CN101628720A - Production process for pressuring and condensing trichlorosilane synthesized product - Google Patents
Production process for pressuring and condensing trichlorosilane synthesized product Download PDFInfo
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- CN101628720A CN101628720A CN200910065895A CN200910065895A CN101628720A CN 101628720 A CN101628720 A CN 101628720A CN 200910065895 A CN200910065895 A CN 200910065895A CN 200910065895 A CN200910065895 A CN 200910065895A CN 101628720 A CN101628720 A CN 101628720A
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- water cooler
- synthetic product
- tail gas
- hydrogen pressure
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Abstract
The invention discloses a production process for pressuring and condensing trichlorosilane synthesized products, which is implemented in a before-compression water cooler, a before-compression copious cooler, a hydrogen compressor, an after-compression copious cooler, a synthetic product storage tank and a tail gas dry-method recovery system. The production process comprises five processes of before-compression water cooling, before-compression copious cooling, hydrogen compressor pressuring, after-compression copious cooling and tail gas dry-method recovery. The invention effectively improves the condensation efficiency of the trichlorosilane synthesized product; after one-time pressuring and condensation, the recovery of chlorosilane is more than 90%; and then after being processed by the tail gas dry-method recovery system, the product is pressured and condensated once again, the condensation recovery of chlorosilane is more than 99%. The production process can reduce refrigerant consumption and extend the service cycle of hydrogen compressors.
Description
Technical field
The invention belongs to chemical production technical field, specially refer to a kind of production technique of pressuring and condensing trichlorosilane synthesized product.
Background technology
Trichlorosilane is an important intermediate of making silane coupling agent and other organosilicon product, still as the important raw and processed materials for preparing semiconductor grade polysilicon and solar-grade polysilicon.Along with international and domestic increase day by day to the polysilicon demand at present, the stable supply of high quality and large batch of trichlorosilane seems particularly important.
The synthetic normal pressure synthesis technology that adopts mostly of trichlorosilane, single device production capacity, raw material availability are lower, the system configuration imperfection, as do not have special-purpose liquid chlorine carburetion system, no liquid chlorine or hydrogenchloride dewatering unit, waste gas vent gas treatment recovery system imperfection etc.
The trichlorosilane synthetic product is meant the mixed gas that adopts after industrial silica fume and HCl synthesize, and this mixed gas is removed dust and comprised H outward
2, HCl, SiHCl
3, SiH
2Cl
2Or SiCl
4Deng, trichlorosilane synthetic product as referred to herein also can refer to this mixed gas.
After condensation separation, still have an appointment 10% chlorosilane (SiHCl of synthetic product
3+ SiCl
4) and a large amount of H
2Enter tail gas with HCl, efflux tail gas and adopt wet processing, not only consume alkali lye and water, and have new waste water and waste residue generation, environment is polluted, and cause the supplies consumption height such as chlorine, hydrogen and silica flour of unit product, product cost increases.Along with production-scale expansion, these problems will be more outstanding, even become the technical bottleneck of restriction enterprise development growth.
Patent CN101279734A discloses a kind of method of synthesizing trichlorosilane, and synthetic product is through water-cooled, pressurization and-40 ℃ of refrigerant deep coolings.Some chlorosilanes is not condensed though this patent has also adopted the mode of pressurization condensation.
Summary of the invention
For addressing the above problem, the invention provides a kind of production technique of pressuring and condensing trichlorosilane synthesized product, it is not high that this production technique efficiently solves the synthetic product condensation efficiency, and the problem that refrigerant consumption is too big has prolonged the turnaround of total system.
For achieving the above object, the present invention adopts following technical scheme:
The production technique of described pressuring and condensing trichlorosilane synthesized product is that water cooler, hydrogen pressure machine, the dark water cooler in compression back, sintetics storage tank and tail gas dry process recovery system are implemented deeply before watercooler, the compression before compression, production technique comprises deep cooling, hydrogen pressure machine pressurization before water-cooled before the compression, the compression, compression back deep cooling and tail gas dry process and reclaims five processes, and the five processes division is as follows:
Water-cooled before I, the compression
After trichlorosilane synthetic product watercooler bottom before compress enters from it portion come out to enter dark water cooler before the compression, watercooler adopts the ordinary cycle water cooling before the compression;
Deep cooling before II, the compression
The trichlorosilane synthetic product that watercooler comes out before compress enters the dark water cooler in compression back, the dark water cooler in compression back adopts-55～-30 ℃ of refrigerants to make refrigerant, the dark water cooler gas outlet temperature in control compression back is at-40～0 ℃, in the trichlorosilane synthetic product that is condensed as SiHCl
3, SiCl
4Be transported to the sintetics storage tank, the trichlorosilane synthetic product such as the H that are not condensed
2, HCl or part Si HCl
3, SiH
2Cl
2, SiCl
4Enter the hydrogen pressure machine;
III, the pressurization of hydrogen pressure machine
The trichlorosilane synthetic product that is not condensed that comes out from dark water cooler enters the compression of hydrogen pressure machine, and this moment, the intake pressure of hydrogen pressure machine was controlled at 0.01～0.1Mpa, is controlled at 0.3～0.8Mpa through the top hole pressure after the pressurization of hydrogen pressure machine;
IV, compression back deep cooling
Enter the dark water cooler in compression back and adopt-55～-30 ℃ of refrigerants to make refrigerant through the trichlorosilane synthetic product after the pressurization of hydrogen pressure machine, in the trichlorosilane synthetic product as SiHCl
3, SiCl
4Be condensed and enter the sintetics storage tank; A large amount of H in the trichlorosilane synthetic product
2, HCl or a spot of SiHCl
3, SiH
2Cl
2, SiCl
4The mixed gas that is not condensed enters the tail gas dry process recovery system;
V, tail gas dry process reclaim
Through containing SiHCl after the processing of tail gas dry process recovery system
3, SiH
2Cl
2, SiCl
4Mixed gas enter compression once more before dark water cooler carry out circular treatment, the H that contains after simultaneously the tail gas dry process recovery system being handled
2, HCl implements to reclaim.
Because adopt aforesaid technical scheme, the present invention has following superiority:
1, the present invention has effectively improved the condensation efficiency of trichlorosilane synthetic product, and after the condensation of once pressurizeing, the chlorosilane rate of recovery is more than 90%, and through the condensation of pressurizeing once more after the processing of tail gas dry process recovery system, the chlorosilane condensation rate of recovery reaches more than 99% again.
2, the present invention can reduce refrigerant consumption, prolongs hydrogen pressure machine life cycle.
Description of drawings
Fig. 1 is a production technique synoptic diagram of the present invention.
Embodiment
Explanation once more: trichlorosilane synthetic product of the present invention is meant the mixed gas that adopts after industrial silica fume and HCl synthesize, and this mixed gas is removed dust and comprised H outward
2, HCl, SiHCl
3, SiH
2Cl
2Or SiCl
4Deng.The trichlorosilane synthetic product of indication also can refer to this mixed gas in the literary composition.
In conjunction with Fig. 1, the production technique of pressuring and condensing trichlorosilane synthesized product of the present invention is that water cooler, hydrogen pressure machine, the dark water cooler in compression back, sintetics storage tank and tail gas dry process recovery system are implemented deeply before watercooler, the compression before compression, production technique comprises deep cooling, hydrogen pressure machine pressurization before water-cooled before the compression, the compression, compression back deep cooling and tail gas dry process and reclaims five processes, and the five processes division is as follows:
Water-cooled before the compression: after trichlorosilane synthetic product watercooler bottom before compress enters from it portion come out to enter dark water cooler before the compression, watercooler adopts the ordinary cycle water cooling before the compression.Water cooling has significantly reduced the mixed gas temperature through ordinary cycle, reduces back technology refrigerant consumption.
Deep cooling before the compression: the trichlorosilane synthetic product that watercooler comes out before compress enters the dark water cooler in compression back, the dark water cooler in compression back adopts-55～-30 ℃ of refrigerants to make refrigerant, refrigerant adopts freonll-11, the dark water cooler gas outlet temperature in control compression back is at-40～0 ℃, in the trichlorosilane synthetic product that is condensed as SiHCl
3, SiCl
4Be transported to the sintetics storage tank, the trichlorosilane synthetic product such as the H that are not condensed
2, HCl or part Si HCl
3, SiH
2Cl
2, SiCl
4Enter the hydrogen pressure machine.
The pressurization of hydrogen pressure machine: the trichlorosilane synthetic product that is not condensed that comes out from dark water cooler enters the compression of hydrogen pressure machine, and this moment, the intake pressure of hydrogen pressure machine was controlled at 0.01～0.1Mpa, is controlled at 0.3～0.8Mpa through the top hole pressure after the pressurization of hydrogen pressure machine;
Compression back deep cooling: enter the dark water cooler in compression back and adopt-55～-30 ℃ of refrigerants to make refrigerant through the trichlorosilane synthetic product after the pressurization of hydrogen pressure machine, in the trichlorosilane synthetic product as SiHCl
3, SiCl
4Be condensed and enter the sintetics storage tank; A large amount of H in the trichlorosilane synthetic product
2, HCl or a spot of SiHCl
3, SiH
2Cl
2, SiCl
4The mixed gas that is not condensed enters the tail gas dry process recovery system;
Tail gas dry process reclaims: will contain SiHCl after handling through the tail gas dry process recovery system
3, SiH
2Cl
2, SiCl
4Mixed gas enter compression once more before dark water cooler carry out circular treatment, through the condensation of pressurizeing once more, SiHCl
3, SiCl
4Get off Deng condensation.
Add for the first time after the condensation and still have a spot of chlorosilane not have condensation to get off in the mixed gas,, not only reduced the chlorosilane rate of recovery of synthetic product, and efflux drip washing and increased burden to environment if can not recycle.The mixed gas that contains small amounts of chlorine silane enters the preceding dark water cooler of compression through the condensation of pressurizeing once more, mixes the back condensation of pressurizeing with gas that watercooler before compress comes out, improved the chlorosilane organic efficiency greatly, it is reached more than 99%, thereby effectively reduced the refrigerant consumption, prolonged the total system turnaround.
The H that contains after simultaneously the tail gas dry process recovery system being handled
2, HCl implements to recycle.
The employed tail gas dry process recovery system of production technique of the present invention mainly is made of three activated carbon adsorbers of parallel connection, wherein the activated carbon adsorber of one deck layout is made adsorption treatment, the activated carbon adsorber that one deck is arranged is done cooling and is handled, the activated carbon adsorber that one deck is arranged is made manipulation of regeneration, sorbent material in each layer activated carbon adsorber state of living in can carry out periodicity automatically by time controller to be adjusted by turns, and other repeats no more.
Claims (1)
1, a kind of production technique of pressuring and condensing trichlorosilane synthesized product, it is characterized in that: this production technique is that water cooler, hydrogen pressure machine, the dark water cooler in compression back, sintetics storage tank and tail gas dry process recovery system are implemented deeply before watercooler, the compression before compression, production technique comprises deep cooling, hydrogen pressure machine pressurization before water-cooled before the compression, the compression, compression back deep cooling and tail gas dry process and reclaims five processes, and the five processes division is as follows:
Water-cooled before I, the compression
After trichlorosilane synthetic product watercooler bottom before compress enters from it portion come out to enter dark water cooler before the compression, watercooler adopts the ordinary cycle water cooling before the compression;
Deep cooling before II, the compression
The trichlorosilane synthetic product that watercooler comes out before compress enters the dark water cooler in compression back, the dark water cooler in compression back adopts-55～-30 ℃ of refrigerants to make refrigerant, the dark water cooler gas outlet temperature in control compression back is at-40～0 ℃, in the trichlorosilane synthetic product that is condensed as SiHCl
3, SiCl
4Be transported to the sintetics storage tank, the trichlorosilane synthetic product such as the H that are not condensed
2, HCl or part Si HCl
3, SiH
2Cl
2, SiCl
4Enter the hydrogen pressure machine;
III, the pressurization of hydrogen pressure machine
The trichlorosilane synthetic product that is not condensed that comes out from dark water cooler enters the compression of hydrogen pressure machine, and this moment, the intake pressure of hydrogen pressure machine was controlled at 0.01～0.1Mpa, is controlled at 0.3～0.8Mpa through the top hole pressure after the pressurization of hydrogen pressure machine;
IV, compression back deep cooling
Enter the dark water cooler in compression back and adopt-55～-30 ℃ of refrigerants to make refrigerant through the trichlorosilane synthetic product after the pressurization of hydrogen pressure machine, in the trichlorosilane synthetic product as SiHCl
3, SiCl
4Be condensed and enter the sintetics storage tank; A large amount of H in the trichlorosilane synthetic product
2, HCl or a spot of SiHCl
3, SiH
2Cl
2, SiCl
4The mixed gas that is not condensed enters the tail gas dry process recovery system;
V, tail gas dry process reclaim
Through containing SiHCl after the processing of tail gas dry process recovery system
3, SiH
2Cl
2, SiCl
4Mixed gas enter compression once more before dark water cooler carry out circular treatment, the H that contains after simultaneously the tail gas dry process recovery system being handled
2, HCl implements to reclaim.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910065895A CN101628720A (en) | 2009-08-24 | 2009-08-24 | Production process for pressuring and condensing trichlorosilane synthesized product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910065895A CN101628720A (en) | 2009-08-24 | 2009-08-24 | Production process for pressuring and condensing trichlorosilane synthesized product |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103599672A (en) * | 2013-11-08 | 2014-02-26 | 中国恩菲工程技术有限公司 | Method and system for treating polycrystalline silicon reducing tail gas |
| CN104310406A (en) * | 2014-10-11 | 2015-01-28 | 江西赛维Ldk太阳能多晶硅有限公司 | Recovery device and recovery method for trichlorosilane synthetic tail gas |
| US11612869B2 (en) | 2017-11-20 | 2023-03-28 | Tokuyama Corporation | Production method for trichlorosilane, and pipe |
-
2009
- 2009-08-24 CN CN200910065895A patent/CN101628720A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103599672A (en) * | 2013-11-08 | 2014-02-26 | 中国恩菲工程技术有限公司 | Method and system for treating polycrystalline silicon reducing tail gas |
| CN103599672B (en) * | 2013-11-08 | 2015-08-05 | 中国恩菲工程技术有限公司 | The processing method of polycrystalline silicon reduction exhaust and system |
| CN104310406A (en) * | 2014-10-11 | 2015-01-28 | 江西赛维Ldk太阳能多晶硅有限公司 | Recovery device and recovery method for trichlorosilane synthetic tail gas |
| CN104310406B (en) * | 2014-10-11 | 2016-06-22 | 江西赛维Ldk太阳能多晶硅有限公司 | The retracting device of technique of trichlorosilane synthetic tail gas and recovery method thereof |
| US11612869B2 (en) | 2017-11-20 | 2023-03-28 | Tokuyama Corporation | Production method for trichlorosilane, and pipe |
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