CN101638233B - Dry method recovery technique of trichlorosilane synthetic tail gas - Google Patents
Dry method recovery technique of trichlorosilane synthetic tail gas Download PDFInfo
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- CN101638233B CN101638233B CN2009100658941A CN200910065894A CN101638233B CN 101638233 B CN101638233 B CN 101638233B CN 2009100658941 A CN2009100658941 A CN 2009100658941A CN 200910065894 A CN200910065894 A CN 200910065894A CN 101638233 B CN101638233 B CN 101638233B
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Abstract
The invention discloses a dry recovery method for trichlorosilane synthetic tail gas, comprising: the synthetic tail gas is sent into a buffer tank, and the pressure of the buffer tank is 0.3-0.8MPa; an adsorption system comprises two adsorption towers which are connected with each other in parallel, wherein one of the two adsorption towers is in an adsorption state, and the other one is in a regeneration state; the two adsorption towers are respectively provided with an inlet control valve and an outlet control valve, and the adsorbent is active carbon; when the synthetic tail gas enters the adsorption tower in the adsorption state, the intensity of pressure in the tower is 0.3-0.8MPa, and the temperature therein is 20-80 DEG C; a great deal of chlorosilane is absorbed by the adsorption tower, the mixed gas of H2 and HCl is exhausted into an adsorption bag type filter and then enters into the buffer tank of the recovered gas after dust removing; one part of the tail gas is transmitted into a hydrogen chloride synthetic system, and the other part is conveyed into the adsorption tower in regeneration state; the temperature in the tower is 100-200 DEG C, and the pressure is 0.01-0.15MPa; the chlorosilane which is absorbed at high temperature is resolved, for regenerating the adsorbent, so that the trichlorosilane synthetic tail gas is recovered by a synthetic tail gas condensation system after being filtered by a regeneration bag type filter and dust removing.
Description
Technical field
The invention belongs to chemical technology field, specially refer to a kind of dry method recovery of technique of trichlorosilane synthetic tail gas.
Background technology
Trichlorosilane consumes a large amount of chlorine and hydrogen aborning, be a kind of good balance chlorine of chlor-alkali enterprise and the product of increasing economic efficiency, also be the important source material that is used for products such as manufacture order crystal silicon, polysilicon, be widely used in the every field of national defence, national economy and daily life.
The main method of trichlorosilane production is:
Si+3HCl=SiHCl
3+ H
2, reaction temperature about 300 ℃, after dedusting, pressurization condensation, still some on-condensible gas such as H
2, HCl or small amounts of chlorine silane.Owing to contain H in the on-condensible gas
2, both made employing-35 ℃ refrigerant deep cooling, but still contained trichlorosilane and silicon tetrachloride about 10%.
In tradition or present production technology, synthesis tail gas is adopted wet-treating, not only consume alkali lye and water, and have new waste water and waste residue and produce, 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.Some adopt the technology that dry method reclaims at present, mainly reclaim the hydrogen chloride in the tail gas, and hydrogen and small amounts of chlorine silane washing emptying are perhaps reclaimed hydrogen and hydrogen chloride separately, not only cause wastage of material, have also increased operation easier and trichlorosilane production cost.Simultaneously in order to reach environmental protection, to satisfy the requirement of national energy-saving and emission-reduction, the recycling of tail gas is become more and more important.
Patent CN101279734A has announced the method that a kind of technique of trichlorosilane synthetic tail gas dry method reclaims, but the H in this method
2Be merged in washing tail gas emptying, not only cause wastage of material, also increased the synthetic cost of trichlorosilane.
Patent CN101125276 hydrogen membrane separator separating hydrogen gas, the hydrogen of separating is as fuel or directly enter atmosphere, causes wastage of material and increases the trichlorosilane production cost.
Summary of the invention
For addressing the above problem, the invention provides a kind of dry method recovery of technique of trichlorosilane synthetic tail gas, this dry method recovery has solved the recycling problem of technique of trichlorosilane synthetic tail gas, makes the H in the tail gas
2, HCl returns the hydrogen chloride synthesis system after mix reclaiming, chlorosilane gas returns the pressuring and condensing trichlorosilane synthesized product system condensing and reclaims.
For achieving the above object, the present invention adopts following technical scheme:
The dry method recovery of described a kind of technique of trichlorosilane synthetic tail gas is that the condensed technique of trichlorosilane synthetic tail gas of pressurization is sent into surge tank, and the pressure that keeps surge tank is at 0.3～0.8Mpa; Adsorption system is made of two adsorption towers of parallel connection, wherein the adsorbent in adsorption tower is in adsorbed state, adsorbent in another adsorption tower is in reproduced state, and two adsorption towers are equipped with import and export by-pass valve control separately respectively, and adsorbent is active carbon; The synthesis tail gas that comes out from surge tank enters in this adsorption tower by the by-pass valve control that adsorbed state adsorption tower bottom is provided with, the pressure of pressure in the adsorption tower and surge tank is consistent and is all 0.3～0.8Mpa at this moment, temperature in the adsorption tower is controlled at 20～80 ℃, synthesis tail gas flows in adsorption tower from bottom to top, a large amount of chlorosilanes in the synthesis tail gas are adsorbed agent absorption, H
2Be discharged to the absorption bag filter from the gas vent by-pass valve control at adsorption tower top with the mist of HCl and filter, remove by filter to enter behind the dust and reclaim the gas buffer jar, the pressure that reclaims the gas buffer jar also remains on 0.3～0.8Mpa; Reclaim the H of gas buffer jar
2With the HCl mist, a part is transported to the hydrogen chloride synthesis system by by-pass valve control and pipeline, a part is transported to the absorption of regenerating in the adsorption tower that is in reproduced state in the adsorption system by by-pass valve control and pipeline, the adsorption tower temperature of reproduced state is controlled at 100～200 ℃, reduce tower internal pressure to 0.01～0.15MPa simultaneously, H
2Flow from top to bottom in adsorption tower with the mist of HCl, under the high-temperature low-pressure state, impel the chlorosilane that is adsorbed from adsorbent, to parse, thereby make adsorbent obtain regeneration, chlorosilane that parses and H
2, the HCl mist comes out to enter into the regeneration bag filter from regeneration adsorption tower bottom by-pass valve control and filters, reclaim by synthesis tail gas pressurization condenser system after removing by filter dust.
The dry method recovery of described a kind of technique of trichlorosilane synthetic tail gas, adsorbent state in two adsorption towers in parallel of its adsorption system can carry out periodicity by turns by the time control program, that is to say that the adsorption tower that is in reproduced state can carry out the transition to the adsorption tower of adsorbed state by lowering the temperature and boosting, this is because the regeneration technology after the adsorbent parsing of reproduced state adsorption tower is at high temperature, carry out under the low-pressure state, the adsorbents adsorb technology of adsorbed state adsorption tower is at low temperature, carry out under the high pressure conditions, the adsorption tower of reproduced state is carried out the transition to the adsorption tower of adsorbed state by lowering the temperature and boosting, the cooling temperature is controlled at 20～80 ℃, and boost pressure is controlled at 0.3～0.8Mpa.
Because adopt aforesaid technical scheme, the present invention has following superiority:
1, the present invention utilizes the characteristic of the synthetic material of trichlorosilane, the H in the synthesis tail gas
2, HCl mixes recovery, it is synthetic to be used for hydrogen chloride, and then returns the trichlorosilane synthesis system, makes material recycling, reduces the step and the energy resource consumption of reclaiming separately.
2, the present invention adopts the dry method recycling, can not produce waste water and waste residue, can not cause environmental pollution, has reduced the synthetic production cost of trichlorosilane.Automatically control by the time control program, reduce manual operation, reduced operation easier.
Description of drawings
Fig. 1 is that dry method of the present invention reclaims schematic diagram.
The specific embodiment
Specify embodiments of the invention in conjunction with Fig. 1.
The condensed technique of trichlorosilane synthetic tail gas that will pressurize is sent into surge tank, the pressure that keeps surge tank is at 0.3～0.8Mpa, then the gas of synthesis tail gas surge tank is sent into the adsorption tower that is in adsorbed state in the adsorption system, because through the condensed technique of trichlorosilane synthetic tail gas pressure of pressurization is 0.3～0.8Mpa, and the adsorption tower of adsorbed state also need carry out under 0.3～0.8Mpa state in the adsorption system, so enter the adsorption tower of adsorbed state after being kept at synthesis tail gas in the surge tank, can reduce step-down, boost operations step, reduce energy resource consumption simultaneously.
Synthesis tail gas is by control valve and pipeline, enters from the adsorption tower bottom of adsorbed state, and gas flows in adsorption tower from bottom to top, and at pressure 0.3～0.8Mpa, under 20～80 ℃ of conditions of temperature, the chlorosilane in the synthesis tail gas is adsorbed agent absorption, H
2Come out to enter the absorption bag filter from adsorption tower top with the mist of HCl and filter, go out to enter behind the dust and reclaim the gas buffer jar, gas buffer pressure tank 0.3～0.8Mpa is reclaimed in control, reclaims the H of gas buffer jar
2With the HCl mist, a part is transported to the hydrogen chloride synthesis system by by-pass valve control and pipeline, and a part is transported to the absorption of regenerating in the adsorption tower that is in reproduced state in the adsorption system by by-pass valve control and pipeline.Synthesis tail gas is handled through absorbing process, has reclaimed H wherein
2Return the trichlorosilane synthesis system with the HCl mist, make material recycling, reduce the step that reclaims separately, gas buffer pressure tank 0.3～0.8Mpa is reclaimed in control simultaneously, can make reclaim gas not consumes energy directly return in the adsorption tower of trichlorosilane synthesis system and reproduced state.
The adsorption tower of adsorbed state is after operation 6～12 hours, and the adsorbent chlorosilane in the adsorption tower reaches capacity, and enters regeneration technology automatically by the time control program.
A part reclaims the H in the gas buffer jar
2With the HCl mist, enter from the adsorption tower top of reproduced state, gas flows in adsorption tower from top to bottom, 100～200 ℃ of control temperature, under pressure 0.01～0.15MPa condition, the chlorosilane that is adsorbed parses from adsorbent, thereby makes adsorbent obtain regeneration, chlorosilane that parses and H
2, the HCl mist comes out to enter into the regeneration bag filter from regeneration adsorption tower bottom by-pass valve control and filters, reclaim by synthesis tail gas pressurization condenser system after removing by filter dust.Chlorosilane by in the pressurization condensation recovery synthesis tail gas has improved raw material availability.
The adsorption tower of reproduced state is after operation 6～12 hours, and the adsorbent chlorosilane in the adsorption tower is parsed fully, and adsorbent obtains regeneration, reduce adsorption tower temperature to 20～80 ℃ after, enter absorbing process automatically by the time control program.
Through the absorbing process and the regeneration technology periodic cycle of adsorption system, the chlorosilane in the synthesis tail gas is delivered to the pressurization condenser system and is obtained reclaiming H by after absorption, resolving like this
2Delivering to the hydrogen chloride synthesis system after being reclaimed simultaneously with the HCl mist obtains recycling, thereby make technique of trichlorosilane synthetic tail gas not produce waste water and waste residue, do not cause to obtain under the situation of environmental pollution recycling, greatly reduce the synthetic production cost of trichlorosilane simultaneously yet.
The time control program is meant sets 6～12 hour time interval, the adsorption tower of adsorption system carries out the periodicity of absorbing process and regeneration technology automatically and rotates, the adsorption tower that is to say adsorbed state is after 6～12 hours, originally gas enters from the adsorption tower bottom, come out from top, gas flows in adsorption tower from bottom to top, changing into gas enters from adsorption tower top, come out in the bottom, gas flows in adsorption tower from top to bottom, the adsorption tower temperature is elevated to 100～200 ℃ simultaneously, and pressure is reduced to 0.01～0.15MPa, thereby makes the adsorption tower of adsorbed state enter reproduced state automatically.After 6～12 hours of the adsorption tower of reproduced state, originally gas enters from adsorption tower top, come out from the bottom, gas flows in adsorption tower from top to bottom, changes into gas and enters from the adsorption tower bottom, comes out in top, gas flows in adsorption tower from bottom to top, reduce adsorption tower temperature to 20～80 ℃ simultaneously, rising pressure to 0.3～0.8Mpa, thus make the adsorption tower of reproduced state enter adsorbed state automatically.Two the adsorption tower that can ensure adsorption system like this moves continuously, and is in running order all the time, improves the utilization rate of whole system.
Claims (2)
1. the dry method recovery of a technique of trichlorosilane synthetic tail gas, it is characterized in that: this dry method recovery is that the condensed technique of trichlorosilane synthetic tail gas of pressurization is sent into surge tank, the pressure that keeps surge tank is at 0.3～0.8MPa; Adsorption system is made of two adsorption towers of parallel connection, wherein the adsorbent in adsorption tower is in adsorbed state, adsorbent in another adsorption tower is in reproduced state, and two adsorption towers are equipped with import and export by-pass valve control separately respectively, and adsorbent is active carbon; The synthesis tail gas that comes out from surge tank enters in this adsorption tower by the by-pass valve control that adsorbed state adsorption tower bottom is provided with, the pressure of pressure in the adsorption tower and surge tank is consistent and is all 0.3～0.8MPa at this moment, temperature in the adsorption tower is controlled at 20～80 ℃, synthesis tail gas flows in adsorption tower from bottom to top, a large amount of chlorosilanes in the synthesis tail gas are adsorbed agent absorption, H
2Be discharged to the absorption bag filter from the gas vent by-pass valve control at adsorption tower top with the mist of HCl and filter, remove by filter to enter behind the dust and reclaim the gas buffer jar, the pressure that reclaims the gas buffer jar also remains on 0.3～0.8MPa; Reclaim the H of gas buffer jar
2With the HCl mist, a part is transported to the hydrogen chloride synthesis system by by-pass valve control and pipeline, a part is transported to the absorption of regenerating in the adsorption tower that is in reproduced state in the adsorption system by by-pass valve control and pipeline, the adsorption tower temperature of reproduced state is controlled at 100～200 ℃, reduce tower internal pressure to 0.01～0.15MPa simultaneously, H
2Flow from top to bottom in adsorption tower with the mist of HCl, under the high-temperature low-pressure state, impel the chlorosilane that is adsorbed from adsorbent, to parse, thereby make adsorbent obtain regeneration, chlorosilane that parses and H
2, the HCl mist comes out to enter into the regeneration bag filter from regeneration adsorption tower bottom by-pass valve control and filters, reclaim by synthesis tail gas pressurization condenser system after removing by filter dust.
2. the dry method recovery of a kind of technique of trichlorosilane synthetic tail gas according to claim 1, it is characterized in that: the adsorbent state in two adsorption towers in parallel of adsorption system carries out periodicity by turns by the time control program, that is to say that the adsorption tower that is in reproduced state carries out the transition to the adsorption tower of adsorbed state by lowering the temperature and boosting, this is because the regeneration technology after the adsorbent parsing of reproduced state adsorption tower is at high temperature, carry out under the low-pressure state, the adsorbents adsorb technology of adsorbed state adsorption tower is at low temperature, carry out under the high pressure conditions, the adsorption tower of reproduced state is carried out the transition to the adsorption tower of adsorbed state by lowering the temperature and boosting, the cooling temperature is controlled at 20～80 ℃, and boost pressure is controlled at 0.3～0.8MPa.
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| CN2009100658941A CN101638233B (en) | 2009-08-24 | 2009-08-24 | Dry method recovery technique of trichlorosilane synthetic tail gas |
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| CN101638233B true CN101638233B (en) | 2011-06-15 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030312B (en) * | 2010-12-23 | 2011-09-14 | 江西嘉柏新材料有限公司 | Method for recovering hydrogen gas from trichlorosilane tail gas |
| CN102009955B (en) * | 2010-12-23 | 2011-09-14 | 江西嘉柏新材料有限公司 | Method for recovering hydrogen chloride from trichlorosilane tail gas |
| CN102580459A (en) * | 2012-03-02 | 2012-07-18 | 洛阳晶辉新能源科技有限公司 | Method for treating waste gas in production of polycrystalline silicon |
| CN102814095B (en) * | 2012-08-10 | 2015-03-18 | 中国恩菲工程技术有限公司 | Processing method of tail gas of trichlorosilane synthesis |
| KR101395275B1 (en) * | 2013-08-28 | 2014-05-16 | 한화케미칼 주식회사 | Purification method for off-gas and apparatus for purification of off-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 |
| CN109847731A (en) * | 2019-01-31 | 2019-06-07 | 内蒙古通威高纯晶硅有限公司 | A kind of reduction tail gas recycle activated carbon adsorber regeneration technology and regenerative system |
| CN110371985A (en) * | 2019-08-27 | 2019-10-25 | 天津中科拓新科技有限公司 | A kind of synthetic method of silicon tetrachloride |
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