixer output is connected to the input of the resonance vortex mill, the output of which is connected to the input of the ultrasonic coagulator, the output of which is connected to the input of the cyclo and whose output is connected to an input of the synthesis furnace silicon monoxide and zirconium oxide, which is made with the possibility of mixing the particles reaktsiynnoy mixture.
  • the Set of the main features of the proposed method provides a solution to the problem.
  • the used resonance vortex mill grinds zircon particles from 50 ⁇ m to 150 ⁇ m in size and silicon particles from 1 mm in size up to 3 mm, to the size of units of micrometers, intensively mixes them, which ensures a high degree of dispersion and homogenization and, consequently, an increase in the surface of the phase distribution of these reagents. This improves the conditions for starting the synthesis.
  • the crushed particles Immediately after exiting this mill, the crushed particles have increased energy activity, which further contributes to the homogenization of the mixture components and their aggregation into structured agglomerates in an ultrasonic coagulator.
  • An additional positive effect of the creation of these agglomerates is the appearance of stable physical contact between a significant part of the components of the mixture of zircon and silicon, which contributes to the active synthesis of silicon monoxide and zirconium oxide at low temperatures. Compared with both analogues, the maximum synthesis temperature is reduced by 400 ° C. Also an additional positive effect in comparison with the prototype is a significant reduction in time for the manufacture of a similar volume of products. In the prototype, operations with containers take hours, and for the proposed method, the time from loading the input components to the manufacture of products from them is about half an hour.
  • FIG. 1 shows a block diagram of an industrial complex for the joint production of nanopowders of silicon monoxide and zirconium oxide.
  • FIG. 2 schematically shows a synthesis furnace of silicon monoxide and zirconium oxide.
  • the industrial complex for the joint production of nanopowders of silicon monoxide and zirconium oxide contains a loader I zircon and a silicon loader 2, which are connected to the mixer 3.
  • the mixer 3 is connected in series with a resonance vortex mill 4, an ultrasonic coagulator 5, a cyclone 6 and a furnace 7 for the synthesis of silicon monoxide and zirconium oxide, which is connected to the product acceptance unit 8, which contains cooling elements .
  • the furnace 7 includes a housing 9 with a heating shell, which, as an option, is installed obliquely and connected with the device 10 for input components and the device
  • the housing 9 is made with the possibility of its rotation and is connected with a drive, which is not shown in the figure.
  • the cavity of the housing 9 contains elements for mixing the reaction mixture.
  • the figure does not show the loading hopper on the device 10, which is connected to the lock chamber, heating elements, which are located in the device 1 1, as well as a system for maintaining a non-oxidizing environment, which is connected with the cavity of the housing 9.
  • the geometric dimensions of the furnace 7 are calculated according to the technical task for it productivity.
  • the input components from the zircon loader 1 and the silicon loader 2 are fed into the mixer 3, from which the resulting mixture enters the resonance vortex mill 4 and is intensively crushed by cavitation forces.
  • the crushed particles of the mixture which have not yet managed to substantially oxidize their surface, enter the ultrasonic coagulator 5 and form structured agglomerates under the influence of ultrasonic vibrations of a certain frequency. They are collected using cyclone 6 and fed into the loading hopper and the lock chamber of the device 10, through which they enter the furnace 7 for the synthesis of silicon monoxide and zirconium oxide.
  • Support synthesis temperature in the range from 1300 ° C to 1600 ° C, depending on the task regarding the size of the nanoparticles of the product and its other parameters.
  • the structured agglomerates are constantly mixed by rotating the housing 9 or, alternatively, by elements for mixing.
  • a forevacuum and / or flow argon is maintained using a non-oxidative environment maintenance system.
  • the movement of gases in the cavity of the housing 9 is carried out under the action of gas, which is pumped, and / or as a result of their evacuation by a vacuum pump of a system for maintaining a non-oxidizing environment.
  • the vacuum pump pumps out the synthesized silicon monoxide gas from the cavity of the casing 9, which enters the device 1 1, heated to a temperature of about 1200 ° C, which prevents solid silicon monoxide from sticking to its walls.
  • silicon monoxide gas is deposited to form a silicon monoxide nanopowder.
  • the structure of these particles is amorphous in the form of fluffy agglomerates.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Composite Materials (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Structural Engineering (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Silicon Compounds (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

Le procédé de production conjointe des nanopoudres de mono-oxyde de silicium et d'oxyde de zirconium ainsi que l'installation industrielle pour sa mise en oeuvre concernent le domaine de la production de nano-matériaux qui s'utilisent en tant que matière de base pour la production d'éléments à semi-conducteurs, de différentes types de céramique, de surfaces réfractaires, de matériaux composites, de catalyseurs, etc. Le zirconium et le silicium sont mélangés, acheminés dans un broyeur à tourbillons (4) par résonance, un coagulateur à ultrasons (5), un cyclone (6) et un four de synthèse de monoxyde de silicium et d'oxyde de zirconium (7). La synthèse conjointe est menée dans un milieu non oxydant à une température dans la gamme de 1300°C à 1600°C. Les produits sont refroidis, à la suite de quoi le gaz de monoxyde de silicium se dépose de manière à former une nanopoudre de monoxyde de silicium. La nanopoudre d'oxyde de zirconium est obtenue sous forme de produit solide de cette synthèse.
PCT/UA2017/000031 2016-03-29 2017-03-28 Procédé de production conjointe des nanopoudres de mono-oxyde de silicium et d'oxyde de zirconium et installation industrielle pour sa mise en oeuvre Ceased WO2017171690A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
UAA201603256A UA114572C2 (uk) 2016-03-29 2016-03-29 Спосіб сумісного виробництва нанопорошків монооксиду кремнію і оксиду цирконію та промисловий комплекс для його реалізації
UAA201603256 2016-03-29

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WO2017171690A1 true WO2017171690A1 (fr) 2017-10-05

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115141024A (zh) * 2022-05-06 2022-10-04 大连海恒纳米科技有限公司 用于预防耐火混凝土开裂的材料制备方法及材料

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5815021A (ja) * 1981-07-15 1983-01-28 Showa Denko Kk β−ＳｉＣとＺｒＯ↓２を同時に製造する方法
US5096685A (en) * 1985-07-27 1992-03-17 Kawasaki Steel Corporation Method for manufacturing fine-grained silicon monoxide
RU2058939C1 (ru) * 1991-06-26 1996-04-27 Всероссийский научно-исследовательский институт химической технологии Способ получения порошка диоксида циркония для изготовления керамики
JP2003119017A (ja) * 2001-10-11 2003-04-23 Denki Kagaku Kogyo Kk 低級酸化ケイ素粉末の製造方法
CN1733611A (zh) * 2005-08-12 2006-02-15 安泰科技股份有限公司 一种二氧化锆纳米粉体材料的制造方法
CN103599736A (zh) * 2013-11-11 2014-02-26 东华大学 一种磁性介孔二氧化锆复合物微球的制备方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5815021A (ja) * 1981-07-15 1983-01-28 Showa Denko Kk β−ＳｉＣとＺｒＯ↓２を同時に製造する方法
US5096685A (en) * 1985-07-27 1992-03-17 Kawasaki Steel Corporation Method for manufacturing fine-grained silicon monoxide
RU2058939C1 (ru) * 1991-06-26 1996-04-27 Всероссийский научно-исследовательский институт химической технологии Способ получения порошка диоксида циркония для изготовления керамики
JP2003119017A (ja) * 2001-10-11 2003-04-23 Denki Kagaku Kogyo Kk 低級酸化ケイ素粉末の製造方法
CN1733611A (zh) * 2005-08-12 2006-02-15 安泰科技股份有限公司 一种二氧化锆纳米粉体材料的制造方法
CN103599736A (zh) * 2013-11-11 2014-02-26 东华大学 一种磁性介孔二氧化锆复合物微球的制备方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115141024A (zh) * 2022-05-06 2022-10-04 大连海恒纳米科技有限公司 用于预防耐火混凝土开裂的材料制备方法及材料

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