CN102642839A - Processing process of industrial grade silicon tetrachloride - Google Patents
Processing process of industrial grade silicon tetrachloride Download PDFInfo
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- CN102642839A CN102642839A CN201210141828XA CN201210141828A CN102642839A CN 102642839 A CN102642839 A CN 102642839A CN 201210141828X A CN201210141828X A CN 201210141828XA CN 201210141828 A CN201210141828 A CN 201210141828A CN 102642839 A CN102642839 A CN 102642839A
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- silicon tetrachloride
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- removing tower
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- 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 title claims abstract description 57
- 239000005049 silicon tetrachloride Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 38
- 239000012535 impurity Substances 0.000 claims abstract description 22
- 239000007787 solid Substances 0.000 claims abstract description 13
- 238000010992 reflux Methods 0.000 claims description 30
- 238000004519 manufacturing process Methods 0.000 claims description 27
- 241000282326 Felis catus Species 0.000 claims description 12
- 239000007792 gaseous phase Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 16
- 238000009835 boiling Methods 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 8
- 238000000746 purification Methods 0.000 abstract description 3
- 230000000903 blocking effect Effects 0.000 abstract description 2
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 238000000605 extraction Methods 0.000 description 14
- 239000000470 constituent Substances 0.000 description 12
- 239000007791 liquid phase Substances 0.000 description 12
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 8
- 229920005591 polysilicon Polymers 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000011345 viscous material Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 2
- 239000005052 trichlorosilane Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- GPATXKGIPSPFHV-UHFFFAOYSA-N Cl[SiH](Cl)Cl.Cl[Si](Cl)(Cl)Cl Chemical compound Cl[SiH](Cl)Cl.Cl[Si](Cl)(Cl)Cl GPATXKGIPSPFHV-UHFFFAOYSA-N 0.000 description 1
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001944 continuous distillation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000407 epitaxy Methods 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
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Abstract
The invention belongs to the field of chemical engineering purification and provides a process processing industrial grade silicon tetrachloride into high-purity silicon tetrachloride. The process comprises the following steps: coarse silicon tetrachloride enters a heavy-removing tower, a produced material at the top of the heavy-removing tower serves as a primary product to enter a buffer tank, and produced materials in a tower kettle of the heavy-removing tower are impurities with a high boiling point and solid impurities; the primary product in the buffer tank enters a light-removing tower, a gas phase material at the top of the light-removing tower serves as a heat source to enter a reboiler of the heavy-removing tower and then is cooled through a condenser, and a produced material of the light-removing tower enters a secondary heavy-removing tower by differential pressure; a produced material of the secondary heavy-removing tower flows back to serve as feed of the heavy-removing tower, and a produced material at the top of the secondary heavy-removing tower is a final product. The process can prevent the solid impurities and sticky materials with the high boiling point in a raw material from blocking a feeding pipe of a follow-up rectification tower, is low in requirements for raw material quality and suitable for processing industrial grade silicon tetrachloride of various different sources, and reduces energy consumption by thermal coupling rectification of the heavy-removing tower and the light-removing tower.
Description
Technical field
The invention belongs to chemical industry purification field, be specifically related to the rectifying of technical grade silicon tetrachloride is obtained the treatment process of high purity silicon tetrachloride.
Background technology
Silicon tetrachloride normal temperature is colourless transparent liquid, density 1.50g/cm down
3, 57.6 ℃ of boiling points are met the water facile hydrolysis and are become silicic acid and hydrogenchloride, and skin is corrosive, and high purity silicon tetrachloride can be used for making preform and high purity quartz and is used for silicon epitaxy etc., is a kind of high value-added product that has.The silicon tetrachloride of technical grade source is very many, as as synthesizing trichlorosilane (HSiCl
3) time by product; As in production of polysilicon, producing a large amount of silicon tetrachloride sub products; Each ton polysilicon just produces the silicon tetrachloride about 10 tons, and therefore, the recoverying and utilizing method of seeking this type of sub product can effectively reduce the production cost and minimizing environmental pollution of polysilicon.Simultaneously, the silicon tetrachloride of technical grade also can obtained through distillation with the chlorine effect more than 200 ℃ by ferrosilicon.
Patent documentation CN 102219222 A disclose a kind of optical fiber and have used the high purity silicon tetrachloride continuous distillation method, and this method is taken off light constituent earlier with thick silicon tetrachloride, take off heavy constituent again, after rectification under vacuum gets high purity silicon tetrachloride, owing to contain HSiCl in the thick silicon tetrachloride
3, HSi
2Cl
5, metal chloride (AlCl
3CuCl
2And FeCl
3Deng), nonmetal muriate (BCl
3And PCl
3Deng), organism (tetrachloroethane, polymkeric substance etc.), complex compound and solid particle polluter, taking off the light constituent step, the viscosity organism and the solid impurity that remain in the thick silicon tetrachloride very easily stop up the feed-pipe that takes off heavies column.Therefore this technology only is applicable to and handles relative heavy constituent, the poor thick silicon tetrachloride of solid impurity.
Patent documentation CN 101920964 B disclose a kind of method for purifying silicon tetrachloride by double-effect distillation, and this method is introduced into spray column with thick silicon tetrachloride, get into lightness-removing column behind the vapor condensation again, get into weight-removing column at last, thereby obtain the product silicon tetrachloride.Though adopt spray column can remove the solid impurity in the thick silicon tetrachloride,, cause the loss of silicon tetrachloride, thereby limited the effect of spray column because silicon tetrachloride and water electrode are prone to react.In addition, thick silicon tetrachloride fails to remove the viscosity organism, makes this method still have the existing blocking pipe problem of preceding method.
Summary of the invention
The objective of the invention is to solve because of heavy constituent in the thick silicon tetrachloride, solid impurity contain the problem that height is prone to cause line clogging, a kind of treatment process that is applicable to the technical grade silicon tetrachloride in various sources is provided.
The present invention realizes that the technical scheme that above-mentioned purpose adopts is following:
The treatment process of technical grade silicon tetrachloride, this process step is following: earlier thick silicon tetrachloride is got into weight-removing column, weight-removing column cat head production gets into surge tank as primary products, and weight-removing column tower still production is high-boiling-point impurity and solid impurity; Primary products in the surge tank pump into lightness-removing column again, and the gaseous phase materials of lightness-removing column cat head is as the reboiler of thermal source entering weight-removing column, and through the condensing surface cooling, lightness-removing column tower still production gets into the secondary weight-removing column through pressure reduction again; Secondary weight-removing column tower still production refluxes as the charging of weight-removing column, and secondary weight-removing column cat head production is the finished product.
Further, the tower still temperature of said weight-removing column is 75～120 ℃, and tower top temperature is 65～100 ℃, and reflux ratio is (6～24): 1.
Further, the tower still temperature of said lightness-removing column is 90～135 ℃, and tower top temperature is 60～100 ℃, and reflux ratio is (35～180): 1.
Further, the tower still temperature of said secondary weight-removing column is 75～110 ℃, and tower top temperature is 65～105 ℃, and reflux ratio is (6～18): 1.
Further, said lightness-removing column tower top pressure is 0.2～0.45MPa, and said secondary weight-removing column tower top pressure is 0.08～0.3MPa.
Three grades of continuous rectifying of process using of the present invention; Thick silicon tetrachloride is earlier after weight-removing column → lightness-removing column → secondary weight-removing column; Weight-removing column and lightness-removing column adopt thermal coupling rectifying simultaneously; Promptly adopt the thermal source of lightness-removing column overhead gas phase materials, realize refining purification and save energy purpose the technical grade silicon tetrachloride as the weight-removing column reboiler.This technology is got rid of the solid impurity in the raw material, high boiling point viscous material with weight-removing column earlier; Prevent that this type of impurity from stopping up the feed pipe of follow-up rectifying tower; Therefore the raw materials quality to thick silicon tetrachloride requires low; Applied widely, can not only handle the silicon tetrachloride by product that is produced when trichlorosilane synthesizes, the silicon tetrachloride by product that is produced in the time of also handling production of polysilicon.Foreign matter content is reduced to ppb (part per billion) level in the prepared silicon tetrachloride the finished product.
Description of drawings
The processing technological flow figure of Fig. 1 technical grade silicon tetrachloride of the present invention.
Among the figure: 1-weight-removing column, 2-lightness-removing column, 3-secondary weight-removing column, (4,5,6)-reboiler, (7,8,9)-condensing surface, 10-surge tank, 11-return tank, 12-reflux pump.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is further specified.
Technical grade silicon tetrachloride of the present invention is the by-product silicon tetrachloride that produced in the production of polysilicon or the trichlorosilane silicon tetrachloride as by-product when synthetic, and this type raw material all is referred to as thick silicon tetrachloride.The theoretical stage of weight-removing column, lightness-removing column and secondary weight-removing column is 45.
Embodiment 1
The thick silicon tetrachloride of 85 (quality) % is got into weight-removing column with the flow of 2000kg/h; Tower still temperature is controlled at 75 ℃, and tower top temperature is controlled at 65 ℃, and reflux ratio is 6:1; The gaseous phase materials of cat head is transformed into liquid phase through condensing surface; The liquid phase material partial reflux weight-removing column that obtains, the part extraction gets into surge tank as primary products and with the flow of 1700kg/h, and the material part of tower still is returned weight-removing column through reboiler; Another part is extraction then, and tower still production is high boiling point viscous substance and solid impurities such as polymkeric substance and complex compound.Primary products in the surge tank get into lightness-removing column with pump delivery again, and tower still temperature is controlled at 90 ℃, and tower top temperature is controlled at 60 ℃; Tower top pressure is 0.2MPa, reflux ratio 35:1, and the material part of tower still is returned lightness-removing column through reboiler; Another part extraction, production gets into the secondary weight-removing column with the flow of 1500kg/h, and the gaseous phase materials of cat head is mainly lower boiling light constituent impurity; This gaseous phase materials through the reboiler 4 of weight-removing column, for reboiler provides heat, gets into return tank 11 earlier again after the condensing surface 8 of lightness-removing column is condensed into liquid phase; Make partial reflux be back to lightness-removing column through reflux pump, another part production is then as the raw material of producing polysilicon.Secondary weight-removing column tower still temperature is controlled at 75 ℃, and tower top temperature is controlled at 65 ℃, tower top pressure 0.08MPa; With the charging of thick silicon tetrachloride as weight-removing column, all the other heavy constituent materials return the secondary weight-removing column through reboiler to the material that reflux ratio 6:1, tower still production are mainly the heavy constituent foreign material with the 100kg/h flow; The overhead gas phase materials is a liquid phase through condenser condenses; Partial reflux secondary weight-removing column, the part extraction, production is limited to highly purified silicon tetrachloride.
The thick silicon tetrachloride of 95 (quality) % is got into weight-removing column with the flow of 2000kg/h; Tower still temperature is controlled at 100 ℃, and tower top temperature is controlled at 88 ℃, reflux ratio 20:1; The gaseous phase materials of cat head is transformed into liquid phase through condensing surface; The liquid phase material partial reflux weight-removing column that obtains, the part extraction gets into surge tank as primary products and with the flow of 1700kg/h, and the material part of tower still is returned weight-removing column through reboiler; Another part is extraction then, and tower still production is high boiling viscous substance and solid impurities such as polymkeric substance and complex compound.Primary products in the surge tank get into lightness-removing column with pump delivery again, and tower still temperature is controlled at 114 ℃, and tower top temperature is controlled at 85 ℃; Tower top pressure 0.37MPa, reflux ratio 150:1, the material part of tower still is returned lightness-removing column through reboiler; Another part extraction, production gets into the secondary weight-removing column with the flow of 1500kg/h, and the gaseous phase materials of cat head is mainly lower boiling light constituent impurity; This gaseous phase materials through the reboiler 4 of weight-removing column, for reboiler provides heat, gets into return tank 11 earlier again after the condensing surface 8 of lightness-removing column is condensed into liquid phase; Make partial reflux be back to lightness-removing column through reflux pump, another part production is then as the raw material of producing polysilicon.Secondary weight-removing column tower still temperature is controlled at 94 ℃, and tower top temperature is controlled at 88 ℃, tower top pressure 0.25MPa; With the charging of thick silicon tetrachloride as weight-removing column, rest materials is returned the secondary weight-removing column through reboiler with the 100kg/h flow for reflux ratio 15:1, one one of the material that is mainly heavy constituent impurity of tower still extraction; The overhead gas phase materials is a liquid phase through condenser condenses; Partial reflux secondary weight-removing column, the part extraction, production is highly purified silicon tetrachloride.
The thick silicon tetrachloride of 90 (quality) % is got into weight-removing column with the flow of 2000kg/h; Tower still temperature is controlled at 120 ℃, and tower top temperature is controlled at 100 ℃, reflux ratio 24:1; The gaseous phase materials of cat head is transformed into liquid phase through condensing surface; The liquid phase material partial reflux weight-removing column that obtains, the part extraction gets into surge tank as primary products and with the flow of 1700kg/h, and the material part of tower still is returned weight-removing column through reboiler; Another part is extraction then, and tower still production is high boiling viscous substance and solid impurities such as polymkeric substance and complex compound.Primary products in the surge tank get into lightness-removing column with pump delivery again, and tower still temperature is controlled at 135 ℃, and tower top temperature is controlled at 100 ℃; Tower top pressure 0.45MPa, reflux ratio 180:1, the material part of tower still is returned lightness-removing column through reboiler; Another part extraction, production gets into the secondary weight-removing column with the flow of 1500kg/h, and the gaseous phase materials of cat head is mainly lower boiling light constituent impurity; This gaseous phase materials through the reboiler 4 of weight-removing column, for reboiler provides heat, gets into return tank 11 earlier again after the condensing surface 8 of lightness-removing column is condensed into liquid phase; Make partial reflux be back to lightness-removing column through reflux pump, another part production is then as the raw material of producing polysilicon.Secondary weight-removing column tower still temperature is controlled at 110 ℃, and tower top temperature is controlled at 105 ℃, tower top pressure 0.3MPa; With the charging of thick silicon tetrachloride as weight-removing column, rest materials is returned the secondary weight-removing column through reboiler with the 100kg/h flow for reflux ratio 18:1, one one of the material that is mainly heavy constituent impurity of tower still extraction; The overhead gas phase materials is a liquid phase through condenser condenses; Partial reflux secondary weight-removing column, the part extraction, production is highly purified silicon tetrachloride.
Adopt ICP-MAS to embodiment 1,2,3 prepared high purity silicon tetrachloride impurity element (mass content) analytical resultss
Claims (5)
1. the treatment process of technical grade silicon tetrachloride; It is characterized in that; Process step is following: earlier thick silicon tetrachloride is got into weight-removing column (1), weight-removing column cat head production gets into surge tank (10) as primary products, and weight-removing column tower still production is high-boiling-point impurity and solid impurity; Primary products in the surge tank (10) get into lightness-removing column (2) again; The gaseous phase materials of lightness-removing column cat head gets into the reboiler (4) of weight-removing column (1) as thermal source; Pass through condensing surface (8) cooling again, lightness-removing column tower still production gets into secondary weight-removing column (3) through pressure reduction; Secondary weight-removing column tower still production refluxes as the charging of weight-removing column (1), and secondary weight-removing column cat head production is the finished product.
2. according to the treatment process of the said technical grade silicon tetrachloride of claim 1, it is characterized in that: the tower still temperature of said weight-removing column is 75～120 ℃, and tower top temperature is 65～100 ℃, and reflux ratio is (6～24): 1.
3. according to the treatment process of the said technical grade silicon tetrachloride of claim 1, it is characterized in that: the tower still temperature of said lightness-removing column is 90～135 ℃, and tower top temperature is 60～100 ℃, and reflux ratio is (35～180): 1.
4. according to the treatment process of the said technical grade silicon tetrachloride of claim 1, it is characterized in that: the tower still temperature of said secondary weight-removing column is 75～110 ℃, and tower top temperature is 65～105 ℃, and reflux ratio is (6～18): 1.
5. according to the treatment process of the said technical grade silicon tetrachloride of claim 1, it is characterized in that: said lightness-removing column tower top pressure is 0.2～0.45MPa, and said secondary weight-removing column tower top pressure is 0.08～0.3MPa.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058408A (en) * | 2014-06-26 | 2014-09-24 | 中国恩菲工程技术有限公司 | Method for purifying silicon tetrachloride |
| CN104058407A (en) * | 2014-06-26 | 2014-09-24 | 中国恩菲工程技术有限公司 | Silicon tetrachloride purification system |
| CN104817091A (en) * | 2014-01-30 | 2015-08-05 | 内蒙古盾安光伏科技有限公司 | Treatment process of silicon tetrachloride |
| CN105314638A (en) * | 2015-11-26 | 2016-02-10 | 新疆大全新能源有限公司 | Method and device for recycling silicon tetrachloride and removing high-boiling residues in trichlorosilane synthetic material |
| CN105330135A (en) * | 2015-12-04 | 2016-02-17 | 太仓市建兴石英玻璃厂 | Preparing method for high-purity silica glass |
| CN106927468A (en) * | 2017-04-06 | 2017-07-07 | 洛阳中硅高科技有限公司 | A kind of device for preparing electron level trichlorosilane |
| CN110357150A (en) * | 2019-08-08 | 2019-10-22 | 中国恩菲工程技术有限公司 | Titanium tetrachloride rectificating method |
| CN114835130A (en) * | 2022-06-30 | 2022-08-02 | 北京化工大学 | Production method of high-purity quartz |
| CN115196638A (en) * | 2022-07-23 | 2022-10-18 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for removing impurities from silicon tetrachloride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5950016A (en) * | 1982-09-10 | 1984-03-22 | Central Glass Co Ltd | Method for purifying silicon tetrafluoride |
| CN101920964A (en) * | 2010-09-11 | 2010-12-22 | 天津大学 | Method for purifying silicon tetrachloride by double-effect distillation |
| CN102219222A (en) * | 2011-04-22 | 2011-10-19 | 武汉新硅科技有限公司 | Continuous rectification method for high-purity silicon tetrachloride for optical fiber |
-
2012
- 2012-05-09 CN CN 201210141828 patent/CN102642839B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5950016A (en) * | 1982-09-10 | 1984-03-22 | Central Glass Co Ltd | Method for purifying silicon tetrafluoride |
| CN101920964A (en) * | 2010-09-11 | 2010-12-22 | 天津大学 | Method for purifying silicon tetrachloride by double-effect distillation |
| CN102219222A (en) * | 2011-04-22 | 2011-10-19 | 武汉新硅科技有限公司 | Continuous rectification method for high-purity silicon tetrachloride for optical fiber |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817091A (en) * | 2014-01-30 | 2015-08-05 | 内蒙古盾安光伏科技有限公司 | Treatment process of silicon tetrachloride |
| CN104058408A (en) * | 2014-06-26 | 2014-09-24 | 中国恩菲工程技术有限公司 | Method for purifying silicon tetrachloride |
| CN104058407A (en) * | 2014-06-26 | 2014-09-24 | 中国恩菲工程技术有限公司 | Silicon tetrachloride purification system |
| CN104058408B (en) * | 2014-06-26 | 2016-07-06 | 中国恩菲工程技术有限公司 | The method of purification Silicon chloride. |
| CN105314638A (en) * | 2015-11-26 | 2016-02-10 | 新疆大全新能源有限公司 | Method and device for recycling silicon tetrachloride and removing high-boiling residues in trichlorosilane synthetic material |
| CN105314638B (en) * | 2015-11-26 | 2018-01-05 | 新疆大全新能源有限公司 | Silicon tetrachloride recycling and the method and apparatus except high-boiling components in trichlorosilane synthesis material |
| CN105330135A (en) * | 2015-12-04 | 2016-02-17 | 太仓市建兴石英玻璃厂 | Preparing method for high-purity silica glass |
| CN106927468A (en) * | 2017-04-06 | 2017-07-07 | 洛阳中硅高科技有限公司 | A kind of device for preparing electron level trichlorosilane |
| CN110357150A (en) * | 2019-08-08 | 2019-10-22 | 中国恩菲工程技术有限公司 | Titanium tetrachloride rectificating method |
| CN114835130A (en) * | 2022-06-30 | 2022-08-02 | 北京化工大学 | Production method of high-purity quartz |
| CN115196638A (en) * | 2022-07-23 | 2022-10-18 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for removing impurities from silicon tetrachloride |
| CN115196638B (en) * | 2022-07-23 | 2023-05-16 | 中船(邯郸)派瑞特种气体股份有限公司 | Silicon tetrachloride impurity removal method |
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| Publication number | Publication date |
|---|---|
| CN102642839B (en) | 2013-03-06 |
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