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WO2005056475A1 - Procede pour produire du trichlorure de bore - Google Patents

Procede pour produire du trichlorure de bore Download PDF

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Publication number
WO2005056475A1
WO2005056475A1 PCT/EP2004/013935 EP2004013935W WO2005056475A1 WO 2005056475 A1 WO2005056475 A1 WO 2005056475A1 EP 2004013935 W EP2004013935 W EP 2004013935W WO 2005056475 A1 WO2005056475 A1 WO 2005056475A1
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WO
WIPO (PCT)
Prior art keywords
reactor
chlorine
boron
boron carbide
reaction
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/EP2004/013935
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German (de)
English (en)
Inventor
Hans-Josef Sterzel
Wilhelm Ruppel
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BASF SE
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BASF SE
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Filing date
Publication date
Application filed by BASF SE filed Critical BASF SE
Publication of WO2005056475A1 publication Critical patent/WO2005056475A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/06—Boron halogen compounds
    • C01B35/061—Halides

Definitions

  • the present invention relates to a method for producing boron trichloride.
  • it relates to a process for the production of high purity boron trichloride.
  • Boron trichloride is an important and industrially manufactured chemical. Boron trichloride is used, among other things, as a Lewis acid catalyst in various reactions catalyzed by Lewis acids in organic chemistry such as some polymerizations. However, further uses are those for the deposition of elemental boron, for example in the deposition of boron-containing layers by means of deposition from the gas phase (“chemical vapor deposition”, “CVD” for short) or in the production of inorganic boron-containing fibers. Boron trichloride is also used as an etchant in the production of semiconductor structures by plasma etching of aluminum or silicon.
  • BCI3 can be produced, for example, by reacting the elements, by reacting boron oxide or an alkali borate such as borax with chlorine in the presence of carbon or by re-halogenating boron trifluoride with aluminum trichloride.
  • the most common technical process for the production of boron trichloride is the reaction of boron carbide with chlorine, optionally in a borax melt.
  • British Patent GB 711 254 discloses a process for producing boron nitride by reacting boron trichloride with ammonia, in which boron trichloride is produced from boron carbide and chlorine at at least 300 ° C. in a first step.
  • British patent GB 971 943 teaches a process for the production of activated carbon by reacting boron carbide with chlorine at 630-790 ° C. in an electrically heated tubular reactor, in which the boron as boron trichloride is removed from the remaining highly porous carbon.
  • German patent application DE 1 957949 discloses a process for the production of boron halides such as boron trichloride from boron carbide and chlorine, in which borides of the 1, 2 and 3 main groups, in particular calcium or aluminum boride, are added as reaction accelerators.
  • boron trichloride takes place at a temperature of 900 - 1050 ° C and is fast enough to take place without external energy supply.
  • DE 2826747 A1 describes a process for the preparation of BCI3 by reacting boron carbide with chlorine in a fluidized bed in the presence of halides of the iron group, in particular nickel (II) chloride or cobalt (II) chloride, at temperatures around 700 ° C.
  • GB 2304 104 A teaches a process for the production of boron trichloride by reacting finely divided boron carbide with chlorine at a temperature of at least 800 ° C., the reaction being carried out in a vertical, 1 m quartz tube filled with boron carbide and flowing through with chlorine from top to bottom Length and 10 cm diameter is performed.
  • the boron carbide is mixed with a electrical resistance at the top of the bed is heated to the reaction temperature, then the reaction proceeds autothermally and the reaction zone migrates from top to bottom through the boron carbide bed.
  • the process according to the invention is characterized by circulating gas cooling, in which the gaseous reactor discharge is split up into a part to be cooled and returned to the reactor (the so-called “circulating gas”) and into a product stream before or after a circuit gas cooler arranged compressor back into the reactor recycled.
  • circulating gas the gaseous reactor discharge is split up into a part to be cooled and returned to the reactor
  • circuit gas cooler arranged compressor back into the reactor recycled.
  • the process according to the invention can be carried out continuously or semi-continuously.
  • a fully continuous reaction requires continuous addition of solid boron carbide and continuous removal of unreacted carbon. This is technically difficult, which is why boron trichloride production is usually carried out semi-continuously, ie chlorine flows through a reactor filled with a certain amount of boron until the boron carbide has reacted.
  • a reaction zone (a "hotspot") moves through the reactor, in which chlorine reacts with boron carbide, behind which the reacted boron carbide (ie essentially graphitic carbon) remains. Boron trichloride is discharged from the reactor.
  • the chlorine flow is switched off, the reactor with inert gas rinsed, cooled and the carbon residue replaced by fresh boron carbide.
  • chlorine breakthrough is to be avoided at all costs, generally at most 95% by weight, preferably at most 90% by weight and in a particularly preferred form at most 80% by weight, however, for economic reasons, generally at least 50% by weight, preferably at least at least 60% by weight and, in a particularly preferred form, at least 80% by weight of the boron carbide used.
  • the chlorine content of the immediate reactor product plays no or only a minor role (for example if a post-reactor or another method for separating chlorine is provided or if a pure product is not required), the boron carbide can also be completely converted.
  • a vertical tube reactor is usually used, which is usually made of quartz.
  • Other materials insofar as they are resistant to chlorine at the reaction temperature, and other known types of reactors for reacting gases with solids can in principle also be used, but in view of the reaction conditions, the simplest possible structure of the reactor is advantageous in most cases.
  • a typical and preferred reactor is a vertical quartz tube, which is provided with side connections for thermocouples, heating elements and the like as required, with a typical diameter of generally at least 2 cm, preferably at least 4 cm and in a particularly preferred form at least 10 cm and generally at most 150 cm, preferably at most 120 cm and in a particularly preferred form at most 100 cm and a typical height of generally at least 20 cm, preferably at least 40 cm and in in a particularly preferred form at least 60 cm and generally at most 10 m, preferably at most 6 m and in a particularly preferred form at most 4 m.
  • the lid and base are made with the necessary passages of reactor material or another suitable material.
  • Chlorine is introduced into the top or bottom of the reactor. It is also possible to introduce chlorine at various points in the reactor, for example at the top and at one or more points along the length of the reactor, but this makes the structure of the reactor more complex. In a vertical tube reactor, the hotspot normally moves from bottom to top regardless of the direction of flow of the chlorine.
  • the temperature in the reactor is generally set to a value of at least 700 ° C., preferably at least 800 ° C. and generally at most 1200 ° C., preferably at most 1100 ° C. and in a particularly preferred manner at most 1000 ° C.
  • the temperature can also be lower in the zone of the reactor in which unreacted carbon remains after passage through the hotspot.
  • the main task in adjusting the heat balance of this reactor is to maintain the desired temperature in the reactor, in particular in the unreacted part of the boron carbide bed, without radial gradients and at the same time to dissipate the heat of reaction generated in the hotspot so that the temperature range also is not left there if possible.
  • the volume ratio between the freshly supplied chlorine and the recirculated cooled cycle gas is set such that, considering the other parameters - in particular the temperature of the cycle gas after the cooler, the freshly supplied amount of chlorine, the heating power applied and the other heat loss from the reactor - the excess heat of reaction generated in the reactor is removed and the set temperature of the reactor is set.
  • a volume ratio of freshly supplied chlorine to cycle gas of at least 1: 0.1, preferably at least 1: 3 and in a particularly preferred form at least 1: 7 and generally of at most 1:30, preferably at most 1:15 and in a particularly preferred form 1:13.
  • the cycle gas is cooled in a cycle gas cooler.
  • a common gas cooler is used as the circulating gas cooler, which emits the heat to a cooling medium such as air or water.
  • a cooling medium such as air or water.
  • the temperature of the cycle gas after the cooler is adjusted in view of the other parameters - in particular the ratio of freshly supplied chlorine to cycle gas, the freshly supplied amount of chlorine, the heating power applied and the other heat loss from the reactor - in such a way that the excess heat of reaction generated in the reactor is discharged and the target temperature of the reactor is reached.
  • the cycle gas is returned to the reactor, this can be done either in a mixture with fresh chlorine or elsewhere in the reactor. In the interest of the simplest possible reactor construction, it is preferred to introduce the cooled cycle gas and the freshly used chlorine together into the reactor.
  • the reactor in particular the boron carbide used, must be brought to a sufficient reaction temperature.
  • the heat of reaction generated during the reaction will also not be sufficient to bring the reactor to the desired minimum reaction temperature everywhere, especially outside the zone in which the reaction is currently taking place, but possibly also there, especially along the outer wall of the reactor hold so that a certain heating output may be necessary despite the exothermic reaction.
  • the reactor is therefore provided with conventional heating means, such as gas burners, electrical heating elements or radiant heaters.
  • the heating power is set so that the excess heat of reaction generated in the reactor is dissipated and the target temperature of the reactor is reached.
  • a convenient and preferred method is heating by direct passage of electrical current through the boron carbide.
  • Boron carbide is a semiconductor.
  • Direct or alternating voltage can be used, preferably an alternating voltage with a frequency of generally at least 10 Hz, preferably at least 30 Hz and in particularly preferably at least 40 Hz and generally at most 200 Hz, preferably at most 100 Hz and in particular preferably used at most 60 Hz, but the frequency is relatively uncritical.
  • the voltage is chosen so high that the desired current flow is achieved.
  • a voltage of at least 5 V, preferably at least 10 V and in a particularly preferred form at least 20 V and generally at most 400 V, preferably at most 380 V and in a particularly preferred form at most 300 V is applied.
  • the electrical conductivity increases with increasing temperature. The current and thus the power consumption and the temperature increase in parallel, so that the temperature can be kept at the desired value in a simple manner by limiting the current strength.
  • a further advantage of heating through direct current passage is that the highly porous graphite residue remaining after the reaction has a higher conductivity, i.e. a lower electrical resistance than boron carbide, and therefore cools down, which saves energy and puts less strain on the reactor material.
  • An additional advantage of this type of heating is that in the reaction zone through the Reaction heat increased temperature, the electrical conductivity increases, so the resistance decreases and less electrical energy is supplied locally at constant current.
  • the heat supply regulates itself to a certain extent and the regulation is therefore very stable.
  • the current is fed into the boron carbide fill via electrodes.
  • Preferred is the use of graphite electrodes which are led into the reaction space at a suitable point via lateral connections on the reactor or passages in the reactor cover or reactor bottom. The position of the electrodes is chosen so that good current passage through the boron carbide fill is achieved.
  • a typical position for such electrodes is generally directly at the top and at the bottom of the boron carbide bed, preferably about 0.1 times the reactor diameter above the bottom end and below the top end of the boron carbide bed, and in a particularly preferred form about 0, 25 times the reactor diameter above the lower end and below the upper end of the boron carbide bed.
  • the electrodes are arranged 0.5 times the reactor diameter above the lower end and below the upper end of the boron carbide bed.
  • the electrodes above and below do not have to be arranged at the same distance from the respective end of the bed.
  • One or more electrodes can be used at each end of the bed.
  • the reactor is usually thermally insulated to a certain extent in order to reduce a possible temperature gradient between the core and the wall of the reactor and to save energy. In addition to cooling, other heat losses are unavoidable in practice, despite insulation, since no insulation can completely avoid heat losses. It is also advisable in many cases to provide an annular gap between the outer wall of the reactor and the insulation, ie not to allow the insulation to rest directly on the reactor, which naturally increases the other heat losses. This annular gap prevents reactions between the reactor material and the insulating material at the high temperature to be used, such as, for example, that between the mineral wool, which is often used as insulating material, and the preferred reactor material quartz, with the formation of low-strength silicates. Of course, if quartz wool is used as the insulating material, this does not matter.
  • An annular gap between the reactor and the insulating material can, however, be provided even if there is no fear of damage to the reactor due to contact with the insulating material in order to dissipate part of the heat of reaction. Due to the chimney effect - the rise of heated gases - some of the heat of reaction is in any case removed from the reactor as other heat loss. This other heat loss can also be deliberately brought about and regulated by a mechanical (optionally also variable in operation) setting of the annular gap and / or the passage of a gas flow through the annular gap, as long as in the reactor, also on it
  • a typical annular gap generally has a radius of at least 0.1 times, preferably at least 0.2 times and in a particularly preferred form at least 0.25 times and generally at most 3 times, preferably at most 2.5 times and in a particularly preferred form at most 2 times the reactor diameter on. If these measures are taken, the other measures for adjusting the heat balance of the reactor, such as heating output, ratio of freshly supplied chlorine to cycle gas, freshly supplied amount of chlorine and temperature of the cycle gas after the cooler must be adjusted accordingly.
  • Boron carbide is used.
  • any boron carbide can be used, preferably boron carbide of stoichiometry B 4 C or B 6 C is used, in a particularly preferred form B 4 C.
  • the boron carbide is used in a grain size which, on the one hand, leads to an acceptably low pressure loss across the reactor, but on the other hand shows a sufficiently high reaction speed and electrical conductivity of the bed.
  • boron carbide with a weight-average grain diameter (ie 50% by weight of the boron carbide passes through a sieve of the specified mesh size and 50% by weight is retained therefrom) of at least 0.1 mm, preferably at least 1 mm and in a particularly preferred manner at least 1.5 mm and in general at most 20 mm, preferably at most 15 mm and in a particularly preferred manner at most 10 mm.
  • the boron carbide fill is arranged in the reactor, as is customary in the prior art, for example on a sieve plate made of reactor material.
  • a post-reactor after the cycle gas-cooled reactor for the reaction of unreacted chlorine in the first reactor with boron carbide.
  • the post-reactor is operated in the same way as the cycle gas-cooled reactor, in particular in the same temperature range. It is designed on the basis of its intended use, in particular on the possible amounts of chlorine to be expected in view of the mode of operation of the first reactor. If it is only used for safety in special operating states of the first reactor, it can be designed to be smaller than the first reactor.
  • the carbon residue is removed from the reactor and fresh boron carbide is introduced.
  • a particularly elegant method of separating The air classification is the boron carbide from the specifically lighter carbon residue.
  • a gas stream of suitable speed through the reactor discharges the carbon residue and leaves the unreacted boron carbide in the reactor.
  • the gas flow is to be set as in the air sifting of materials of the given specific weights.
  • the carbon residue is collected using conventional methods, such as filters or a cyclone.
  • boron trichloride If particularly pure boron trichloride is to be produced, it is preferred to provide filters or other cleaning devices at suitable points in the system. This is state of the art. A filter in the circulating gas flow to remove entrained fine dust prevents the possible build-up of pressure loss in the reactor. Passing the boron trichloride produced over a further filter, for example an activated carbon bed, removes entrained metal chlorides such as FeCI 3 or AICI 3 , which often originate from impurities in the boron carbide used.
  • a further filter for example an activated carbon bed
  • boron trichloride Due to the water sensitivity of boron trichloride, it is advisable to dry the system before the start of the reaction and to pass the gases used into the system in at least a largely anhydrous form, since otherwise not only boric acid and boron oxide will precipitate in the system and can lead to blockages, but also hydrogen chloride occurs as an impurity in the product.
  • a water content of the gases used of at most 2 ppm by volume, preferably at most 1 ppm by volume, is tolerable. Drying is state of the art and is carried out, for example, by freezing out the water or using drying agents such as zeolites or phosphorus pentoxide.
  • Flushing nitrogen and chlorine are fed to the drying apparatus 1 via metering devices and dried there.
  • the chlorine - in this embodiment from below - is introduced into a first reactor 2 filled with boron carbide and directly heated by electrodes, and the boron trichloride produced leaves the reactor at the other end and is passed through the fine dust filter 3.
  • part of the boron trichloride stream is sucked in via the circulating gas pump 5, passed through the circulating gas cooler 4 and mixed at point a with the fresh chlorine and returned to the reactor.
  • the boron trichloride not recycled at point b is fed into the second reactor 6, which is also filled with boron carbide and is directly electrically heated. After passing through the reactor 6, the boron trichloride stream is passed through the filter 7. The pure boron trichloride obtained thereafter is liquefied by cooling and recovered. With a further stream of nitrogen, the contents of the reactors 2 and 6 or the filter 7 are discharged into the cyclone 8 if necessary.
  • Boron trichloride was produced using the experimental setup shown schematically in the figure.
  • the filter 3 consisted of a glass wash bottle filled with quartz wool.
  • the cooler 4 consisted of an air-cooled laboratory cooler made of glass.
  • a diaphragm vacuum pump was used as circulating gas pump 5.
  • the filter 7 consisted of a glass tube with a diameter of 2.5 cm, which was filled over a length of 25 cm with granular activated carbon (Sorbonorit ® 4 from Norit Nederland NV, grain diameter 4 mm).
  • the resistance of the boron carbide bulk decreased from approx. 2 k ⁇ at room temperature to approx. 10 ⁇ at 800 ° C.
  • the temperature gradient from the center of the reactor to the wall was 5 - 10 ° C.
  • the temperature control was practically without inertia.
  • the circulating gas pump 5 was put into operation and a circulating gas flow of 650 l / h was set. The nitrogen purge was ended and 70 l / h of chlorine were metered in.
  • the reaction zone forming in reactor 1 had a length of about 3-4 cm, its maximum temperature was 1020 ° C. The temperature of the returned Circulating gas flow was below 100 ° C.
  • the boron trichloride produced was liquefied in a cold trap cooled with dry ice.
  • the boron trichloride contained less than 10 ppm by weight of phosgene, 10 ppm by weight of chlorine, 45 ppm by weight of iron and 35 ppm by weight of aluminum. After the activated carbon filter, the concentrations of iron and aluminum were each about 10 ppb by weight.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

L'invention concerne un procédé pour produire du trichlorure de bore, selon lequel du carbure de bore est mis à réagir avec du chlore à une température de 700 à 1200 °C dans un réacteur, la chaleur de la réaction étant au moins partiellement évacuée par refroidissement d'une partie des rejets gazeux du réacteur et par leur remise en circulation dans le réacteur.
PCT/EP2004/013935 2003-12-10 2004-12-08 Procede pour produire du trichlorure de bore Ceased WO2005056475A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10358080.8 2003-12-10
DE2003158080 DE10358080A1 (de) 2003-12-10 2003-12-10 Verfahren zur Herstellung von Bortrichlorid

Publications (1)

Publication Number Publication Date
WO2005056475A1 true WO2005056475A1 (fr) 2005-06-23

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PCT/EP2004/013935 Ceased WO2005056475A1 (fr) 2003-12-10 2004-12-08 Procede pour produire du trichlorure de bore

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DE (1) DE10358080A1 (fr)
WO (1) WO2005056475A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103950949A (zh) * 2014-05-20 2014-07-30 方治文 高纯三溴化硼-11的制备方法
CN106957061A (zh) * 2017-05-25 2017-07-18 江西瑞合精细化工有限公司 一种低光气含量的三氯化硼生产装置及方法
WO2017221642A1 (fr) * 2016-06-23 2017-12-28 昭和電工株式会社 Procédé de production de trichlorure de bore.
CN112062134A (zh) * 2020-09-21 2020-12-11 齐齐哈尔大学 一种利用固相原料制备三氯化硼-11的方法
KR20210005268A (ko) * 2018-06-26 2021-01-13 쇼와 덴코 가부시키가이샤 삼염화붕소의 제조 방법
CN114162830A (zh) * 2021-12-31 2022-03-11 大连科利德光电子材料有限公司 电子级三氯化硼的制备方法及其所获得的三氯化硼

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2826747A1 (de) * 1978-06-19 1980-01-03 Hans Dr Kral Verfahren zur kontinuierlichen darstellung von borhalogeniden
GB2304104A (en) * 1995-08-12 1997-03-12 Epichem Ltd Process for producing boron trichloride

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2826747A1 (de) * 1978-06-19 1980-01-03 Hans Dr Kral Verfahren zur kontinuierlichen darstellung von borhalogeniden
GB2304104A (en) * 1995-08-12 1997-03-12 Epichem Ltd Process for producing boron trichloride

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103950949A (zh) * 2014-05-20 2014-07-30 方治文 高纯三溴化硼-11的制备方法
WO2017221642A1 (fr) * 2016-06-23 2017-12-28 昭和電工株式会社 Procédé de production de trichlorure de bore.
TWI643816B (zh) * 2016-06-23 2018-12-11 日商昭和電工股份有限公司 三氯化硼之製造方法
CN109195909A (zh) * 2016-06-23 2019-01-11 昭和电工株式会社 三氯化硼的制造方法
JPWO2017221642A1 (ja) * 2016-06-23 2019-04-11 昭和電工株式会社 三塩化ホウ素の製造方法
CN109195909B (zh) * 2016-06-23 2022-08-16 昭和电工株式会社 三氯化硼的制造方法
CN106957061A (zh) * 2017-05-25 2017-07-18 江西瑞合精细化工有限公司 一种低光气含量的三氯化硼生产装置及方法
JPWO2020003924A1 (ja) * 2018-06-26 2021-07-08 昭和電工株式会社 三塩化ホウ素の製造方法
KR20210005268A (ko) * 2018-06-26 2021-01-13 쇼와 덴코 가부시키가이샤 삼염화붕소의 제조 방법
EP3816108A4 (fr) * 2018-06-26 2021-09-22 Showa Denko K.K. Méthode de production de trichlorure de bore
JP7264164B2 (ja) 2018-06-26 2023-04-25 株式会社レゾナック 三塩化ホウ素の製造方法
KR102549707B1 (ko) 2018-06-26 2023-07-03 가부시끼가이샤 레조낙 삼염화붕소의 제조 방법
US11878912B2 (en) 2018-06-26 2024-01-23 Resonac Corporation Method of producing boron trichloride
CN112062134A (zh) * 2020-09-21 2020-12-11 齐齐哈尔大学 一种利用固相原料制备三氯化硼-11的方法
CN112062134B (zh) * 2020-09-21 2023-05-09 齐齐哈尔大学 一种利用固相原料制备三氯化硼-11的方法
CN114162830A (zh) * 2021-12-31 2022-03-11 大连科利德光电子材料有限公司 电子级三氯化硼的制备方法及其所获得的三氯化硼

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