CN103101914B - 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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- CN103101914B CN103101914B CN201310059040.9A CN201310059040A CN103101914B CN 103101914 B CN103101914 B CN 103101914B CN 201310059040 A CN201310059040 A CN 201310059040A CN 103101914 B CN103101914 B CN 103101914B
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- 239000005046 Chlorosilane Substances 0.000 title claims abstract description 63
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 31
- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000011084 recovery Methods 0.000 title abstract description 15
- 239000007788 liquid Substances 0.000 title abstract description 10
- 238000000746 purification Methods 0.000 title description 11
- 238000005194 fractionation Methods 0.000 claims abstract 12
- 238000009835 boiling Methods 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 30
- 238000003860 storage Methods 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 21
- 238000004821 distillation Methods 0.000 claims description 16
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 15
- 239000000460 chlorine Substances 0.000 claims description 15
- 229910052801 chlorine Inorganic materials 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 150000001282 organosilanes Chemical class 0.000 claims description 9
- 150000001367 organochlorosilanes Chemical class 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 229920002545 silicone oil Polymers 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- 238000004508 fractional distillation Methods 0.000 claims 3
- 238000000998 batch distillation Methods 0.000 claims 1
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000011017 operating method Methods 0.000 claims 1
- 238000012856 packing Methods 0.000 claims 1
- 238000010025 steaming Methods 0.000 claims 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 11
- 229920005591 polysilicon Polymers 0.000 abstract description 11
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000002893 slag Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000011946 reduction process Methods 0.000 abstract 1
- 229910000077 silane Inorganic materials 0.000 description 24
- 238000012545 processing Methods 0.000 description 7
- 229910007245 Si2Cl6 Inorganic materials 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000000470 constituent Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000005049 silicon tetrachloride Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 206010019233 Headaches Diseases 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910000577 Silicon-germanium Inorganic materials 0.000 description 1
- CYVTYWBDUINCRE-UHFFFAOYSA-N [Si].[SiH3]Cl Chemical compound [Si].[SiH3]Cl CYVTYWBDUINCRE-UHFFFAOYSA-N 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- NTQGILPNLZZOJH-UHFFFAOYSA-N disilicon Chemical compound [Si]#[Si] NTQGILPNLZZOJH-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 239000013529 heat transfer fluid Substances 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- WCTAGTRAWPDFQO-UHFFFAOYSA-K trisodium;hydrogen carbonate;carbonate Chemical compound [Na+].[Na+].[Na+].OC([O-])=O.[O-]C([O-])=O WCTAGTRAWPDFQO-UHFFFAOYSA-K 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
本发明的目的在于提供一种间歇式氯硅烷残液及残渣回收处理工艺及其装置，特别是针对回收具有极高价值的六氯乙硅烷（又称六氯二硅烷、全氯乙硅烷）的方法及其装置。本发明是根据残液处理量小的情况下提出的一种间歇式技术方案。本工艺主要包括初分精馏塔与间歇精馏塔。本发明特别适用于处理多晶硅生产中冷氢化渣浆及精馏残液、合成工序精馏残液等脏残液，也同样适用于还原工序精馏残液与热氢化工序精馏残液或混合类型等残液。本发明处理工艺可以回收得到纯度98％以上的六氯乙硅烷。
The purpose of the present invention is to provide an intermittent chlorosilane raffinate and residue recovery treatment process and its device, especially for the recovery of extremely high value hexachlorodisilane (also known as hexachlorodisilane, perchlorodisilane) Method and device thereof. The present invention is a batch-type technical scheme proposed under the condition that the raffinate treatment amount is small. This process mainly includes a primary fractionation tower and a batch rectification tower. The invention is especially suitable for treating dirty raffinate such as intercooled hydrogenation slag and rectification raffinate in polysilicon production, and rectification raffinate in synthesis process, and is also suitable for mixing rectification raffinate in reduction process and rectification raffinate in thermal hydrogenation process type etc. residual liquid. The treatment process of the invention can recover and obtain hexachlorodisilane with a purity of more than 98%.
Description
Technical field
The present invention relates to a kind of recovery and periodical operation method and the device of purification disilicone hexachloride from 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 to great harm.Chlorosilane raffinate becomes the bottleneck problem that allows many polysilicon enterprise's headaches and limit polysilicon industry development at present.
By cold (heat) hydrogenation slag slurry and distillation residual liquid, synthetic furnace distillation residual liquid, reduction furnace distillation residual liquid etc. having been done to the pertinent literature research of a large amount of home and abroads and to after the detection of indivedual samples, substantially having been determined that chlorosilane raffinate is mainly 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.The high boiling material of mentioning in patent EP0634418 more than Si2Cl6 boiling point can be used for producing the Chemicals such as heat-transfer fluid, lubricant, silicon rubber, resin, sealed binder, also has certain recovery value.In addition it should be noted that the large hexachloro-silane of proportion that the height in 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, in addition Si2Cl6 is also a kind of extremely highly active reductor, 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, raffinate hydrolysis can cause huge waste, particularly along with the continuous expansion of polysilicon output, the raffinate rationally not reclaimed is multiplied, if high added value component, particularly hexachloro-silane in energy efficient recovery raffinate, will make enterprise establish oneself in an unassailable position in current fierce polysilicon market competition.But, because impurity in the chlorosilane raffinate containing cold hydrogenation process, synthesis procedure is many, organochlorosilane, as trichloromethyl silane (70.2 ℃ of boiling points) and silicon tetrachloride (56.8 ℃ of boiling points), titanium tetrachloride (136 ℃ of boiling points) approach again with hexachloro-silane (145 ℃ of boiling points), requires very high to reclaiming 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 used in urao and remaining raffinate and solid slag after reclaiming, 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 processing production of polysilicon, cold (heat) hydrogenation slag slurry and distillation residual liquid, synthesis procedure distillation residual liquid, reduction furnace distillation residual liquid form, reclaim various valuable components in raffinate and, as silicon tetrachloride and high boiling point silicon oil, particularly there is the hexachloro-silane of high value.Comprehensive above requirement, the situation few according to raffinate treatment capacity, the invention provides a kind of from chlorosilane raffinate periodical operation method and the device of recovery and purification disilicone hexachloride.
Technical scheme of the present invention is as follows:
From chlorosilane raffinate, reclaim 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 at the bottom of minute rectifying tower (6) tower, being provided with just minute rectifying tower kettle-type reboiler (1), just dividing rectifying tower kettle-type reboiler (1) top to be provided with the feed entrance of chlorosilane raffinate (8), the just top of minute rectifying tower kettle-type reboiler (1) connection high boiling material silicone oil removes drip washing pipeline (9), just on minute rectifying tower kettle-type reboiler (1), be provided with the entrance of low-pressure steam pipeline (10) and high pressure steam line (11), just minute rectifying tower (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 (6) condenser arranges a just minute product pipeline (13) and is connected to batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) bottom is provided with batch fractionating tower kettle-type reboiler (2), on batch fractionating tower kettle-type reboiler (2), be provided with low-pressure steam pipeline (16), 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 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 batch fractionating mode, by low-pressure steam pipeline (10), use low-pressure steam as thermal source, chlorosilane in raffinate distills successively by boiling point, when tower top starts from equilibrium temperature to rise, by tower top tail gas and vacuum lines (12), start to vacuumize gradually the light constituent chlorosilane in chlorosilane raffinate (8), organochlorosilane, hexachloro-silane finally carries out further separation by boiling point 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) successively, after hexachloro-silane has steamed in high boiling material, to high pressure steam line (11), through high boiling material silicone oil, go drip washing pipeline (9) to send to drip washing high boiling point silicon oil gasification substance in chlorosilane raffinate (8) heating steam plugging, evaporation finishes rear tower reactor residual powder and draws off by extracting just minute rectifying tower kettle-type reboiler (1) heating tubulation out,
2). just divide product through just dividing a product pipeline (13) to enter batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) is used low-pressure steam as thermal source by low-pressure steam pipeline (16), chlorosilane in raffinate distills successively by boiling point, when tower top starts from equilibrium temperature to rise, by tower top tail gas and vacuum lines (14), start to vacuumize gradually, raffinate light constituent chlorosilane in batch fractionating tower (7) tower reactor, organochlorosilane, hexachloro-silane reclaims respectively and enters chlorosilane storage tank (3) through product pipeline (15) from batch fractionating tower (7) overhead condenser by boiling point successively, organosilane storage tank (4), hexachloro-silane storage tank (5).
Within described first minute, rectifying tower (6) working pressure is 0 ~ 80KPa, and tower top temperature is 30 ~ 105 ℃, and 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.
In the time of rectifying tower (6) use low-pressure steam heating in described first minute, through chlorine material pipeline (17), pass into a certain amount of chlorine, when thermal source switches to middle pressure steam, through nitrogen material pipeline (18), pass into the chlorine of nitrogen replacement remnants, increase 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 the raffinates such as cold hydrogenation process raffinate and 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 providing in the situation that raffinate treatment capacity is low is provided in the present invention.
[4] the present invention can be used and be take low-pressure steam as the type of heating that main heat source, middle pressure steam are 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 in minute tower (6) use low-pressure steam heating, through chlorine material pipeline (17), passing into a certain amount of chlorine, when thermal source switches to middle pressure steam, through nitrogen material pipeline (18), pass into the chlorine of a certain amount of nitrogen replacement remnants, with this, increase hexachloro-silane yield.
Accompanying drawing explanation
Fig. 1: intermittent type chlorosilane raffinate recycling technical scheme schema of the present invention.
Embodiment
Below in conjunction with Fig. 1, 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 at the bottom of minute rectifying tower (6) tower, being provided with just minute rectifying tower kettle-type reboiler (1), just dividing rectifying tower kettle-type reboiler (1) top to be provided with the feed entrance of chlorosilane raffinate (8), the just top of minute rectifying tower kettle-type reboiler (1) connection high boiling material silicone oil removes drip washing pipeline (9), just on minute rectifying tower kettle-type reboiler (1), be provided with low-pressure steam pipeline (10) and high pressure steam line (11), just minute rectifying tower (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 (6) condenser arranges a just minute product pipeline (13) and is connected to batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) bottom is provided with batch fractionating tower kettle-type reboiler (2), on batch fractionating tower kettle-type reboiler (2), be provided with low-pressure steam pipeline (16), 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 batch fractionating mode, by low-pressure steam pipeline (10), use low-pressure steam as thermal source, in tower, through chlorine material pipeline (17), pass into chlorine simultaneously, chlorosilane in raffinate distills successively by boiling point, when tower top starts from 55 ~ 60 ℃ of equilibrium temperatures to rise, by tower top tail gas and vacuum lines (12), start to be evacuated to gradually vacuum tightness 80KPa, light constituent chlorosilane in chlorosilane raffinate (8), organochlorosilane, hexachloro-silane finally carries out further separation by boiling point 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) successively, after in high boiling material, hexachloro-silane has steamed, by heating steam plugging to high pressure steam line (11), in tower, through nitrogen material pipeline (18), pass into the chlorine of nitrogen replacement remnants simultaneously, through high boiling material silicone oil, go drip washing pipeline (9) to send to drip washing high boiling point silicon oil gasification substance in chlorosilane raffinate (8), evaporation finishes rear tower reactor residual powder through just dividing a rectifying tower kettle-type reboiler (1) to draw off.Just minute product is through just dividing a product pipeline (13) to enter batch fractionating tower kettle-type reboiler (2), batch fractionating tower (7) is used low-pressure steam as thermal source by low-pressure steam pipeline (16), chlorosilane in raffinate distills successively by boiling point, when tower top starts from 55 ~ 60 ℃ of equilibrium temperatures to rise, by tower top tail gas and vacuum lines (14), start to be evacuated to gradually vacuum tightness 80KPa, raffinate light constituent chlorosilane in batch fractionating tower (7) tower reactor, organochlorosilane, hexachloro-silane reclaims respectively and enters chlorosilane storage tank (3) through product pipeline (15) from batch fractionating tower (7) overhead condenser by boiling point successively, organosilane storage tank (4), hexachloro-silane storage tank (5), the hexachloro-silane obtaining needs low temperature, ground connection, nitrogen-sealed stores.
Technology and equipment of the present invention is applicable to recycle the chlorosilane raffinate producing in polysilicon production process, in order to illustrate that better the present invention is in the advantage aspect resource maximization, chooses an application example and is illustrated.
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 (1) working pressure is 0 ~ 80KPa(vacuum tightness), tower top temperature is 30 ~ 105 ℃, 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, by embodiment, be described, person skilled obviously can be changed system and method as herein described or suitably change and combination within not departing from content of the present invention, spirit and scope, realizes technology of the present invention.Special needs to be pointed out is, all similar replacements 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)
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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 |
| CN104096368A (en) * | 2014-07-23 | 2014-10-15 | 安庆市东徽机械有限公司 | Reboiler |
| CN104841195A (en) * | 2015-06-02 | 2015-08-19 | 中国恩菲工程技术有限公司 | Purification and recovery device for chlorosilane waste liquid and purification and recovery method for chlorosilane waste liquid |
| CN105037414A (en) * | 2015-07-29 | 2015-11-11 | 湖北兴瑞化工有限公司 | Method and device for recovering efficient high-boiling substance from organic silicon residue slurry |
| 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 |
| CN109126358B (en) * | 2017-06-27 | 2024-02-20 | 昆明先导新材料科技有限责任公司 | Purification process and purification device for special gas |
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Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59195519A (en) * | 1983-04-15 | 1984-11-06 | Mitsui Toatsu Chem Inc | Manufacture of hexachlorodisilane |
| KR100731558B1 (en) * | 2000-08-02 | 2007-06-22 | 미쯔비시 마테리알 폴리실리콘 가부시끼가이샤 | Method for producing dihexachloride |
| JP2006169012A (en) * | 2004-12-13 | 2006-06-29 | Sumitomo Titanium Corp | Hexachlorodisilane and method of producing the same |
| SG174957A1 (en) * | 2009-03-30 | 2011-11-28 | Denki Kagaku Kogyo Kk | Method for collection of hexachlorodisilane and plant for the method |
| CN101538045A (en) * | 2009-04-21 | 2009-09-23 | 天津大学 | Trichlorosilane differential pressure coupling rectification system and operation method thereof |
| CN102234112B (en) * | 2010-09-30 | 2012-06-27 | 河南尚宇新能源股份有限公司 | Method for rectifying trichlorosilane |
| CN202011749U (en) * | 2011-03-24 | 2011-10-19 | 成都化工股份有限公司 | Novel batch-type rectifying tower system |
| CN102649019B (en) * | 2012-04-17 | 2014-10-22 | 中国恩菲工程技术有限公司 | Trichlorosilane rectification system |
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2013
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