CN1330569C - Process for pressure purification of silicon trichlorohydrgen and apparatus thereof - Google Patents
Process for pressure purification of silicon trichlorohydrgen and apparatus thereof Download PDFInfo
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- CN1330569C CN1330569C CNB2005102003344A CN200510200334A CN1330569C CN 1330569 C CN1330569 C CN 1330569C CN B2005102003344 A CNB2005102003344 A CN B2005102003344A CN 200510200334 A CN200510200334 A CN 200510200334A CN 1330569 C CN1330569 C CN 1330569C
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- Prior art keywords
- trichlorosilane
- purification tower
- purification
- silicon tetrachloride
- liquid
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- 238000000746 purification Methods 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 6
- 229910052710 silicon Inorganic materials 0.000 title claims description 6
- 239000010703 silicon Substances 0.000 title claims description 6
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000005052 trichlorosilane Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 21
- 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 claims abstract description 20
- 238000009835 boiling Methods 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 239000005046 Chlorosilane Substances 0.000 claims abstract description 7
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000009833 condensation Methods 0.000 claims abstract description 7
- 230000005494 condensation Effects 0.000 claims abstract description 7
- 239000007791 liquid phase Substances 0.000 claims abstract description 6
- 238000009834 vaporization Methods 0.000 claims abstract description 5
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 claims description 15
- 229910003902 SiCl 4 Inorganic materials 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000012071 phase Substances 0.000 claims description 7
- 230000008016 vaporization Effects 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 2
- 238000004821 distillation Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000007710 freezing Methods 0.000 abstract description 2
- 230000008014 freezing Effects 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract 6
- 239000012808 vapor phase Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 4
- 229920005591 polysilicon Polymers 0.000 description 4
- 238000012423 maintenance Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000282326 Felis catus Species 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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Abstract
The present invention relates to a method and a device for purifying trichlorosilane by pressurization. A mixed solution of trichlorosilane, silicon tetrachloride and chlorosilane to be purified is introduced into the charging inlet of a purification tower, and the mixed solution flows downwards from the purification tower to a distillation still, wherein the pressure of the distillation still ranges from 0.15MPa to 1.5MPa, and the temperature of the distillation still ranges from 70 DEG C to 200 DEG C; then, steam from the distillation still is introduced into the purification tower for the exchange and separation of heat and ingredients, operating temperature in the purification tower ranges from 40 DEG C 150 DEG C, trichlorosilane ingredients with low boiling points are gathered in a vapor phase, and silicon tetrachloride ingredients with high boiling points are gathered in a liquid phase; vaporisation and condensation are carried out for many times, and trichlorosilane vaporized ingredients are finally obtained in the vapor pahse; then, the trichlorosilane vaporized ingredients are introduced into a water condenser at the top of the purification tower, and the trichlorosilane vaporized ingredients are cooled by circulating water and are condensed into trichlorosilane liquid. The method can increase yield of purification towers with the same tower diameter by 50%, equipment investment and equipment operating cost for freezing are reduced, the heat exchange efficiency of the water condenser at the top of the purification tower is improved by about 15%, and energy consumption is greatly reduced.
Description
(1), technical field
The present invention relates to a kind of method of purification and device thereof of method of purification and equipment thereof, particularly a kind of trichlorosilane of chemical materials.
(2), background technology
Polysilicon is a raw material of producing computer chip and semiconducter device, is called as " foundation stone of Microelectronics Building ", and trichlorosilane (SiHcl
3) purification techniques is one of gordian technique of producing polysilicon.Existing trichlorosilane purifying technique is linked in sequence by still kettle, purification tower and overhead condenser and forms, and belongs to highly energy-consuming technology, and the proportion that energy charge accounts for total cost is very big.Along with the exhaustion day by day of worldwide petroleum resources, energy prices go up significantly, and the production cost of this technology is also corresponding to be increased greatly, and some developed countries have been unwilling to continue to increase input on this high energy-consuming industry, shift to developing country gradually.Siemens adopts the normal pressure process for separating and purifying in the purification of trichlorosilane, when adopting this explained hereafter, overhead condensation needs to freeze system with 7 ℃ of water-cooleds, therefore, need 7 ℃ of water-cooleds of investment construction to freeze system, make this method working cost and maintenance cost height, investment is high, energy consumption is high, causes the trichlorosilane production cost high.
(3), summary of the invention
The purpose of this invention is to provide a kind of Trichlorosilane Pressurizing Purifying Method And Device, solve that existing trichlorosilane purifying technology parameter is unreasonable, energy consumption is high, working cost and maintenance cost height, the high problem of investment.
Technical scheme of the present invention: this process for pressure purification of silicon trichlorohydrgen is characterized in that its method and technical parameter are as follows:
(1), trichlorosilane (SiHCl that will be to be purified
3) and silicon tetrachloride (SiCl
4) the charging opening of chlorosilane mixed solution input purification tower, mixed solution flow to still kettle under purification tower;
(2), add thermal still to 70 ℃～200 ℃, make the mixing liquid of trichlorosilane and silicon tetrachloride be distilled and produce vaporization, the still kettle control pressure is 0.15MPa～1.5MPa with heating agent;
(3), the boil-off of coming out from the still kettle steam discharge pipe enters the purification tower by pipe connecting, the service temperature in the purification tower is 40～150 ℃, from the SiHCl of still kettle
3, SiCl
4The exchange of on the sieve plates at different levels of purification tower, carrying out heat and composition of mixing boil-off with separate, the enrichment in vapour phase of low-boiling trichlorosilane component, silicon tetrachloride component enrichment in liquid phase that boiling point is high, through repeatedly partly vaporizing or partial condensation, finally in vapour phase, obtain volatile, purer trichlorosilane vaporized component, in purification tower, obtain the high silicon tetrachloride component of boiling point;
(4), the trichlorosilane vaporized component of coming out from purification tower enters the overhead water condenser by conduit, the overhead water condenser adopts the ordinary cycle water cooling, the trichlorosilane vaporized component is condensed into liquid, promptly low-boiling trichlorosilane liquid through cooling;
(5), discharge more difficult evaporable silicon tetrachloride liquid from the liquid discharge pipe of still kettle.
Heating agent described in above-mentioned (2) is steam, hot water or thermal oil.
Trichlorosilane SiHCl to be purified described in above-mentioned (1)
3With silicon tetrachloride SiCl
4The charging opening of chlorosilane mixed solution by purification tower between the 8th to the 35th block of column plate of purification tower, add.
Still kettle, purification tower and overhead water condenser polyphone that above-mentioned two covers or two covers are above form slightly the heating up in a steamer of pressurization continuously, rectifying and purifying system.
This trichlorosilane pressurization purifying plant, purification tower is a sieve-plate structure, have charging opening on the tower side wall, it is characterized in that: be connected in series in proper order by still kettle, purification tower and overhead water condenser, the steam discharge pipe of still kettle is communicated with purification tower through pipe connecting, the purification tower top is communicated with the overhead water condenser through conduit, and the bottom vent pipe of above-mentioned still kettle and purification tower is communicated with the silicon tetrachloride liquid storage tank, and the liquid discharge pipe of overhead water condenser bottom is communicated with the trichlorosilane storage tank.
The position of charging opening is between the 8th to the 35th block of column plate of purification tower on the above-mentioned purification tower.
The present invention has utilized SiHCl
3, SiCl
4Boiling point with working pressure raise increase, ultimate principle that the relative volatility of the two is directly proportional with boiling-point difference.SiHCl
3, SiCl
4Mixture under the pressurized operation condition of still kettle, gas phase raises with pressure, density increases, viscosity increases; Liquid phase raises with pressure, and service temperature improves, and density of liquid phase reduces, and viscosity reduces.The plate efficiency liquid body viscosity influence of rectification and purification tower is big, and viscosity reduces, and total tray efficiency rises, and helps SiHCl
3And SiCl
4Separation.The present invention is increased to 0.15Mpa～1.5Mpa with the pressure range of still kettle; The operating temperature range of purification still kettle is increased to 70～200 ℃; Operating temperature range in the purification tower is increased to 40～150 ℃; Change 7 ℃ of refrigerated waters of overhead water condenser the water cooling of into employing ordinary cycle.And designed the equipment that is fit to upward pressure, temperature condition.
After the present invention has strengthened the pressure of purification tower,, help SiCl owing to rectification and purification pressure height, temperature height
4And SiHCl
3Separation, through impurity separating effects such as B, P relatively, separate BCl
3Than normal pressure purification tower remarkable advantages is arranged with the pressurization purification tower.Under the condition of pressurization, BCl
3Deng lower-boiling impurity muriate every plate enrichment multiple and accumulation rate than condition of normal pressure height, BCl
3Almost eliminate at cat head.After adopting technology of the present invention, can strengthen production system and equipment, the rectifying tower output of same tower diameter improves 50%; Changing 7 ℃ of water coolants is normal temperature ordinary cycle cooling process, has reduced freezing required facility investment and equipment working cost, and under the pressurized conditions, it is about 15% that the heat exchange efficiency of interchanger improves, and helps saving cold consumption.
The present invention uses in the embodiment that produces 2000 tons of trichlorosilanes per year, saves refrigeration system and invests 1,200,000 yuan.Save working cost: product per ton can be saved cold 107 * 10
4Kcal saves power consumption of refrigerating 300kWh/t.Under the pressurized conditions, it is about 15% that the heat exchange efficiency of interchanger improves, and under the condition of equal production capacity, equipment can reduce 15%, reduces facility investment and occupation area of equipment thus.
The present invention removes some electrically active impurities through purifying technique, carbon and transition element impurity, make the purity of SiHC13 reach semiconductor grade standard-required, the separation that is applicable to all trichlorosilanes is purified, and is applicable to that the trichlorosilane in the production of polysilicon of solar battery grade polysilicon production and unicircuit level slightly heats up in a steamer and rectification and purification.
(4), description of drawings
Fig. 1 is the structural representation of trichlorosilane pressurization purifying plant of the present invention.
Among the figure: 1-still kettle, 2-purification tower, 3-overhead water condenser, 4-pipe connecting, 5-conduit, 6-silicon tetrachloride liquid storage tank, 7-trichlorosilane storage tank, 8-charging opening.
(5), embodiment
Embodiment is referring to Fig. 1, and still kettle 1 adopts the shell and tube heat exchanger that is suitable for the distillation procedure condition, operation of equipment pressure range: 0.15Mpa～1.5Mpa, operating temperature range: 70～200 ℃.Add thermal still 1 with steam, hot water or heat conduction wet goods heating agent, make the trichlorosilane and the silicon tetrachloride liquid vaporization that are distilled, the steam that is vaporized enters in the purification 2 by pipe connecting 4.
In the tower of purification tower 2 is the sieve-board type structure, operation of equipment pressure range: 0.15Mpa～1.5Mpa; Operating temperature range: 40～150 ℃.SiHCl from still kettle 1
3, SiCl
4The mixing steam exchange of on the sieve plates at different levels of purification tower, carrying out heat and composition with separate low-boiling component (SiHCl
3) enrichment in vapour phase, the component (SiCl that boiling point is high
4) enrichment in liquid phase, through repeatedly partly vaporizing or partial condensation, finally in vapour phase, obtain purer volatile components (SiHCl
3), in still kettle, obtain the high component (SiCl of boiling point
4), SiHCl to be purified
3, SiCl
4The charging opening 8 of mixed solution between the 8th to the 33rd block of column plate of purification tower 2 adds.
This trichlorosilane pressurization purifying plant, be connected in series by still kettle 1, purification tower 2 and overhead water condenser 3 orders, the steam discharge pipe of still kettle 1 is communicated with purification tower 2 through pipe connecting 4, the purification tower top is communicated with overhead water condenser 3 through conduit 5, the bottom vent pipe of above-mentioned still kettle 1 and purification tower 2 is communicated with silicon tetrachloride liquid storage tank 6, the liquid discharge pipe of overhead water condenser 3 bottoms is communicated with trichlorosilane storage tank 7, and above-mentioned overhead water condenser is the ortho-water condenser.
The position of charging opening 8 is between the 8th to the 35th block of column plate of purification tower on the purification tower.SiHCl
3, SiCl
4Chlorosilane mixed solution charging opening between the 8th to the 33rd block of column plate of purification tower adds, and filling tube is communicated with chlorosilane mixed solution storage tank.
Two covers or above still kettle, purification tower and the overhead water condenser of two covers are made up, can form slightly the heating up in a steamer of continuous pressurization, rectifying and purifying system, can satisfy trichlorosilane and silicon tetrachloride purifying technique that different purity requires.
Claims (4)
1. process for pressure purification of silicon trichlorohydrgen is characterized in that its method and technical parameter are as follows:
(1), trichlorosilane (SiHCl that will be to be purified
3) and silicon tetrachloride (SiCl
4) the charging opening of chlorosilane mixed solution input purification tower, mixed solution flow to still kettle under purification tower;
(2), add thermal still to 70 ℃～200 ℃, make the mixing liquid of trichlorosilane and silicon tetrachloride be distilled and produce vaporization, the still kettle control pressure is 0.15MPa～1.5MPa with heating agent;
(3), the boil-off of coming out from the still kettle steam discharge pipe enters the purification tower by pipe connecting, the service temperature in the purification tower is 40～150 ℃, from the SiHCl of still kettle
3, SiCl
4The exchange of on the sieve plates at different levels of purification tower, carrying out heat and composition of mixing boil-off with separate, the enrichment in vapour phase of low-boiling trichlorosilane component, silicon tetrachloride component enrichment in liquid phase that boiling point is high, through repeatedly partly vaporizing or partial condensation, finally in vapour phase, obtain volatile, purer trichlorosilane vaporized component, in purification tower, obtain the high silicon tetrachloride component of boiling point;
(4), the trichlorosilane vaporized component of coming out from purification tower enters the overhead water condenser by conduit, the overhead water condenser adopts the ordinary cycle water cooling, the trichlorosilane vaporized component is condensed into liquid, promptly low-boiling trichlorosilane liquid through cooling;
(5), discharge more difficult evaporable silicon tetrachloride liquid from the liquid discharge pipe of still kettle.
2. process for pressure purification of silicon trichlorohydrgen according to claim 1 is characterized in that: the heating agent described in above-mentioned (2) is steam, hot water or thermal oil.
3. process for pressure purification of silicon trichlorohydrgen according to claim 1 is characterized in that: the trichlorosilane (SiHCl to be purified described in above-mentioned (1)
3) and silicon tetrachloride (SiCl
4) the charging opening of chlorosilane mixed solution by purification tower between the 8th to the 35th block of column plate of purification tower, add.
4. according to claim 1 or 2 or 3 described process for pressure purification of silicon trichlorohydrgen, it is characterized in that: still kettle, purification tower and overhead water condenser polyphone that above-mentioned two covers or two covers are above form slightly the heating up in a steamer of pressurization continuously, rectifying and purifying system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005102003344A CN1330569C (en) | 2005-06-16 | 2005-06-16 | Process for pressure purification of silicon trichlorohydrgen and apparatus thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005102003344A CN1330569C (en) | 2005-06-16 | 2005-06-16 | Process for pressure purification of silicon trichlorohydrgen and apparatus thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1693192A CN1693192A (en) | 2005-11-09 |
| CN1330569C true CN1330569C (en) | 2007-08-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005102003344A Active CN1330569C (en) | 2005-06-16 | 2005-06-16 | Process for pressure purification of silicon trichlorohydrgen and apparatus thereof |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101357292B (en) * | 2007-07-31 | 2012-07-04 | 中国恩菲工程技术有限公司 | Method for recovering tail-gas generated during producing polycrystalline silicon using silicon tetrachloride |
| CN101372335B (en) * | 2007-08-20 | 2011-08-10 | 中国恩菲工程技术有限公司 | Method for preparing polysilicon |
| KR101292545B1 (en) * | 2009-12-28 | 2013-08-12 | 주식회사 엘지화학 | Apparatus for purifying trichlorosilane and method of purifying trichlorosilane |
| CN102101672A (en) * | 2011-01-10 | 2011-06-22 | 华陆工程科技有限责任公司 | Control method for stably adjusting purity of trichlorosilane |
| CN102417182A (en) * | 2011-08-30 | 2012-04-18 | 沁阳市瑞元物资有限公司 | Separation device and method for purifying trichlorosilane in high-low-boiling-point substances |
| CN102502654A (en) * | 2011-10-20 | 2012-06-20 | 中国恩菲工程技术有限公司 | Method for treating solution containing silicon tetrachloride |
| CN102381712A (en) * | 2011-10-20 | 2012-03-21 | 中国恩菲工程技术有限公司 | Equipment for treating solution containing silicon tetrachloride |
| WO2015012257A1 (en) * | 2013-07-26 | 2015-01-29 | 株式会社 テクノ・バンダリー | Continuous-distillation-type trichlorosilane vaporization supply device and continuous-distillation-type trichlorosilane gas vaporization method |
| CN111153925B (en) * | 2019-12-31 | 2022-08-12 | 江西宏柏新材料股份有限公司 | Device and method for continuously purifying 2-cyanoethyl trichlorosilane |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3516803A (en) * | 1966-10-06 | 1970-06-23 | Texas Instruments Inc | Method for the purification of trichlorosilane |
| US4481178A (en) * | 1982-11-08 | 1984-11-06 | General Electric Company | Purification of chlorosilanes |
| JP2000319095A (en) * | 1999-04-30 | 2000-11-21 | Komatsu Electronic Metals Co Ltd | Apparatus and method for vaporizing and supplying trichlorosilane |
| JP2002362917A (en) * | 2001-06-07 | 2002-12-18 | Sumitomo Titanium Corp | Chlorosilane purifying method |
| CN1403372A (en) * | 2002-10-23 | 2003-03-19 | 同济大学 | Method of producing polysilicon with mixed source of trichloro-hydrosilicon and silicon tetrachloride |
-
2005
- 2005-06-16 CN CNB2005102003344A patent/CN1330569C/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3516803A (en) * | 1966-10-06 | 1970-06-23 | Texas Instruments Inc | Method for the purification of trichlorosilane |
| US4481178A (en) * | 1982-11-08 | 1984-11-06 | General Electric Company | Purification of chlorosilanes |
| JP2000319095A (en) * | 1999-04-30 | 2000-11-21 | Komatsu Electronic Metals Co Ltd | Apparatus and method for vaporizing and supplying trichlorosilane |
| JP2002362917A (en) * | 2001-06-07 | 2002-12-18 | Sumitomo Titanium Corp | Chlorosilane purifying method |
| CN1403372A (en) * | 2002-10-23 | 2003-03-19 | 同济大学 | Method of producing polysilicon with mixed source of trichloro-hydrosilicon and silicon tetrachloride |
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|---|---|
| CN1693192A (en) | 2005-11-09 |
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Assignee: Luoyang Zhonggui High-tech Co., Ltd. Assignor: China Non-ferrous Engineering Design General Inst. Contract fulfillment period: 2007.1.1 to 2016.12.31 contract change Contract record no.: 2008410000161 Denomination of invention: Process for pressure purification of silicon trichlorohydrgen and apparatus thereof Granted publication date: 20070808 License type: Exclusive license Record date: 2008.12.3 |
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