CN100556507C - A kind of method for recovering tail gas of trichlorosilane production - Google Patents
A kind of method for recovering tail gas of trichlorosilane production Download PDFInfo
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- CN100556507C CN100556507C CNB2007100185811A CN200710018581A CN100556507C CN 100556507 C CN100556507 C CN 100556507C CN B2007100185811 A CNB2007100185811 A CN B2007100185811A CN 200710018581 A CN200710018581 A CN 200710018581A CN 100556507 C CN100556507 C CN 100556507C
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Abstract
The invention discloses a kind of method for recovering tail gas of trichlorosilane production, it is characterized in that, this method with the forming gas of fluidized-bed reactor after condensation, on-condensible gas (tail gas) enters hydrogen membrane separator separating hydrogen gas after sending into the compressor overcompression, the non-infiltration pneumatic transmission of hydrogen membrane separator goes into to reclaim in the condenser, after reclaiming the further condensation of condenser, obtain trichlorosilane, silicon tetrachloride, on-condensible gas is a hydrogen chloride, again return fluidized-bed reactor as raw material and use, trichlorosilane and silicon tetrachloride be the product for reclaiming then.Separated hydrogen can be used as fuel or is used to produce the raw material of other products, also can directly enter atmosphere.
Description
Technical field
The present invention relates to a kind of technology of chemical technology field, particularly a kind of method for recovering tail gas of trichlorosilane production.
Background technology
Trichlorosilane (HSiCl
3) be a kind of purposes organic silicon monomer very widely, be mainly used in the raw material of producing semiconductor silicon, monocrystalline silicon and polysilicon, be widely used in the every field of national defence, national economy and even people's daily life.In recent years, China is increasing to the demand of trichlorosilane.In that to build or plan to build the trichlorosilane device also more and more.But, each place in view of more and more higher to environmental requirement, in order to make trichlorosilane production reach environmental requirement, to satisfy the requirement of national energy-saving and emission-reduction, the recycling of tail gas is also become more and more important.
As everyone knows, produce in the trichlorosilane process at fluidized-bed reactor, forming gas comes out from fluidized-bed reactor, temperature has reached 250 ℃～350 ℃, through dedusting, step by step the cooling and condensation after, some on-condensible gas contains hydrogen chloride, hydrogen and trichlorosilane and silicon tetrachloride in this part gas.Common understanding is; boiling point is respectively 31.8 ℃ and 57.6 ℃ under the normal pressure of trichlorosilane and silicon tetrachloride; as long as can be cooled to be lower than its minimum boiling point theoretically can get off the whole condensations of trichlorosilane; but in fact because the existence of hydrogen is arranged in the mist; even be as cold as-30 ℃; all condensation is got off; this part contains have an appointment about 13% the trichlorosilane and the mist of silicon tetrachloride; traditional or at present in the existing manufacturing technique; this part has directly been sent to washing; this part gas is not further reclaimed (mainly is to reclaim trichlorosilane; silicon tetrachloride and hydrogen chloride); cause the consumption of raw materials height; uneconomical, also be unfavorable for environmental protection.
Summary of the invention
Defective or deficiency at above-mentioned prior art exists the objective of the invention is to, and a kind of method for recovering tail gas of trichlorosilane production is provided.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of method for recovering tail gas of trichlorosilane production, it is characterized in that, this method with the fluidized-bed reactor forming gas after condensation, on-condensible gas (being tail gas) is sent into compressor and is gone into hydrogen membrane separator separating hydrogen gas through overcompression is laggard, the non-infiltration pneumatic transmission of hydrogen membrane separator goes into to reclaim in the condenser, after reclaiming the further condensation of condenser, obtain trichlorosilane, silicon tetrachloride, on-condensible gas is a hydrogen chloride, hydrogen chloride wherein returns fluidized-bed reactor as raw material again and uses, and trichlorosilane and silicon tetrachloride be the product for reclaiming then.
The present invention utilizes the strong characteristics of hydrogen permeability, adopt compression, hydrogen membrane separator separating hydrogen gas and non-infiltration gas, make hydrogen to infiltrate through film easily, other gas then is difficult for infiltration this film (non-infiltration gas), thereby reach hydrogen is separated (infiltration gas) from mist purpose, the hydrogen of separating (infiltration gas) can be used as fuel or is used to produce the raw material of other products, also can directly enter atmosphere.Non-infiltration gas is through under again can be with trichlorosilane and silicon tetrachloride condensation after the condensation, and the hydrogen chloride in the on-condensible gas then returns use.
Description of drawings
Fig. 1 is the method for recovering tail gas of trichlorosilane production block diagram;
Fig. 2 is the production process block diagram;
The present invention is described in further detail below in conjunction with accompanying drawing.
The specific embodiment
Method of the present invention, the technology of existing fluidized-bed reactor being produced trichlorosilane adopts the direct evaporative condenser technology in fluorine Lyons through dedusting, forming gas, step by step after cooling and the condensation, some on-condensible gas overflows, therefore, this part gas must be reclaimed, and the hydrogen chloride of recovery returns use as raw material again; The trichlorosilane that reclaims is as product, and the hydrogen of recovery acts as a fuel or is used to produce the raw material of other products.
The applicant uses method for recovering tail gas of trichlorosilane production of the present invention (Fig. 1) first in production technology, this method is utilized the strong characteristics of hydrogen permeability, separate, recompress through overcompression, hydrogen one-level film, hydrogen secondary membrane separation process makes hydrogen to infiltrate through film easily hydrogen is separated from process tail gas.The purpose of separating hydrogen gas is exactly further to reclaim trichlorosilane and hydrogen chloride, improves total recovery.
The forming gas that the process fluidized-bed reactor comes out is after condensation, on-condensible gas (tail gas) enters hydrogen membrane separator (this hydrogen membrane separator provides for Dalian Chemical Physics Research Institute) after overcompression (0.65MPa A), the gas that penetrates in the hydrogen membrane separator is referred to as to permeate gas, i.e. hydrogen of Hui Shouing, purity can reach more than 98%; The gas that does not penetrate film is referred to as non-infiltration gas, i.e. mist such as hydrogen chloride and trichlorosilane.The non-infiltration gas of removing hydrogen reclaims trichlorosilane through reclaiming condenser again, to improve product yield; On-condensible gas then is back in the raw material system for hydrogen chloride.
Method for recovering tail gas of trichlorosilane production of the present invention is seen Fig. 1, and each thing stream number title, composition and operating parameter see Table 1.
Table 1: each thing stream number title, composition and operating parameter are as follows:
The production process that adopts method of the present invention is referring to accompanying drawing 2.In this technology, the raw material silica flour is transported to the former feed bin of silica flour by pipeline under protection of nitrogen gas.By star-like feeder the silica flour in the former feed bin is joined in the formula strength delivery pump of storehouse, silica flour is sent into the baking powder stove of monomer synthesizer continuously by pipeline, and in baking powder stove, carry out drying, send out that to dry by the fire the powder furnace temperature surely be 150 ℃ by storehouse formula strength delivery pump.
At the qualified silica flour of baking powder stove after the hot nitrogen oven dry, be transported to trichlorosilane large-scale fluidized bed reactor of the present invention bottom with the hydrogen chloride gas that is heated to 150 ℃.In the trichlorosilane fluidized-bed reactor, the control temperature is under 250 ℃～350 ℃ and 0.05MPa (G) pressure, and silica flour and hydrogen chloride carry out gas-solid phase reaction, generation trichlorosilane and silicon tetrachloride.More than reaction all is exothermic reactions.
Reaction emit heat adopt 220 ℃ conduction oil shifting out with reaction heat, after the conduction oil heat absorption, temperature is raised to 235 ℃, heat exchange takes place with conduction oil and water in this moment in waste heat boiler, can produce the steam of 1.0MPa, the synthesis reactor reaction temperature can be effectively controlled in conduction oil circulation like this, reaches safety, aim of stable operation.
Trichlorosilane that the reaction of trichlorosilane fluidized-bed reactor generates and silicon tetrachloride mist are earlier through cyclone separator and bag filter, wherein remaining silica flour is reclaimed, send into the condenser cooling again, condenser send tail gas washing tower with part tail gas, drain into the alert area by tail gas washing tower and carry out wastewater treatment or emptying, all the other most chlorosilanes are condensed into liquid.The chlorosilane mixture of gained is delivered to the monomer rectifying device and is separated, thereby obtains the trichlorosilane and the silicon tetrachloride product (more than 99.5%) of higher degree.
Reaction emit heat adopt 220 ℃～250 ℃ conduction oil shifting out with reaction heat, after the conduction oil heat absorption, temperature is raised to 235～265 ℃, heat exchange takes place with conduction oil and water in this moment in waste heat boiler, can produce the steam of 1.0MPa, the synthesis reactor reaction temperature can be effectively controlled in conduction oil circulation like this, reaches safety, aim of stable operation.
Characteristics of the present invention are: utilize the strong characteristics of hydrogen permeability, at first with hydrogen from exhaust system Separate, and then by condensation trichlorosilane and silicon tetrachloride condensation are got off, fixed gas is hydrogen chloride Gas is back to trichlorosilane fluidized bed reactor feedstocks system. Adopt the present invention can make trichlorosilane Production process in produce a certain amount of tail gas, by method for recovering tail gas of the present invention, can be complete Entirely reclaim tail gas, reach the effect of energy-saving and emission-reduction, satisfy environmental requirement. And trichlorosilane production is always received Rate reaches 92%, has reduced consumption of raw materials, remarkable in economical benefits.
Claims (3)
1. method for recovering tail gas of trichlorosilane production, it is characterized in that, this method is produced the condensed on-condensible gas of tail gas with fluidized-bed reactor and is sent into compressor and go into hydrogen membrane separator separating hydrogen gas through overcompression is laggard, the non-infiltration pneumatic transmission of hydrogen membrane separator goes into to reclaim in the condenser, after reclaiming the further condensation of condenser, obtain trichlorosilane, silicon tetrachloride and hydrogen chloride, hydrogen chloride wherein returns fluidized-bed reactor as raw material again and uses, and trichlorosilane and silicon tetrachloride be the product for reclaiming then.
2. the method for claim 1 is characterized in that, the outlet pressure of described compressor is 0.65MPa, to satisfy the requirement of hydrogen membrane separator.
3. the method for claim 1 is characterized in that, described non-infiltration gas is as cold as-35 ℃ through reclaiming condenser.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100185811A CN100556507C (en) | 2007-09-04 | 2007-09-04 | A kind of method for recovering tail gas of trichlorosilane production |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2007100185811A CN100556507C (en) | 2007-09-04 | 2007-09-04 | A kind of method for recovering tail gas of trichlorosilane production |
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| CN101125276A CN101125276A (en) | 2008-02-20 |
| CN100556507C true CN100556507C (en) | 2009-11-04 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101569817B (en) * | 2008-05-30 | 2011-06-15 | 中蓝晨光化工研究院有限公司 | Tail gas recycling method in trichlorosilane production |
| EP2233195A1 (en) * | 2009-03-27 | 2010-09-29 | Meridionale Impianti S.p.A. | System and method for recovering hydrogen from exhausted gas of epitaxial processes and other industrial processes |
| US8187361B2 (en) | 2009-07-02 | 2012-05-29 | America Air Liquide, Inc. | Effluent gas recovery system in polysilicon and silane plants |
| CN102100998B (en) * | 2009-12-21 | 2013-03-20 | 重庆大全新能源有限公司 | Method and device for processing trichlorosilane synthesis tail gas |
| CN104229802A (en) * | 2013-06-24 | 2014-12-24 | 潘龙祥 | Preparation method of polycrystalline silicon |
| CN104003402B (en) * | 2014-05-30 | 2016-08-24 | 中国恩菲工程技术有限公司 | The method of purification of trichlorosilane |
| CN105327600A (en) * | 2014-08-08 | 2016-02-17 | 新特能源股份有限公司 | Treating apparatus for chlorosilane-containing tail gas produced in polysilicon production process |
| CN107304050B (en) * | 2016-04-18 | 2019-07-23 | 新特能源股份有限公司 | Polycrystalline silicon reduction exhaust recovery method and recovery system |
| CN110947267A (en) * | 2018-09-27 | 2020-04-03 | 新特能源股份有限公司 | Gas-solid mixture dust removal system and dust removal method |
| CN109879289A (en) * | 2019-04-12 | 2019-06-14 | 四川永祥多晶硅有限公司 | A kind of low value silicon powder recycling system |
| CN114477093B (en) * | 2022-01-27 | 2023-09-12 | 巴彦淖尔聚光硅业有限公司 | Polycrystalline silicon reduction tail gas recovery system |
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Non-Patent Citations (1)
| Title |
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| 三氯氢硅合成尾气的综合回收. 朱骏业.世界有色金属，第6期. 1995 * |
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