CN102100998A - Method and device for processing trichlorosilane synthesis tail gas - Google Patents
Method and device for processing trichlorosilane synthesis tail gas Download PDFInfo
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- CN102100998A CN102100998A CN2009102605811A CN200910260581A CN102100998A CN 102100998 A CN102100998 A CN 102100998A CN 2009102605811 A CN2009102605811 A CN 2009102605811A CN 200910260581 A CN200910260581 A CN 200910260581A CN 102100998 A CN102100998 A CN 102100998A
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Abstract
The invention provides a method for processing trichlorosilane synthesis tail gas, which comprises the following steps of: absorbing synthesis tail gas generated by preparing trichlorosilane by using chlorosilane to obtain chlorosilane absorption liquid, wherein the synthesis tail gas comprises HCL, SiHCl3, SiCl4, H2, silicon dust and high-boiling substance dust; heating the chlorosilane absorption liquid to the temperature of between 90 and 150 DEG C; and recovering a gas mixture and a solid mixture which are obtained by heating the chlorosilane absorption liquid respectively. The invention also provides a device for processing the trichlorosilane synthesis tail gas, which comprises a heating device, wherein the heating device comprises a shell with a heating jacket; and a feeding hole, a gas discharge hole and a solid discharge hole are formed on the shell. By the method and the device for processing the trichlorosilane synthesis tail gas, HCl, SiHCL3, SiCl4, H2, silicon dust and high-boiling substances in the chlorosilane absorption liquid processed by a wet method are recovered, raw materials are saved, and the production cost is reduced.
Description
Technical field
The present invention relates to the processing method of synthesis tail gas, be specifically related to a kind of processing method and equipment of technique of trichlorosilane synthetic tail gas.
Background technology
Trichlorosilane (SiHCl
3) be a kind of widely used organic silicon monomer, be the raw material of making solar level and electronic-grade polycrystalline silicon and manufacturing semiconductor grade monocrystalline silicon, also be simultaneously the synthetic basic monomer of multiple organosilicon.Along with progress of science and technology, sciemtifec and technical sphere fast developments such as fine chemistry industry, new forms of energy, photoelectricity communication, demand to silicon and various siliceous products is increasing, especially is the favor that product that raw material or intermediate product make more and more is subjected to current silicon industry with the trichlorosilane.
Industrial silicon Si after trichlorosilane is pulverized by process and anhydrous hydrogen chloride HCl carry out gas-solid phase reaction and obtain in fluidized-bed reactor.Main reaction is:
Si+3HCl→SiHCl
3+H
2↑
Main side reaction is:
Si+4HCl→SiCl
4+2H
2↑
Because the synthetic reaction of described trichlorosilane is exothermic reaction, and temperature is 280 ℃～300 ℃, so product is a gaseous mixture, comprising: hydrogen H
2, hydrogen chloride HCl, trichlorosilane SiHCl
3, silicon tetrachloride SiCl
4, silica soot and high-boiling components dust, the composition of high-boiling components dust is the solid particle of other side reaction except that silica soot well known to those skilled in the art, as metallic particles etc.After the reaction, described gaseous mixture is fed condensing tower, the SiHCl in the described gaseous mixture
3, SiCl
4Be condensed into liquid, other a spot of SiHCl
3, SiCl
4And a large amount of H
2, HCl and Si and high-boiling components dust be not condensed into liquid, uncooled gas is the synthesis tail gas of trichlorosilane.
Use the described synthesis tail gas of wet-treating in the prior art earlier, so-called wet method is used the described synthesis tail gas of liquid chlorosilane drip washing exactly, absorbs HCl, SiHCl in the described synthesis tail gas
3, SiCl
4And a spot of H
2, settle solids silica soot and high-boiling components dust obtain the chlorosilane absorption liquid, more described chlorosilane absorption liquid are fed in the hydrolysis tower, use in the alkali treatment method and HCl, SiHCl in the described chlorosilane absorption liquid
3, SiCl
4, discharge described solid silicon dust and high-boiling components dust.
Each component in the synthesis tail gas all has very high recycle value, in the prior art, just use alkali treatment method neutralization HCl and hydrolysis chlorosilane wherein, and do not have the high-boiling components dust in unreacted solid silicon dust of recycling and the tail gas, caused the waste of raw material.The method of alkali treatment is simultaneously used a large amount of alkali, and very high to the technological parameter and the performance requirement of equipment, has increased the cost of vent gas treatment.
Summary of the invention
The technical problem that the present invention solves is, a kind of processing method and device of technique of trichlorosilane synthetic tail gas are provided, hydrogen chloride, chlorosilane, hydrogen and solid silicon dust and high-boiling components dust after the recovery wet-treating in the chlorosilane absorption liquid have been saved raw material, have reduced production cost.
In order to solve above technical problem, the invention provides a kind of processing method of technique of trichlorosilane synthetic tail gas, comprising:
The synthesis tail gas that uses chlorosilane to absorb the generation of preparation trichlorosilane obtains the chlorosilane absorption liquid, and described synthesis tail gas comprises HCl, SiHCl
3, SiCl
4, H
2, silica soot and high-boiling components dust;
Heat described chlorosilane absorption liquid to 90 ℃～150 ℃;
Reclaim admixture of gas and solid mixture that the described chlorosilane absorption liquid of heating obtains respectively.
Preferably, use the described chlorosilane absorption liquid of Steam Heating.
Preferably, the temperature of described steam is 100 ℃～200 ℃.
Preferably, describedly reclaim admixture of gas and the solid mixture that the described chlorosilane absorption liquid of heating obtains respectively and comprise:
Described admixture of gas is filtered, and the admixture of gas feeding TCS device for recovering tail gas after the described filtration reclaims hydrogen chloride, chlorosilane, hydrogen wherein;
Described solid mixture is reclaimed the preparation trichlorosilane.
Preferably, described solid mixture is the mixture of silica soot and high-boiling components dust.
A kind for the treatment of apparatus of technique of trichlorosilane synthetic tail gas, comprise: heater, described heater comprises the housing that has heating jacket, and the gas discharging opening and being used to that described housing is provided with the charging aperture that is used to add the chlorosilane absorption liquid, be used to discharge the admixture of gas that obtains of the described chlorosilane absorption liquid of heating discharges the solid discharging opening of the solid mixture that the described chlorosilane absorption liquid of heating obtains.
Preferably, be connected with the condensation-water drain of the condensed water of the described steam heat exchange of steam inlet and discharge back formation on the described heating jacket.
Preferably, also comprise the filter that is connected with described gas discharge outlet.
Preferably, described filter comprises filter, and described filter is installed in the top of described filter by filter mounting.
Preferably, it is characterized in that also comprise the agitating device that is arranged in the described housing, described agitating device comprises stirrer paddle, described stirrer paddle links to each other by the puddler stirring motor outer with being arranged on heater.
The invention provides a kind of processing method of technique of trichlorosilane synthetic tail gas, at first use the described synthesis tail gas of chlorosilane drip washing to obtain the chlorosilane absorption liquid; Heating described absorption liquid then makes chlorosilane wherein gasify HCl and H
2Separate out with described gasification after chlorosilane form admixture of gas, solid silica flour and high-boiling components are separated out the formation solid mixture; Reclaim admixture of gas and solid mixture at last respectively.The present invention also provides a kind for the treatment of apparatus of technique of trichlorosilane synthetic tail gas, comprises heater, filter, charging aperture, boil discharging opening, mist discharging opening, nitrogen mouth admittedly.The processing method of technique of trichlorosilane synthetic tail gas provided by the invention and device reclaim admixture of gas and the solid mixture in the chlorosilane absorption liquid after the wet-treating respectively, have saved raw material, have reduced production cost.
Description of drawings
Fig. 1 technique of trichlorosilane synthetic tail gas treating apparatus schematic diagram;
The filter holder schematic diagram of Fig. 2 technique of trichlorosilane synthetic tail gas treating apparatus;
The filter schematic diagram of Fig. 3 technique of trichlorosilane synthetic tail gas treating apparatus;
The specific embodiment
In order further to understand the present invention, below in conjunction with example the preferred embodiment of the invention is described, but should be appreciated that these describe just to further specifying the features and advantages of the present invention, rather than to the restriction of claim of the present invention.
The invention provides the scheme that a kind of technique of trichlorosilane synthetic tail gas is handled, comprising:
The synthesis tail gas that uses chlorosilane to absorb the generation of preparation trichlorosilane obtains the chlorosilane absorption liquid, and described synthesis tail gas comprises HCl, SiHCl
3, SiCl
4, H
2, silica soot and high-boiling components dust;
Heat described chlorosilane absorption liquid to 90 ℃～150 ℃;
Reclaim admixture of gas and solid mixture that the described chlorosilane absorption liquid of heating obtains respectively.
According to the solution of the present invention, trichlorosilane carries out the gas-solid phase reaction preparation by industrial silicon and anhydrous hydrogen chloride (HCl) in fluidized-bed reactor, and product is a gaseous mixture, through after a series of condensation process, and most of SiHCl
3Condensation becomes liquid, and all the other products form synthesis tail gas.Contain a large amount of H that respond and generate in the described synthesis tail gas
2, unreacted HCl, a small amount of uncooled SiHCl
3With accessory substance SiCl
4And silica soot and high-boiling components dust.Use unreacted HCl, uncooled SiHCl in the described synthesis tail gas of liquid chlorosilane drip washing
3And SiCl
4, a spot of H
2, the described solid silicon dust of sedimentation and high-boiling components dust, form the chlorosilane absorption liquid.Most of H in the synthesis tail gas
2Feeding reclaimer utilizes again.
Described liquid chlorosilane is a liquefied mixture, comprises SiH
3Cl, SiH
2Cl
2, SiHCl
3, SiCl
4In one or more.The principle that the liquid chlorosilane absorbs HCl is a Physical Absorption, and principle is similar soluble in water the same with HCl.Physical Absorption is exactly to be that the adhesion between gas molecule and the fluid molecule is different with the different of chemical absorbing maximum, and the adhesion in the Physical Absorption between the liquids and gases molecule is a Van der Waals force, and what lean in the chemical absorbing is chemical bond.The present invention has relied on the Physical Absorption effect of HCl in chlorosilane liquid to reach separation HCl and H just
2Purpose owing to be Physical Absorption, HCl separated needed energy consumption in last handling process with chlorosilane just few.
According to the present invention program, heating chlorosilane absorption liquid, heating-up temperature is 90 ℃～150 ℃, is preferably 100 ℃～120 ℃.The gasification of being heated of chlorosilane in the described chlorosilane absorption liquid, HCl and small amount of H
2Separate out with described gasification after chlorosilane form admixture of gas, described admixture of gas is fed the TCS device for recovering tail gas reclaims.Continue the solid mixture that residual silica soot of the described chlorosilane absorption liquid of heating and high-boiling components form,, described dried solid mixture is reclaimed as reaction raw materials up to described solid mixture drying.
The heater that provides according to the present invention program can be heater well known in the art, as electric heater, steam heater, high-pressure heater, low-pressure heater, coal-fired heater etc., the preferred steam heater of the present invention.And that steam heater is divided into is multiple, for example shell-and-tube steam heater, bushing type steam heater, jacket type steam heater, preferred jacket formula steam heater of the present invention.As shown in Figure 1, described jacket type steam heater 1 is made up of housing 11 and vapour jacket 12, upper left quarter 11 is provided with charging aperture 4, be provided with solid mixture discharging opening 5 at 11 lower left quarters, left 11 is provided with nitrogen mouth 111,12 upper right quarter is provided with steam inlet 121, is provided with condensation-water drain 122 at 12 right lower quadrants.
Jacket type steam heater provided by the invention is a horizontal heater, and it is circular-arc that the left and right sides is, level up and down, and with left and right sides smooth connection, housing and steam jacketed material are preferably mild steel, and thickness is 5mm～15mm, is preferably 8mm～10mm.Described housing major diameter is that 2m～4m is preferably 3m～3.5m, and minor axis is 0.5m～1m, preferred 0.75m～0.8m, and described housing and described vapour jacket spacing are 10cm～20cm, are preferably 12cm～15cm.
For described chlorosilane absorption liquid is heated evenly, the present invention also is provided with agitating device in described jacket type steam heater, described agitating device is an agitator well known in the art, as turbine agitator, arm stirrer, anchor agitator, helix(ribbon type) agitator, magnetic stirring apparatus, magnetic force heating stirrer etc., the preferred arm stirrer of the present invention, described arm stirrer has flat oar formula and two kinds of oblique oar formulas again according to the difference of blade form.The preferably flat oar formula of the present invention, described flat-blade paddle agitator is made of straight blade more than two, preferred 3 of the present invention,
According to agitator provided by the invention, as shown in Figure 1, comprise stirrer paddle 31, puddler 32, stirring motor 33.Wherein stirrer paddle is in described jacket type steam heater housing 11, and described stirrer paddle 31 is installed on the puddler 32, the long 30cm～50cm of blade, preferred 35cm～45cm, wide 15cm～30cm, preferred 20cm～25cm, blade pitch is 20cm～60cm, preferred 30cm～50cm.The two-layer light body that described puddler 32 passes described jacket type steam heater is connected with described stirring motor 33, and the rotating speed of described stirring motor is 60r/min～120r/min, is preferably 80r/min～100r/min.
Described chlorosilane absorption liquid heating back chlorosilane liquid gasification, HCl and H
2Separate out the formation mist, described mist enters the TCS exhaust gas processing device after by filter, further separates each component in the described mist.Along with the rising of temperature and the continuous gasification of described chlorosilane absorption liquid, described mist is taken away a spot of silica soot and high-boiling components, and by filter the time, described silica soot and high-boiling components are filtered, and reach the purpose of separation.
According to the present invention program, filter 2 comprises filtration cavity 21, filter 22 filter mountings 23, nitrogen mouth 24, mist discharging opening 6.Wherein filtering cavity 21 is connected with the housing of described jacket type steam heater; Filter 22 is installed on the filter mounting 23, is in the bottom of filter mounting 23; Filter mounting 23 is installed in the filtration inside cavity, will filter cavity 21 and be divided into two parts up and down; Nitrogen mouth 24 is arranged on the upper left quarter that filters cavity, and nitrogen enters by described nitrogen mouth 24 and filters solid silicon and the high-boiling components of cavity 21 from the absorption of filter mounting top blowback filter, makes its sedimentation; Mist discharging opening 6 is arranged on the top of filtering cavity.Described nitrogen mouth 24 is identical with described nitrogen mouth 111 structures.Described filter mounting 23 is for being preferably circle, and described filter 22 is preferably and is that cylinder, the number of described filter are 1～8, and the present invention is preferably 4.
The Different Effects of filter medium Selection of Filters, because it is silica soot and the high-boiling components that filters in the described admixture of gas that the present invention selects the purpose of filter for use, so the present invention selects air cleaner well known in the art for use, the main filtration chipware of air cleaner is an activated charcoal strainer, and the characteristics of its porous have guaranteed passing through of described admixture of gas and silica soot and the high-boiling components of carrying secretly in the described admixture of gas filtered out.According to bill of the present invention, the activated charcoal strainer in the described filter is 5～15 layers, preferred 10 layers of the present invention.
When described chlorosilane absorption liquid constantly gasifies, constantly there are silica soot and high-boiling components to separate out the formation solid mixture in the described jacket type steam heater 1.Rising along with temperature, final chlorosilane all gasifies, and the solid mixture in the described housing in back that gasifies is continued heating, dry described solid mixture, under stirring action, discharge described solid mixture, and it is recycled to reactor participation reaction by solid mixture discharging opening 5.
According to scheme provided by the invention, the handling process of technique of trichlorosilane synthetic tail gas is a batch (-type), described chlorosilane absorption liquid injects described jacket type steam heater by charging aperture, when liquid level reaches 1/2～1 housing volume, when being preferably 2/3～4/5 housing volume, open agitating device, and while feeding steam in described vapour jacket heats.The control of liquid level can be taken into account the related valve realization by a liquid level in the housing.After described admixture of gas reclaims and finishes, by nitrogen mouth 24 to the inner nitrogen that feeds of filter, blowback filter, the absorption that makes the silica soot of adsorbing on the filter and high-boiling components break away from filter, and final settlement mixes with described solid mixture at described housing bottom.
After all feed separation are discharged and finished, feed inert gas and protect and dedusting in described housing, described inert gas is well known in the art as nitrogen, neon, argon gas, xenon etc.; preferred nitrogen of the present invention; because the economic environmental protection of nitrogen easily stores transportation, good stability.
According to the present invention program, the processing time of whole technique of trichlorosilane synthetic tail gas is 30min～120min, is preferably 60min～90min.
The present invention has carried out detailed elaboration by processing method and the device to technique of trichlorosilane synthetic tail gas, used specific case herein principle of the present invention and embodiment are set forth, the explanation of above example just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (10)
1. the processing method of a technique of trichlorosilane synthetic tail gas comprises:
The synthesis tail gas that uses chlorosilane to absorb the generation of preparation trichlorosilane obtains the chlorosilane absorption liquid, and described synthesis tail gas comprises HCl, SiHCl
3, SiCl
4, H
2, silica soot and high-boiling components dust;
Heat described chlorosilane absorption liquid to 90 ℃～150 ℃;
Reclaim admixture of gas and solid mixture that the described chlorosilane absorption liquid of heating obtains respectively.
2. processing method according to claim 1 is characterized in that, uses the described chlorosilane absorption liquid of Steam Heating.
3. processing method according to claim 2 is characterized in that, the temperature of described steam is 100 ℃～200 ℃.
4. processing method according to claim 1 is characterized in that, admixture of gas and solid mixture that the described chlorosilane absorption liquid of the described heating of recovery respectively obtains comprise:
Described admixture of gas is filtered, and the admixture of gas after the described filtration feeds the TCS device for recovering tail gas and reclaims;
Described solid mixture is reclaimed the preparation trichlorosilane.
5. processing method according to claim 4 is characterized in that, described solid mixture is the mixture of silica soot and high-boiling components dust.
6. the treating apparatus of a technique of trichlorosilane synthetic tail gas, it is characterized in that, comprise: heater, described heater comprises the housing that has heating jacket, and the gas discharging opening and being used to that described housing is provided with the charging aperture that is used to add the chlorosilane absorption liquid, be used to discharge the admixture of gas that obtains of the described chlorosilane absorption liquid of heating discharges the solid discharging opening of the solid mixture that the described chlorosilane absorption liquid of heating obtains.
7. treating apparatus according to claim 6 is characterized in that, the condensation-water drain of the condensed water of formation after being connected with steam inlet on the described heating jacket and discharging described steam heat exchange.
8. device according to claim 6 is characterized in that, also comprises the filter that is connected with described gas discharge outlet.
9. device according to claim 8 is characterized in that described filter comprises filter, and described filter is installed in the top of described filter by filter mounting.
10. according to any described device of claim 6 to 8, it is characterized in that, also comprise the agitating device that is arranged in the described housing, described agitating device comprises stirrer paddle, and described stirrer paddle links to each other by the puddler stirring motor outer with being arranged on heater.
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|---|---|---|---|
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|---|---|---|---|
| CN 200910260581 CN102100998B (en) | 2009-12-21 | 2009-12-21 | Method and device for processing trichlorosilane synthesis tail gas |
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| CN102989379A (en) * | 2011-09-09 | 2013-03-27 | 曲靖师范学院 | Gas-solid phase reactor |
| CN103041684A (en) * | 2013-01-28 | 2013-04-17 | 六九硅业有限公司 | Treatment method and device for tail gas of silane purifying process |
| CN103159217A (en) * | 2013-03-07 | 2013-06-19 | 江西景德半导体新材料有限公司 | Polysilicon reducing furnace tail gas silicon powder collection device and application method |
| CN105797543A (en) * | 2016-05-17 | 2016-07-27 | 山东瑞川硅业有限公司 | SiHCl3 synthetic tail gas treatment device |
| CN109835904A (en) * | 2019-04-12 | 2019-06-04 | 四川永祥多晶硅有限公司 | Restore the treatment process of amorphous silicon in tail gas |
| CN111249887A (en) * | 2020-02-24 | 2020-06-09 | 洛阳中硅高科技有限公司 | Method for treating silicon tetrachloride tail gas |
| CN115650241A (en) * | 2022-10-28 | 2023-01-31 | 内蒙古通威高纯晶硅有限公司 | Polysilicon production slag slurry treatment process |
| US11612869B2 (en) | 2017-11-20 | 2023-03-28 | Tokuyama Corporation | Production method for trichlorosilane, and pipe |
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| CN2426756Y (en) * | 2000-06-06 | 2001-04-18 | 中国科学院山西煤炭化学研究所 | Evaporator |
| WO2008059883A1 (en) * | 2006-11-14 | 2008-05-22 | Mitsubishi Materials Corporation | Hydrogen purification/collection method and hydrogen purification/collection facility |
| CN100556507C (en) * | 2007-09-04 | 2009-11-04 | 浙江开化合成材料有限公司 | A kind of method for recovering tail gas of trichlorosilane production |
| CN101444681B (en) * | 2008-12-15 | 2010-08-18 | 浙江富士特硅材料有限公司 | Method for recovering tail gas from trichlorosilane production and special equipment thereof |
| CN101538043B (en) * | 2009-03-27 | 2011-01-26 | 华陆工程科技有限责任公司 | Method for recovering trichlorosilane synthesis tail gas |
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| CN102989379A (en) * | 2011-09-09 | 2013-03-27 | 曲靖师范学院 | Gas-solid phase reactor |
| CN102989379B (en) * | 2011-09-09 | 2014-07-23 | 曲靖师范学院 | Gas-solid phase reactor |
| CN103041684A (en) * | 2013-01-28 | 2013-04-17 | 六九硅业有限公司 | Treatment method and device for tail gas of silane purifying process |
| CN103041684B (en) * | 2013-01-28 | 2015-11-18 | 六九硅业有限公司 | A kind of processing method of silane purification process tail gas and device |
| CN103159217A (en) * | 2013-03-07 | 2013-06-19 | 江西景德半导体新材料有限公司 | Polysilicon reducing furnace tail gas silicon powder collection device and application method |
| CN105797543A (en) * | 2016-05-17 | 2016-07-27 | 山东瑞川硅业有限公司 | SiHCl3 synthetic tail gas treatment device |
| CN105797543B (en) * | 2016-05-17 | 2019-03-29 | 山东瑞川硅业有限公司 | A kind of processing unit of technique of trichlorosilane synthetic tail gas |
| US11612869B2 (en) | 2017-11-20 | 2023-03-28 | Tokuyama Corporation | Production method for trichlorosilane, and pipe |
| CN109835904A (en) * | 2019-04-12 | 2019-06-04 | 四川永祥多晶硅有限公司 | Restore the treatment process of amorphous silicon in tail gas |
| CN111249887A (en) * | 2020-02-24 | 2020-06-09 | 洛阳中硅高科技有限公司 | Method for treating silicon tetrachloride tail gas |
| CN115650241A (en) * | 2022-10-28 | 2023-01-31 | 内蒙古通威高纯晶硅有限公司 | Polysilicon production slag slurry treatment process |
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Effective date of registration: 20160216 Address after: 832000 Shihezi Economic Development Zone, the Xinjiang Uygur Autonomous Region Province, the new chemical materials Industrial Park weft Road, six Patentee after: Xinjiang DAQO New Energy Co., Ltd. Address before: 666 No. 404000 Chongqing District of Wanzhou City long road Patentee before: Chongqing Daqo New Energy Co., Ltd. |