CN101486465B - Production method of refined trichlorosilane - Google Patents
Production method of refined trichlorosilane Download PDFInfo
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- CN101486465B CN101486465B CN2009100762979A CN200910076297A CN101486465B CN 101486465 B CN101486465 B CN 101486465B CN 2009100762979 A CN2009100762979 A CN 2009100762979A CN 200910076297 A CN200910076297 A CN 200910076297A CN 101486465 B CN101486465 B CN 101486465B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to a method for producing purified trichlorosilane. The method comprises the following steps: (1) a preliminary tower is added at the rectification section of industrial trichlorosilane; (2) a heater is added in front of the preliminary tower to pre-heat feed; (3) the interior of the preliminary tower, the trichlorosilane tower and a silicon tetrachloride tower adopt the form of the compound of filler and trays; (4) silicon tetrachloride can come from the gas phase side at the lower part of the silicon tetrachloride tower; (5) the trichlorosilane tower and the silicon tetrachloride tower can be integrated into a tower or a double-effect distillation method is adopted; (6) a cleaning tower is added behind a dust catcher and in front of a condenser in a cooling section; (7) the cleaning tower adopts base waste heat to drive a lithium bromide set to generate cold water for cooling; (8) heat integration is carried out to synthesized heat so as to save energy and recycle heat; and (9) during the super pure distillation and purification process of trichlorosilane, 3 to 8 rectification towers and adsorption towers or complex distillation towers are adopted. The method has the advantages of low investment, low energy consumption, high purity of the target product, trichlorosilane, and the like.
Description
Technical field
The present invention relates to a kind of production method and rectifying separation purification techniques of Chemicals, particularly relate to a kind of production method of refined trichlorosilane.
Background technology
Trichlorosilane is the important source material of producing solar level and microelectronics level polysilicon, also be the important intermediate of synthesizing organo-silicon simultaneously, be used for the synthetic of organosilane and alkyl, aryl and organo-functional group chlorosilane, it is monomer the most basic in the organo silane coupling agent, also be the raw material of producing semiconductor silicon, silicon single crystal, also can be used for making silicone compounds.Along with China's rapid development of economy, the especially fast development of industries such as fine chemistry industry, organosilicon industry, electronic product, optical-fibre communications is for the production of trichlorosilane and the exploitation of derived product provide the huge market space and opportunity.But owing to be subjected to the restriction that foreign technology blocks, the production technology of domestic trichlorosilane enterprise is perfect inadequately, causes the quality of product and output can't satisfy the requirement of manufacture order crystal silicon and the demand in market.
The present technological process of production both domestic and external is roughly as follows: hydrogenchloride and dried silicon powder are reacted in synthetic furnace and are generated trichlorosilane and silicon tetrachloride mixture, mixture reclaims remaining silica flour through cyclonic separator and sack cleaner, deliver to condenser system then, the chlorosilane mixture that condensation is got off is delivered to distillation system and is isolated trichlorosilane and silicon tetrachloride, and uncooled tail gas is delivered to exhaust gas recovery system.
The oven dry of silica flour and sack cleaner reclaim silica flour a large amount of heats need be provided in the production technique, fail fully to recycle and produce a large amount of heats in the building-up reactions, have caused great energy expenditure and waste.Cooling workshop section, mixture is directly delivered to condenser through dedusting after, and owing to containing material such as aluminum chloride in the mixture, the easy crystallization blocking pipe of these matter-poles has caused very big inconvenience to the operation of condenser, needs parking maintenance often.For the Chinese patent CN 1693192A of rectifying workshop section single tower purify trichlorosilane is proposed, Chinese patent CN 1010455362A proposes double tower and separates trichlorosilane, can not effectively separate trichlorosilane, impurity such as low-boiling-point substance and boron, phosphorus can not effectively be removed, and product index is also unstable.
The present invention be directed to the characteristics and the requirement of trichlorosilane production technique, trichlorosilane technology is improved, propose a kind of trichlorosilane production and make with extra care the method for purifying, solve in the trichlorosilane production and invest greatly energy consumption height, the problem that separation efficiency is low.
Summary of the invention
The present invention provides a kind of production method of refined trichlorosilane for solving the deficiencies in the prior art.Use method provided by the invention, have the investment low, energy consumption is low and the separation purity height of target product trichlorosilane and rate of recovery advantages of higher.
A kind of production method of refined trichlorosilane, hydrogenchloride and dried silicon powder are reacted mixtures such as generating trichlorosilane and silicon tetrachloride in synthetic furnace, mixture reclaims remaining silica flour through dedusting, deliver to condenser system then, the chlorosilane mixture that condensation is got off is delivered to distillation system and is obtained the technical grade trichlorosilane, obtain refined trichlorosilane through refining purification workshop section afterwards, its feature is as follows:
(1) to process of cooling optimization, increase the washing tower device: as Fig. 1, mixture reclaims remaining silica flour through cyclonic separator and sack cleaner, delivers to washing tower and removes aluminum chloride, and then enter condenser system.
(2) synthetic heat is carried out the integrated and energy-conservation utilization of heat: as Fig. 3, building-up reactions produces a large amount of heats in the synthetic furnace, thermal oil or other heat-eliminating mediums flow out through synthetic furnace and pass through moisture eliminator respectively, collector, waste heat boiler, cooling then, but the dry silica flour of cooling heat heat drier, add heat trap and collect silica flour, the heating waste heat boiler produces steam thermal energy for system applies, cooled thermal oil is transported in the thermal oil collector, synthetic furnace is sent in heating through interchanger again, the circulation of thermal oil realizes the recycle of synthetic heat, saves cost greatly, reduces energy consumption.
(3) rectifying workshop section is optimized, adopt following method: as Fig. 4, chlorosilane mixture heater via under the condensation of condensation workshop section is preheating to 45～60 ℃ and enters pre-tower, pre-tower opening for feed is located at the tower middle part, impurity such as cat head extraction low-boiling-point substance, the mixture that obtains at the bottom of the tower after the preliminary purification is sent into the trichlorosilane tower, trichlorosilane tower opening for feed is arranged on the tower middle part, trichlorosilane mixture after the cat head extraction is purified, the mixture that obtains at the bottom of the tower is delivered to the silicon tetrachloride tower again, silicon tetrachloride tower opening for feed is arranged on the tower middle part, cat head extraction trichlorosilane and silicon tetrachloride are circulated to rectifying workshop section feed chute, remaining raffinate is provided with gas phase side in silicon tetrachloride tower bottom in addition and adopts a mouthful extraction silicon tetrachloride at the bottom of the tower.
(4) increase the refining purification workshop section of trichlorosilane: make with extra care the associating rectifying tower device that adopts 3～8 rectifying tower and adsorption tower or complexing in the purification process at trichlorosilane, working pressure is at 0.1～0.6MPa, and temperature is controlled at 30～120 ℃.3～8 rectifying tower are tray columns, and column plate is 40～120, or the inner packing tower that filler is housed, and the filler virtual height is 10～50 meters, or both combinations.As Fig. 5, the trichlorosilane mixture that obtains in the industry rectifying is delivered to refining purification workshop section, take off impurity such as the high and low thing that boils through 3～8 rectifying tower essences, process adsorption tower or complexing rectifying tower further remove impurity cats head such as boron, phosphorus, arsenic and obtain the high purity refined trichlorosilane then.Impurity such as extraction boron, phosphorus, arsenic at the bottom of adsorption tower or the complexing rectifying Tata, they can be located at the front or the back of 3～8 rectifying tower.
Pre-tower of the present invention, trichlorosilane tower, inner filler and the column plate compound form of adopting of silicon tetrachloride tower, filler pattern and volume and column plate pattern and the number of plies are calculated according to actual process and are determined, material can remove the impurity that balances each other through packing layer, can remove the non-impurity that balances each other through column plate.
Washing tower working pressure of the present invention is at 0.1～0.6MPa, and temperature is controlled at 30 ℃～120 ℃, and opening for feed is arranged on the tower middle part, and the mixture after the separation enters condenser from the cat head extraction, isolates solid substances such as aluminum chloride at the bottom of the tower.Increase washing tower auxiliary facility lithiumbromide unit in addition, as Fig. 2, the lithiumbromide unit utilizes bottom end warm water's heat energy to produce refrigerants such as cold water, feeds overhead condenser, because technical process needs a large amount of cold water as refrigerant, the present invention can save the cost and the energy greatly.
Trichlorosilane tower of the present invention and silicon tetrachloride tower can integrated towers, cat head extraction trichlorosilane, and gas phase side is adopted silicon tetrachloride at the bottom of the tower.Perhaps adopt the double-effect rectification technology, the double-effect rectification technology is with silicon tetrachloride column overhead steam-heated cal(l)andria trichlorosilane tower or with trichlorosilane column overhead steam-heated cal(l)andria silicon tetrachloride tower.Adopt any technology all can save cost greatly, reduce energy consumption.
The selected sorbent material of adsorption tower of the present invention is an inorganic acids, and the mixture of sequestrant (polyalcohols with aromatic nucleus).
The selected complexing agent of complexing rectifying tower of the present invention is nitrogen, phosphorus, the arsenic that contains V family in the periodic table of elements, the oxygen of IV family, phosphorus, the compound of the iron of VII family, chlorine element.
The invention has the advantages that by the reasonably optimizing design, rectification process is done technological improvement, improved the purity of rectification efficiency and product greatly, wherein foreign matter content such as boron, phosphorus is less than 10ppt, and flow process of the present invention is simple simultaneously, the turndown ratio height.The present invention has saved cost greatly reasonably to energy recycle in addition, has reduced energy consumption, has favorable economic benefit and social benefit.
Description of drawings
Fig. 1 is bosher's segment process synoptic diagram of the present invention.
Fig. 2 is a lithiumbromide unit process schematic representation of the present invention.
Fig. 3 is a synthetic gas integrated utilization process schematic representation of the present invention.
Fig. 4 is a rectifying of the present invention workshop section process schematic representation.
Fig. 5 is the associating rectifying tower device that adopts a plurality of rectifying tower, adsorption tower and complexing.
Wherein: 1. sack cleaner; 2. washing tower; 3. a water cooler; 4. two water coolers; 5. low-temperature water heating groove; 6. lithiumbromide unit; 7. condenser 8. thermal oil collectors; 9. interchanger; 10. synthesis gas reaction stove; 11. moisture eliminator; 12. silica flour collector; 13. waste heat boiler 14. well heaters; 15. pre-tower; 16. trichlorosilane tower; 17. silicon tetrachloride tower; 18～22. first to the 5th rectifying tower; 23. adsorption tower; 24. complexing rectifying tower.
Embodiment
A kind of production method of refined trichlorosilane, hydrogenchloride and dried silicon powder are reacted mixtures such as generating trichlorosilane and silicon tetrachloride in synthetic furnace, mixture reclaims remaining silica flour through dedusting, deliver to condenser system then, the chlorosilane mixture that condensation is got off is delivered to distillation system and is obtained the technical grade trichlorosilane, obtain highly purified refined trichlorosilane through refining purification workshop section afterwards, its feature is as follows:
(1) to process of cooling optimization, increase the washing tower device: as Fig. 1, mixture reclaims remaining silica flour through cyclonic separator and sack cleaner, delivers to washing tower and removes solid substances such as aluminum chloride, and then enter condenser system.
(2) synthetic heat is carried out the integrated and energy-conservation utilization of heat: as Fig. 3, building-up reactions produces a large amount of heats in the synthetic furnace, thermal oil or other heat-eliminating mediums flow out through synthetic furnace and pass through moisture eliminator respectively, collector, waste heat boiler, cooling then, but the dry silica flour of cooling heat heat drier, add heat trap and collect silica flour, the heating waste heat boiler produces steam thermal energy for system applies, cooled thermal oil is transported in the thermal oil collector, synthetic furnace is sent in heating through interchanger again, the circulation of thermal oil realizes the recycle of synthetic heat, saves cost greatly, reduces energy consumption.
(3) rectifying workshop section is optimized, adopt following method: as Fig. 4, chlorosilane mixture heater via under the condensation of condensation workshop section is preheating to 45～60 ℃ and enters pre-tower, pre-tower opening for feed is located at the tower middle part, impurity such as cat head extraction low-boiling-point substance, the mixture that obtains at the bottom of the tower after the preliminary purification is sent into the trichlorosilane tower, trichlorosilane tower opening for feed is arranged on the tower middle part, trichlorosilane mixture after the cat head extraction is purified, the mixture that obtains at the bottom of the tower is delivered to the silicon tetrachloride tower again, silicon tetrachloride tower opening for feed is arranged on the tower middle part, cat head extraction trichlorosilane and silicon tetrachloride are circulated to rectifying workshop section feed chute, remaining raffinate is provided with gas phase side in silicon tetrachloride tower bottom in addition and adopts a mouthful extraction silicon tetrachloride at the bottom of the tower.
(4) increase the refining purification workshop section of trichlorosilane: make with extra care the associating rectifying tower device that adopts 3～8 rectifying tower and adsorption tower or complexing in the purification process at trichlorosilane, working pressure is at 0.1～0.6MPa, and temperature is controlled at 30～120 ℃.3～8 rectifying tower are tray columns, and column plate is 40～120, or the inner packing tower that filler is housed, and the filler virtual height is 10～50 meters, or both combinations.As Fig. 5, the trichlorosilane mixture that obtains in the industry rectifying is delivered to refining purification workshop section, take off impurity such as the high and low thing that boils through 3～8 rectifying tower essences, process adsorption tower or complexing rectifying tower further remove impurity cats head such as boron, phosphorus, arsenic and obtain highly purified refined trichlorosilane then.Impurity such as extraction boron, phosphorus, arsenic at the bottom of adsorption tower or the complexing rectifying Tata, they can be located at the front or the back of 3～8 rectifying tower.
Pre-tower of the present invention, trichlorosilane tower, inner filler and the column plate compound form of adopting of silicon tetrachloride tower, filler pattern and volume and column plate pattern and the number of plies are calculated according to actual process and are determined, material can remove the impurity that balances each other through packing layer, can remove the non-impurity that balances each other through column plate.
Washing tower working pressure of the present invention is at 0.1～0.6MPa, and temperature is controlled at 30 ℃～120 ℃, and opening for feed is arranged on the tower middle part, and the mixture after the separation enters condenser from the cat head extraction, isolates solid substances such as aluminum chloride at the bottom of the tower.Increase washing tower auxiliary facility lithiumbromide unit in addition, as Fig. 2, the lithiumbromide unit utilizes bottom end warm water's heat energy to produce refrigerants such as cold water, feeds overhead condenser, because technical process needs a large amount of cold water as refrigerant, the present invention can save the cost and the energy greatly.
Trichlorosilane tower of the present invention and silicon tetrachloride tower can integrated towers, cat head extraction trichlorosilane, and gas phase side is adopted silicon tetrachloride at the bottom of the tower.Perhaps adopt the double-effect rectification technology, the double-effect rectification technology is with silicon tetrachloride column overhead steam-heated cal(l)andria trichlorosilane tower or with trichlorosilane column overhead steam-heated cal(l)andria silicon tetrachloride tower.Adopt any technology all can save cost greatly, reduce energy consumption.
Claims (5)
1. the production method of a refined trichlorosilane, hydrogenchloride and dried silicon powder are reacted mixtures such as generating trichlorosilane and silicon tetrachloride in synthetic furnace, mixture reclaims remaining silica flour through dedusting, deliver to condenser system then, the chlorosilane mixture that condensation is got off is delivered to distillation system and is obtained the technical grade trichlorosilane, obtain refined trichlorosilane through refining purification workshop section afterwards, it is characterized in that:
Workshop section increases pre-tower apparatus in the rectifying of technical grade trichlorosilane;
Before pre-tower, increase well heater and carry out preheating feeding in raw material;
Pre-tower, trichlorosilane tower, inner filler and the column plate compound form of adopting of silicon tetrachloride tower;
Silicon tetrachloride is adopted from the gas phase side of silicon tetrachloride tower bottom;
In cooling workshop section, increase the washing tower device before the condenser after the fly-ash separator;
The dry silica flour of the heat that utilizes thermal oil or other heat-eliminating mediums to take out of perhaps adds heat trap, perhaps heats waste heat boiler and produces steam thermal energy;
Make with extra care purify trichlorosilane: make with extra care at trichlorosilane and adopt 3～8 rectifying tower and adsorption tower in the purification workshop section.
2. according to the production method of the described refined trichlorosilane of claim 1, it is characterized in that: trichlorosilane tower and silicon tetrachloride tower are integrated into a tower: cat head distillates the trichlorosilane product, and tower bottom gas phase side is adopted the silicon tetrachloride product;
Perhaps adopt double-effect distillation method: with reboiler at the bottom of the silicon tetrachloride column overhead hot gas heating trichlorosilane Tata, or with reboiler at the bottom of the trichlorosilane column overhead steam-heated cal(l)andria silicon tetrachloride Tata.
3. according to the production method of the described refined trichlorosilane of claim 1, it is characterized in that: adopt end temperature waste heat to drive the lithiumbromide unit for washing tower and provide cold water to cat head.
4. according to the production method of the described refined trichlorosilane of claim 1, it is characterized in that: 3～8 rectifying tower are tray columns, and column plate is 40～120.
5. according to the production method of the described refined trichlorosilane of claim 1, it is characterized in that: 3～8 rectifying tower are packing towers, and the filler virtual height is 10～50 meters.
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780958B (en) * | 2010-03-30 | 2011-08-10 | 中国天辰工程有限公司 | Method for rectifying trichlorosilane and silicon tetrachloride |
| CN101966993B (en) * | 2010-09-30 | 2012-03-14 | 河南尚宇新能源股份有限公司 | Method for recycling waste silicon powder in production process of trichlorosilane |
| CN102058992B (en) * | 2010-11-13 | 2013-02-13 | 天津大学 | Clapboard adsorption device and method for removing boron impurities in chlorosilane system |
| CN102764613A (en) * | 2011-05-06 | 2012-11-07 | 北京先锋创新科技发展有限公司 | Reaction heat recovery and wet-method cooling dedusting processing technology |
| CN102642834B (en) * | 2012-05-10 | 2013-10-30 | 雅安永旺硅业有限公司 | Method adopting trichlorosilane and dichlorosilane mixed raw materials to produce polycrystalline silicon |
| CN103073002A (en) * | 2013-01-09 | 2013-05-01 | 天津大学 | Water-free type condensation and reboiling system and method in trichlorosilane distillation process |
| CN103435044B (en) * | 2013-07-19 | 2016-04-20 | 新特能源股份有限公司 | A kind of method of chlorosilane in purifies and separates polysilicon tail gas |
| CN108502889A (en) * | 2018-06-14 | 2018-09-07 | 四川瑞能硅材料有限公司 | The separation of polysilicon cold hydrogenation product and purifying plant and method |
| CN109607547B (en) * | 2018-11-21 | 2019-12-10 | 亚洲硅业（青海）有限公司 | Method for preparing high-purity chlorosilane |
| CN109908621A (en) * | 2019-04-12 | 2019-06-21 | 四川永祥多晶硅有限公司 | Slurry separates preposition transportation system and method |
| CN110156026B (en) * | 2019-04-26 | 2020-09-04 | 新疆大全新能源股份有限公司 | Purification process of polycrystalline silicon raw material |
| CN113401907B (en) * | 2020-03-16 | 2023-03-07 | 新疆新特晶体硅高科技有限公司 | Method and device for purifying and separating silicon tetrachloride in polycrystalline silicon synthesis |
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Application publication date: 20090722 Assignee: HEBEI HUADA SCIENCE & TECHNOLOGY CO., LTD. Assignor: Beijing Xianfeng Innovation and Technology Development Co., Ltd. Contract record no.: 2012990000654 Denomination of invention: Production method of refined trichlorosilane Granted publication date: 20110601 License type: Exclusive License Record date: 20120907 |
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