CN103101914A - Intermittent operation method and device for recovery and purification of hexachlorodisilane from chlorosilane residual liquid - Google Patents
Intermittent operation method and device for recovery and purification of hexachlorodisilane from chlorosilane residual liquid Download PDFInfo
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Abstract
The invention aims to provide an intermittent technology and a device for treatment and recovery of chlorosilane residual liquid and residue thereof, especially a method and a device for recovering hexachlorodisilane with very high value. The invention puts forward an intermittent technical scheme for the circumstance of a small residual liquid treatment amount. The technology mainly involves a primary rectification tower and an intermittent rectification tower. The method and the device provided in the invention are particularly applicable to treatment of the cold hydrogenation slag slurry and rectification residual liquid in polysilicon production, the rectification residual liquid and other dirty residual liquids in a synthesis process, and are also applicable to the rectification residual liquid in a reduction process and the rectification residual liquid in a thermal hydrogenation process or mixed type residual liquids, etc. With the treatment technology disclosed in the invention, hexachlorodisilane with purity above 98% can be recovered.
Description
Technical field
The present invention relates to a kind of the recovery and periodical operation method and the device of purification disilicone hexachloride from the chlorosilane raffinate, particularly relate to high boiling material disilicone hexachloride in chlorosilane recovery method and the device thereof of (also claiming hexachloro-silane, perchloro-silicoethane).
Background technology
Polysilicon is the required main raw material of electronic industry and photovoltaic industry, is China's electronics and information industry and the necessary strategic materials of photovoltaic industry development.
in the production process of polysilicon, be accompanied by rectification and purification chlorosilane building-up reactions, the carrying out of reduction reaction and cold (heat) hydrogenation tail gas can unavoidably produce a certain amount of raffinate, the direct utility value of this part raffinate nothing with regard to the production of polysilicon, in addition because solid content in this part raffinate is higher, contain superpolymer, viscosity is large, normal continuous blow-down process is difficult to realize, need manual operation, and this part material oxidisability is strong, very easily hydrolysis produces hydrogenchloride, to impact sensitive, easily burning, be exposed in air abnormally dangerous, general processing mode is the hydrolysis of extensive style, this is the waste to raw material, again human and environment has been caused great harm.The chlorosilane raffinate becomes the bottleneck problem that allows many polysilicon enterprise's headaches and limit the polysilicon industry development at present.
After cold (heat) hydrogenation slag slurry and distillation residual liquid, synthetic furnace distillation residual liquid, reduction furnace distillation residual liquid etc. having been done the pertinent literature research of a large amount of home and abroads and the detection to individual samples, determine that substantially the chlorosilane raffinate mainly is comprised of following four parts:
What in raffinate, content was maximum is single silicon chlorosilane, is the important source material of production of polysilicon, has certain recovery value.Mention the above high boiling material of Si2Cl6 boiling point in patent EP0634418 and can be used for producing the Chemicals such as heat-transfer fluid, lubricant, silicon rubber, resin, sealed binder, also have certain recovery value.It should be noted that in addition the large hexachloro-silane of proportion that height in the chlorosilane raffinate boils in component has high added value, can bring very large extra economic benefit if carry out suitable purification.
Si2Cl6 can be used for vapour deposition and make amorphous si film and epitaxial film (as SiN, SiGe, SiC etc.) thereof, with respect to traditional silane, dichloro-dihydro silicon vapour deposition process, its depositing temperature is low, selectivity is high, density of film is even and film performance is superior, Si2Cl6 is also a kind of extremely highly active reductor in addition, optical fiber raw material, glass, silicoethane raw material are a kind of very expensive industrial chemicals.
Obviously, compare with various components in reasonable recovery raffinate, the raffinate hydrolysis can cause huge waste, particularly along with the continuous expansion of polysilicon output, the raffinate that is not rationally reclaimed is multiplied, if high added value component, particularly hexachloro-silane in energy efficient recovery raffinate will make enterprise stand on the invincible position in current fierce polysilicon market competition.But, because impurity in the chlorosilane raffinate that contains cold hydrogenation process, synthesis procedure is many, organochlorosilane such as trichloromethyl silane (70.2 ℃ of boiling points) approach again with hexachloro-silane (145 ℃ of boiling points) with silicon tetrachloride (56.8 ℃ of boiling points), titanium tetrachloride (136 ℃ of boiling points), require very high to reclaiming the purification separating technology.
US Patent No. 0193958 proposes to use a kind of step blade dryer dried recovered to process the method for chlorosilane raffinate, evaporation is reclaimed in complete rear use urao and remaining raffinate and solid slag, this method is a kind of environmentally friendly method and can reclaims a certain amount of chlorosilane, but do not relate to the recovery to the hexachloro-silane of high boiling material and high added value.
Summary of the invention
The object of the present invention is to provide a kind of economy, environment-friendly type recovery and treatment method and device thereof, the chlorosilane raffinate that in the processing production of polysilicon, cold (heat) hydrogenation slag slurry and distillation residual liquid, synthesis procedure distillation residual liquid, reduction furnace distillation residual liquid consist of, reclaim various valuable components such as silicon tetrachloride and high boiling point silicon oil in raffinate, the hexachloro-silane that particularly has high value.Comprehensive above requirement, the situation few according to the raffinate treatment capacity, the invention provides a kind of from the chlorosilane raffinate periodical operation method and the device of recovery and purification disilicone hexachloride.
Technical scheme of the present invention is as follows:
reclaim from the chlorosilane raffinate and grasp device the intermittence of purification disilicone hexachloride: comprise just minute rectifying tower (6), just divide rectifying tower kettle-type reboiler (1), batch fractionating tower (7), batch fractionating tower kettle-type reboiler (2), chlorosilane storage tank (3), organosilane storage tank (4), hexachloro-silane storage tank (5), it is characterized in that just being provided with just minute rectifying tower kettle-type reboiler (1) at the bottom of minute rectifying tower (6) tower, be provided with the feed entrance of chlorosilane raffinate (8) on first minute rectifying tower kettle-type reboiler (1) top, the just top of minute rectifying tower kettle-type reboiler (1) connection high boiling material silicone oil removes drip washing pipeline (9), just be provided with the entrance of low-pressure steam pipeline (10) and high pressure steam line (11) on minute rectifying tower kettle-type reboiler (1), just minute rectifying tower (a 6) tower top arranges tail gas and vacuum lines (12), tower top is provided with the entrance of chlorine material pipeline (17) and nitrogen material pipeline (18), just minute rectifying tower (a 6) condenser arranges and just divides a product pipeline (13) to be connected to batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) bottom is provided with batch fractionating tower kettle-type reboiler (2), be provided with low-pressure steam pipeline (16) on batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) top arranges tail gas and vacuum lines (14), batch fractionating tower (7) condenser arranges rectifying product pipeline (15), and product pipeline (15) is connected to chlorosilane storage tank (3), organosilane storage tank (4) and hexachloro-silane storage tank (5).
The working method of recovery and purification disilicone hexachloride from the chlorosilane raffinate is characterized in that step is as follows:
1) chlorosilane raffinate (8) is from just minute rectifying tower kettle-type reboiler (1) top charging, just minute rectifying tower (6) adopts the batch fractionating mode, use low-pressure steam as thermal source by low-pressure steam pipeline (10), chlorosilane in raffinate distills successively by boiling point, after beginning from equilibrium temperature when tower top to rise, vacuumize gradually light constituent chlorosilane in chlorosilane raffinate (8) by the beginning of tower top tail gas and vacuum lines (12), organochlorosilane, hexachloro-silane finally further separates from just dividing rectifying tower (6) overhead condenser to enter to batch fractionating tower kettle-type reboiler (2) through a first minute product pipeline (12) by boiling point successively, after in high boiling material, hexachloro-silane has steamed, to high pressure vapour line (11), go drip washing pipeline (9) to send to drip washing through high boiling material silicone oil high boiling point silicon oil gasification substance in chlorosilane raffinate (8) the heating steam plugging, after evaporation finishes, minute rectifying tower kettle-type reboiler (a 1) heating tubulation draws off the tower reactor residual powder by extracting out just,
2). just divide product through just dividing a product pipeline (13) to enter batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) uses low-pressure steam as thermal source by low-pressure steam pipeline (16), chlorosilane in raffinate distills successively by boiling point, after beginning from equilibrium temperature when tower top to rise, vacuumize gradually by tower top tail gas and vacuum lines (14) beginning, raffinate light constituent chlorosilane in batch fractionating tower (7) tower reactor, organochlorosilane, hexachloro-silane reclaims respectively through product pipeline (15) from batch fractionating tower (7) overhead condenser by boiling point successively and enters chlorosilane storage tank (3), organosilane storage tank (4), hexachloro-silane storage tank (5).
Described just minute rectifying tower (a 6) working pressure is 0 ~ 80KPa, and tower top temperature is 30 ~ 105 ℃, and the tower theoretical stage is 15 ~ 30, tower diameter 280 ~ 320mm, 130 ~ 140 ℃ of low-pressure heating vapor temperatures, 200 ~ 250 ℃ of middle pressure heating steam temperature.
Described batch fractionating tower (7) working pressure is 0 ~ 80KPa, and tower top temperature is 30 ~ 105 ℃, and packed height is 45 ~ 55m, tower diameter 180 ~ 220mm.
Described just minute rectifying tower (6) passes into a certain amount of chlorine through chlorine material pipeline (17) when using the low-pressure steam heating, pass into the chlorine of nitrogen replacement remnants through nitrogen material pipeline (18) when thermal source switches to middle pressure steam, increase the hexachloro-silane yield.
Compared with prior art, intermittent type chlorosilane raffinate intermittent type technical scheme beneficial effect of the present invention is:
[1] the present invention is not limited to the cleaner hot hydrogenation of recycling, reduction furnace distillation residual liquid, is applicable to too cold hydrogenation process raffinate and the raffinates such as synthesis procedure raffinate or mixed type.
[2] the present invention than traditional raffinate technology for hydrolyzing, can reclaim chlorosilane in raffinate, the particularly high component of hexachloro-silane added value, is that a kind of utilization of resources maximizes, the technique of economy, environment-friendly type.
[3] a kind of mobile type intermittent type processing scheme that provides in the low situation of raffinate treatment capacity is provided in the present invention.
[4] the present invention can use take low-pressure steam as main heat source, the middle pressure steam type of heating as auxiliary thermal source by vacuum operating, has avoided the residual full use higher-grade middle pressure steam of rectifying separation chlorosilane.
[5] the present invention can provide chlorosilane in a kind of chlorosilane raffinate, height boils, solid phase recycles respectively technique, has greatly reduced the expenses such as various processing, transportation, storage, landfill.
[6] the present invention can provide a kind of chloridization process of high chlorosilane, just passing into a certain amount of chlorine through chlorine material pipeline (17) in minute tower (6) use low-pressure steam heating, pass into the chlorine of a certain amount of nitrogen replacement remnants through nitrogen material pipeline (18) when thermal source switches to middle pressure steam, increase the hexachloro-silane yield with this.
Description of drawings
Fig. 1: intermittent type chlorosilane raffinate recycling technical scheme schema of the present invention.
Embodiment
Below in conjunction with Fig. 1, the intermittent type scheme is described in further detail
Intermittent type chlorosilane raffinate recycling technical scheme 1 of the present invention is as follows:
a kind of intermittent type chlorosilane raffinate recycling and processing device: comprise just minute rectifying tower (6), just divide rectifying tower kettle-type reboiler (1), batch fractionating tower (7), batch fractionating tower kettle-type reboiler (2), chlorosilane storage tank (3), organosilane storage tank (4), hexachloro-silane storage tank (5), it is characterized in that just being provided with just minute rectifying tower kettle-type reboiler (1) at the bottom of minute rectifying tower (6) tower, be provided with the feed entrance of chlorosilane raffinate (8) on first minute rectifying tower kettle-type reboiler (1) top, the just top of minute rectifying tower kettle-type reboiler (1) connection high boiling material silicone oil removes drip washing pipeline (9), just be provided with low-pressure steam pipeline (10) and high pressure steam line (11) on minute rectifying tower kettle-type reboiler (1), just minute rectifying tower (a 6) tower top arranges tail gas and vacuum lines (12), tower top is provided with chlorine material pipeline (17) and nitrogen material pipeline (18), just minute rectifying tower (a 6) condenser arranges and just divides a product pipeline (13) to be connected to batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) bottom is provided with batch fractionating tower kettle-type reboiler (2), be provided with low-pressure steam pipeline (16) on batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) top arranges tail gas and vacuum lines (14), and batch fractionating tower (7) condenser arranges rectifying product pipeline (15) and is connected to chlorosilane storage tank (3), organosilane storage tank (4), hexachloro-silane storage tank (5).
Intermittent type chlorosilane raffinate working method of the present invention is as follows:
chlorosilane raffinate (8) is from just minute rectifying tower kettle-type reboiler (1) top charging, just minute rectifying tower (6) adopts the batch fractionating mode, use low-pressure steam as thermal source by low-pressure steam pipeline (10), pass into chlorine through chlorine material pipeline (17) in tower simultaneously, chlorosilane in raffinate distills successively by boiling point, after beginning from 55 ~ 60 ℃ of equilibrium temperatures when tower top to rise, be evacuated to gradually vacuum tightness 80KPa by tower top tail gas and vacuum lines (12) beginning, light constituent chlorosilane in chlorosilane raffinate (8), organochlorosilane, hexachloro-silane finally further separates from just dividing rectifying tower (6) overhead condenser to enter to batch fractionating tower kettle-type reboiler (2) through a first minute product pipeline (13) by boiling point successively, after in high boiling material, hexachloro-silane has steamed, with the heating steam plugging to high pressure vapour line (11), pass into simultaneously the chlorine of nitrogen replacement remnants in tower through nitrogen material pipeline (18), go drip washing pipeline (9) to send to drip washing through high boiling material silicone oil high boiling point silicon oil gasification substance in chlorosilane raffinate (8), after evaporation finishes, the tower reactor residual powder draws off through a first minute rectifying tower kettle-type reboiler (1).just minute product is through just dividing a product pipeline (13) to enter batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) uses low-pressure steam as thermal source by low-pressure steam pipeline (16), chlorosilane in raffinate distills successively by boiling point, after beginning from 55 ~ 60 ℃ of equilibrium temperatures when tower top to rise, be evacuated to gradually vacuum tightness 80KPa by tower top tail gas and vacuum lines (14) beginning, raffinate light constituent chlorosilane in batch fractionating tower (7) tower reactor, organochlorosilane, hexachloro-silane reclaims respectively through product pipeline (15) from batch fractionating tower (7) overhead condenser by boiling point successively and enters chlorosilane storage tank (3), organosilane storage tank (4), hexachloro-silane storage tank (5), the hexachloro-silane that obtains needs low temperature, ground connection, nitrogen-sealed stores.
Technology and equipment of the present invention is applicable to recycle the chlorosilane raffinate that produces in polysilicon production process, for the present invention being described better in the advantage aspect the resource maximization, choosing an application example and is illustrated.
The charging situation is as follows:
Cold hydrogenation slag slurry and distillation residual liquid 3t/hr, feed composition: content of silicon tetrachloride is 60%; Trichlorosilane content is 1.5%; It is 2% that organochlorosilane adds up to content; Hexachloro-silane content is 10%; High boiling material silicone oil content is 5%;
Just minute rectifying tower (a 1) working pressure is 0 ~ 80KPa(vacuum tightness), tower top temperature is 30 ~ 105 ℃, the tower theoretical stage is 15 ~ 30, tower diameter 280 ~ 320mm, 130 ~ 140 ℃ of low-pressure heating vapor temperatures, 200 ~ 250 ℃ of middle pressure heating steam temperature; Batch fractionating tower (2) working pressure is 0 ~ 80KPa(vacuum tightness), tower top temperature is 30 ~ 105 ℃, and packed height is 45 ~ 55m, and tower diameter 180 ~ 220mm after the thick product-collecting of Si2Cl6 is extremely a certain amount of, can returns to batch fractionating tower and purify to desired purity.
The operating time of material is about 24h, and separately establishing non-cutting time is 4h, and the total time of processing a batch materials is about 28h.Batch fractionating mode Si2Cl6 product purity depends on the number of times of repetition rectification and purification, and the product purity of process primary purification is greater than 98%.
Intermittent type chlorosilane raffinate recovery processing technique and device that the present invention proposes, be described by embodiment, person skilled obviously can be changed system and method as herein described within not breaking away from content of the present invention, spirit and scope or suitably change and combination, realizes technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are deemed to be included in spirit of the present invention, scope and content.
Claims (5)
1. one kind is reclaimed from the chlorosilane raffinate and grasp device the intermittence of purification disilicone hexachloride: comprise just minute rectifying tower (6), just divide rectifying tower kettle-type reboiler (1), batch fractionating tower (7), batch fractionating tower kettle-type reboiler (2), chlorosilane storage tank (3), organosilane storage tank (4), hexachloro-silane storage tank (5), it is characterized in that just being provided with just minute rectifying tower kettle-type reboiler (1) at the bottom of minute rectifying tower (6) tower, be provided with the feed entrance of chlorosilane raffinate (8) on first minute rectifying tower kettle-type reboiler (1) top, the just top of minute rectifying tower kettle-type reboiler (1) connection high boiling material silicone oil removes drip washing pipeline (9), just be provided with the entrance of low-pressure steam pipeline (10) and high pressure steam line (11) on minute rectifying tower kettle-type reboiler (1), just minute rectifying tower (a 6) tower top arranges tail gas and vacuum lines (12), tower top is provided with the entrance of chlorine material pipeline (17) and nitrogen material pipeline (18), just minute rectifying tower (a 6) condenser arranges and just divides a product pipeline (13) to be connected to batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) bottom is provided with batch fractionating tower kettle-type reboiler (2), be provided with low-pressure steam pipeline (16) on batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) top arranges tail gas and vacuum lines (14), batch fractionating tower (7) condenser arranges rectifying product pipeline (15), and product pipeline (15) is connected to chlorosilane storage tank (3), organosilane storage tank (4) and hexachloro-silane storage tank (5).
2. adopt the device of claim 1 to reclaim from the chlorosilane raffinate and the working method of purification disilicone hexachloride, it is characterized in that step is as follows:
1). chlorosilane raffinate (8) is from just minute rectifying tower kettle-type reboiler (1) top charging, just minute rectifying tower (6) adopts the batch fractionating mode, use low-pressure steam as thermal source by low-pressure steam pipeline (10), chlorosilane in raffinate distills successively by boiling point, after beginning from equilibrium temperature when tower top to rise, vacuumize gradually by tower top tail gas and vacuum lines (12) beginning, light constituent chlorosilane in chlorosilane raffinate (8), organochlorosilane, hexachloro-silane finally further separates from just dividing rectifying tower (6) overhead condenser to enter to batch fractionating tower kettle-type reboiler (2) through a first minute product pipeline (12) by boiling point successively, after in high boiling material, hexachloro-silane has steamed, to high pressure vapour line (11), go drip washing pipeline (9) to send to drip washing through high boiling material silicone oil high boiling point silicon oil gasification substance in chlorosilane raffinate (8) the heating steam plugging, after evaporation finishes, minute rectifying tower kettle-type reboiler (a 1) heating tubulation draws off the tower reactor residual powder by extracting out just,
2). just divide product through just dividing a product pipeline (13) to enter batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) uses low-pressure steam as thermal source by low-pressure steam pipeline (16), chlorosilane in raffinate distills successively by boiling point, after beginning from equilibrium temperature when tower top to rise, vacuumize gradually by tower top tail gas and vacuum lines (14) beginning, raffinate light constituent chlorosilane in batch fractionating tower (7) tower reactor, organochlorosilane, hexachloro-silane reclaims respectively through product pipeline (15) from batch fractionating tower (7) overhead condenser by boiling point successively and enters chlorosilane storage tank (3), organosilane storage tank (4), hexachloro-silane storage tank (5).
3. method as claimed in claim 2, is characterized in that described just minute rectifying tower (a 6) working pressure is 0～80KPa, and tower top temperature is 30～105 ℃, the tower theoretical stage is 15～30, tower diameter 280～320mm, 130～140 ℃ of low-pressure heating vapor temperatures, 200～250 ℃ of middle pressure heating steam temperature.
4. method as claimed in claim 2, is characterized in that described batch fractionating tower (7) working pressure is 0～80KPa, and tower top temperature is 30～105 ℃, and packed height is 45～55m, tower diameter 180～220mm.
5. method as claimed in claim 2, it is characterized in that passing into a certain amount of chlorine through chlorine material pipeline (17) when described just minute rectifying tower (6) uses the low-pressure steam heating, pass into the chlorine of nitrogen replacement remnants through nitrogen material pipeline (18) when thermal source switches to middle pressure steam, increase the hexachloro-silane yield.
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| CN104016353B (en) * | 2014-06-18 | 2016-06-29 | 四川永祥多晶硅有限公司 | A kind of cold hydrogenation wet dust collection slurry discharges system and method thereof |
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| CN106178386B (en) * | 2016-07-06 | 2021-12-14 | 合盛硅业股份有限公司 | Treatment method and treatment device of organic silicon slag slurry |
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| CN109607548A (en) * | 2018-12-29 | 2019-04-12 | 内蒙古自治区浩森新材料开发有限公司 | A kind of method and device using polysilicon waste production silicon tetrachloride |
| CN110078080A (en) * | 2019-04-26 | 2019-08-02 | 天津科技大学 | A kind of chlorosilane high-boiling components recovery process of combination slurry processing and cracking reaction |
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| CN113599856A (en) * | 2021-08-11 | 2021-11-05 | 安徽晟捷新能源科技有限公司 | Equipment for recycling tar at bottom of NMP (N-methyl pyrrolidone) rectifying tower |
| CN114130052A (en) * | 2021-12-20 | 2022-03-04 | 青海亚洲硅业半导体有限公司 | Recovery unit of high boiling thing in chlorosilane raffinate |
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