CN105731465A - Method and equipment for removing boron and phosphorous by utilizing chlorosilane fixed bed chemical adsorption reaction method - Google Patents
Method and equipment for removing boron and phosphorous by utilizing chlorosilane fixed bed chemical adsorption reaction method Download PDFInfo
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- CN105731465A CN105731465A CN201610112604.4A CN201610112604A CN105731465A CN 105731465 A CN105731465 A CN 105731465A CN 201610112604 A CN201610112604 A CN 201610112604A CN 105731465 A CN105731465 A CN 105731465A
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- chlorosilane
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
- C01B33/10794—Purification by forming addition compounds or complexes, the reactant being possibly contained in an adsorbent
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Abstract
The invention relates to a method and equipment for removing boron and phosphorous by utilizing a chlorosilane fixed bed chemical adsorption reaction method. The equipment comprises a heat exchanger, a fixed bed adsorption column and a heat conduction oil circulation pump; both a feed line at the bottom of the heat exchanger and a discharge line at the top of the heat exchanger are connected with the bottom of a fixed bed; the heat conduction oil circulation pump conveys heat conduction oil as a heat-transfer medium to the fixed bed. A chlorosilane gas phase or a liquid phase firstly enters the heat exchanger and then enters the chemical adsorption fixed bed, an adsorbent loaded with a chemical complexing agent is used for performing chemical adsorption reaction on boron and phosphorous impurities, and finally, high-purity chlorosilane is obtained. With the adoption of the chlorosilane fixed bed chemical adsorption reaction method, the boron and phosphorous impurity removal process is simple, the equipment investment is low, and the boron and phosphorous impurity in the chlorosilane can be effectively removed, so that the purity of the chlorosilane obtained is high. In the purification by utilizing the fixed bed chemical adsorption reaction method, the adsorbent is easy to regenerate and low in cost. The removal of the boron and phosphorous impurities in the chlorosilane by utilizing the fixed bed chemical adsorption reaction method is creatively proposed in China for the first time, so that a foundation is laid for realizing the stable production of electronic-grade polysilicon.
Description
Technical field
The present invention relates to the purification technique field that electronic-grade polycrystalline silicon produces, particularly relate to the removal technique of boron in chlorosilane, phosphorus impurities.Adopt fixing bed Chemisorption method separating-purifying so that product is finally reached the level of polysilicon stable yields electron level；The fixing bed Chemisorption method of a kind of chlorosilane especially set out is except the method and apparatus of boron phosphorus.
Background technology
China's polycrystalline silicon industry is started in the fifties in last century, and the mid-1960s achieves industrialization.The development of electronic information and solar photovoltaic industry has driven the growth of polysilicon demand, particularly under the overall background of domestic solar energy industry high speed development, the newly-increased installation amount of the photovoltaic of continuous blow past expectations drives device requirements vigorous so that the raw material polysilicon demand of upstream increases substantially.Between 2005-2008 4 years, production of polysilicon technology is introduced or developed in domestic various places one after another, introduces kiloton polycrystalline silicon production line, and the market entirety of polysilicon presents thriving trend.Meanwhile, for a long time, China is carried out blockade on new techniques by external polysilicon manufacturer, most domestic enterprise adopt fall behind production technology, so far domestic but without an enterprise can steady production electronic-grade polycrystalline silicon, technical merit still suffers from bigger gap compared with abroad.Overall gap shows that production scale is little, production cost height, and quality is unstable, and environmental pollution is serious, and even many manufacturers were difficult to maintain production in recent years, in succession stopped production.
Improved Siemens is the prevailing technology producing polysilicon now: metallurgical grade silica flour and hydrogen chloride generate trichlorosilane in the reactor, then Trichlorosilane purification is refined, and finally in reduction furnace, trichlorosilane and hydrogen obtain high purity polycrystalline silicon by reduction reaction.Additionally, also can produce substantial amounts of silicon tetrachloride as by-product in reduction furnace, Silicon chloride. is obtained by reacting trichlorosilane with hydrogen, silica flour again, it is achieved recycling of material.Chlorosilane is as the topmost recycle stock in this technique, even if wherein containing the impurity of trace, finally also can affect polysilicon product purity.The major source of impurity is the introducing of metallurgical grade silica flour in technique, including metal chloride, the chloride of boracic phosphorus and hydride and carbonaceous organic material etc., therefore chlorosilane also inevitably exists the trace impurity such as boron, phosphorus, and final products polysilicon quality can be produced tremendous influence by these impurity.
The purification technology of current chlorosilane is mainly rectification method.Domestic general sloughing light impurity and sloughing heavy seeds repeatedly that chlorosilane is carried out, rectifying column progression is many.Owing to the boiling point of partial impurities and chlorosilane is close, also have partial impurities can form azeotropic with chlorosilane, the problems such as energy consumption height, equipment investment expense height, unstable product quality can be brought only by traditional rectification method.The present invention then by fixing bed form, removes the boron in chlorosilane, phosphorus impurities by Chemisorption so that the level of final products polysilicon stable yields electron level, solves a difficult problem for polysilicon enterprise.
Summary of the invention
It is an object of the invention to solve above-mentioned not enough problem, it is provided that a kind of electronic-grade polycrystalline silicon production process is fixed bed form except the chemisorbed impurity removal process of boron, phosphorus impurities, it is achieved the target of stable yields electronic-grade polycrystalline silicon.
For achieving the above object, the fixing bed Chemisorption method of a kind of chlorosilane of the present invention is except the method and apparatus of boron phosphorus, and concrete technical scheme is as follows:
The fixing bed Chemisorption method of a kind of chlorosilane of the present invention is except the equipment of boron, phosphorus, including heat exchanger, ADSORPTION IN A FIXED BED post and heat conduction oil circulating pump；Exchanger base feeding line is all connected with bottom fixing bed with heat exchanger top discharge pipeline, and heat conduction oil circulating pump carries heat transfer medium conduction oil to fixing bed.
The fixing bed Chemisorption method of a kind of chlorosilane of the present invention is except the method for boron, phosphorus, chlorosilane gas phase or liquid phase initially enter heat exchanger, entering back into the fixing bed of chemisorbed, by load, boron, phosphorus impurities are carried out Chemisorption by the adsorbent of chemical complexing agent, finally give high-purity chlorosilane.
It is when chlorosilane is liquid phase, if with liquid form charging, then fixing bed need to be directly entered by heat exchanger cross-line；If with gas phase charging, then steam or other thermal medium need to be passed into heat exchanger shell pass, chlorosilane enters fixing bed by heat exchanger after being gasified.
When chlorosilane is gas phase, if with gas phase charging, then fixing bed need to be directly entered by heat exchanger cross-line；If with liquid form charging, then recirculated water or other cooling medium need to be passed into heat exchanger shell pass, chlorosilane enters fixing bed by heat exchanger tube pass after being condensed.
Described heat exchanger is vertical fixed tube-sheet exchanger, and tube side walks chlorosilane, material bottom in and top out；When needing heating and gasifying material, the thermal medium that adds of shell side is 200kPa (G) saturated vapor, and temperature is 110-200 DEG C, it is necessary to during condensation material, the cooling medium of shell side is 33-43 DEG C of recirculated water.
Described fixing bed is tubulation structure, is filled with adsorbent, chlorosilane material bottom in and top out in tubulation, and shell side passes into conduction oil to regulate and control adsorption temp, and adsorption temp is 20～150 DEG C.Immobilized chemical reaction chelating agent on adsorbent, chemical reaction chelating agent does not react with chlorosilane, can be formed chemically with impurity and thermodynamically high stability complex, and this complex and chlorosilane can be easily separated.
Adsorbent difficulty volatilization and have chemical inertness, uniform particle sizes has bigger specific surface area, is mainly that active silica-alumina oxide, permutite, molecular sieve, activated carbon, silica gel, resin be a kind of or their combination.
Chemical reaction chelating agent includes ammonium pyrrolidine dithiocarboxylate, p-hydroxyazobenzene, triphenylchloromethane, capryl alcohol, benzene-azo-α-naphthalene, AlCl3Chelating agent, nitrile, thioglycolic acid (β naphthalene)-amide be a kind of or their combination or their homologue.
The effect advantage of the present invention illustrates as follows:
[1] the fixing bed Chemisorption method of chlorosilane of the present invention except the technique of boron, phosphorus impurities simple, equipment investment is few, can effectively remove the boron in chlorosilane, phosphorus impurities, and the chlorosilane purity obtained is high.
[2] adsorbent regenerating easily in fixing bed chemiadsorption purification, cost is low.
[3] creative and novelty, utilizing the boron in fixing bed Chemisorption method dechlorination silane, phosphorus impurities is at home first and creationary proposition, creative and novelty；Lay the foundation for realizing stable yields electronic-grade polycrystalline silicon.
Accompanying drawing explanation
Fig. 1 is electronic-grade polycrystalline silicon production process Raw of the present invention when being liquid-phase chlorosilane, and fixing bed Chemisorption method is except the process flow diagram of boron phosphorus.
Fig. 2 is electronic-grade polycrystalline silicon production process Raw of the present invention when being gas phase chlorosilane, and fixing bed Chemisorption method is except the process flow diagram of boron phosphorus.
Wherein: heat exchanger-1, adsorption column-2, heat conduction oil circulating pump-3.
Detailed description of the invention
Below in conjunction with accompanying drawing 1 and accompanying drawing 2, the technical scheme in inventive embodiments is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention.
The fixing bed Chemisorption method of a kind of chlorosilane of the present invention is except the equipment of boron, phosphorus, including heat exchanger, ADSORPTION IN A FIXED BED post and heat conduction oil circulating pump；Exchanger base feeding line is all connected with bottom fixing bed with heat exchanger top discharge pipeline, and heat conduction oil circulating pump carries heat transfer medium conduction oil to fixing bed.
Chlorosilane gas phase or liquid phase initially enter heat exchanger, then enter the fixing bed of chemisorbed from bottom, and by load, boron, phosphorus impurities are carried out Chemisorption by the adsorbent of chemical complexing agent, finally give high-purity chlorosilane.
It is when chlorosilane is liquid phase, if with liquid form charging, then fixing bed need to be directly entered by heat exchanger cross-line；If with gas phase charging, then steam or other thermal medium need to be passed into heat exchanger shell pass, chlorosilane enters fixing bed by heat exchanger after being gasified.
When chlorosilane is gas phase, if with gas phase charging, then fixing bed need to be directly entered by heat exchanger cross-line；If with liquid form charging, then recirculated water or other cooling medium need to be passed into heat exchanger shell pass, chlorosilane enters fixing bed by heat exchanger tube pass after being condensed.
Described heat exchanger is vertical fixed tube-sheet exchanger, and tube side walks chlorosilane, material bottom in and top out；When needing heating and gasifying material, the thermal medium that adds of shell side is 200kPa (G) saturated vapor, and temperature is 110-200 DEG C, it is necessary to during condensation material, the cooling medium of shell side is 33-43 DEG C of recirculated water.
Described fixing bed is tubulation structure, is filled with adsorbent, chlorosilane material bottom in and top out in tubulation, and shell side passes into conduction oil to regulate and control adsorption temp, and adsorption temp is 20～150 DEG C.Immobilized chemical reaction chelating agent on adsorbent, chemical reaction chelating agent does not react with chlorosilane, can be formed chemically with impurity and thermodynamically high stability complex, and this complex and chlorosilane can be easily separated.
Adsorbent difficulty volatilization and have chemical inertness, uniform particle sizes has bigger specific surface area, is mainly that active silica-alumina oxide, permutite, molecular sieve, activated carbon, silica gel, resin be a kind of or their combination.
Chemical reaction chelating agent includes ammonium pyrrolidine dithiocarboxylate, p-hydroxyazobenzene, triphenylchloromethane, capryl alcohol, benzene-azo-α-naphthalene, AlCl3Chelating agent, nitrile, thioglycolic acid (β naphthalene)-amide be a kind of or their combination or their homologue.
Embodiment 1:
The active silica-alumina oxide of load ammonium pyrrolidine dithiocarboxylate it is filled with in fixing bed.Liquid-phase chlorosilane initially enters heat exchanger 1, and generating gasification after heating, the chlorosilane temperature after gasification is 40～110 DEG C；Gas phase chlorosilane enters fixing bed 2 and boron and phosphorus matter is adsorbed, and before purifying, boron, phosphorus content are 0.5%, and after purification, Boron contents is down to 0.05ppb, and phosphorus content is down to 0.1ppb.
Embodiment 2:
The permutite of ammonium pyrrolidine dithiocarboxylate for load filled in fixing bed.Liquid-phase chlorosilane is directly entered fixing bed 2 by heat exchanger cross-line and boron and phosphorus matter is adsorbed, and before purifying, boron, phosphorus content are 0.5%, and after purification, Boron contents is down to 0.05ppb, and phosphorus content is down to 0.1ppb.
Embodiment 3:
The molecular sieve of p-hydroxyazobenzene for load filled in fixing bed.Gas phase chlorosilane initially enters heat exchanger 1, is 40～110 DEG C through condensed liquid-phase chlorosilane temperature；Liquid-phase chlorosilane enters fixing bed 2 and boron and phosphorus matter is adsorbed, and before purifying, boron, phosphorus content are 0.5%, and after purification, Boron contents is down to 0.05ppb, and phosphorus content is down to 0.1ppb.
Embodiment 4:
The active silica-alumina oxide of p-hydroxyazobenzene for load filled in fixing bed.Gas phase chlorosilane is directly entered fixing bed 2 by heat exchanger cross-line and boron and phosphorus matter is adsorbed, and before purifying, boron, phosphorus content are 0.5%, and after purification, Boron contents is down to 0.05ppb, and phosphorus content is down to 0.1ppb.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (9)
1. the fixing bed Chemisorption method of chlorosilane is except an equipment for boron, phosphorus, including heat exchanger, ADSORPTION IN A FIXED BED post and heat conduction oil circulating pump；Exchanger base feeding line is all connected with bottom fixing bed with heat exchanger top discharge pipeline, and heat conduction oil circulating pump carries heat transfer medium conduction oil to fixing bed.
2. the fixing bed Chemisorption method of chlorosilane is except the method for boron, phosphorus, it is characterized in that chlorosilane gas phase or liquid phase initially enter heat exchanger, enter back into the fixing bed of chemisorbed, by load, boron, phosphorus impurities are carried out Chemisorption by the adsorbent of chemical complexing agent, finally give high-purity chlorosilane.
3. method as claimed in claim 2, is characterized in that when chlorosilane is liquid phase, if with liquid form charging, then fixing bed need to be directly entered by heat exchanger cross-line；If with gas phase charging, then steam or other thermal medium need to be passed into heat exchanger shell pass, chlorosilane enters fixing bed by heat exchanger after being gasified.
4. method as claimed in claim 2, is characterized in that when chlorosilane is gas phase, if with gas phase charging, then fixing bed need to be directly entered by heat exchanger cross-line；If with liquid form charging, then recirculated water or other cooling medium need to be passed into heat exchanger shell pass, chlorosilane enters fixing bed by heat exchanger tube pass after being condensed.
5. method as claimed in claim 2, is characterized in that heat exchanger is vertical fixed tube-sheet exchanger, and tube side walks chlorosilane, material bottom in and top out；When needing heating and gasifying material, the thermal medium that adds of shell side is 200kPa (G) saturated vapor, and temperature is 110-200 DEG C, it is necessary to during condensation material, the cooling medium of shell side is 33-43 DEG C of recirculated water.
6. method as claimed in claim 2, is characterized in that fixing bed is tubulation structure, is filled with adsorbent, chlorosilane material bottom in and top out in tubulation, shell side passes into conduction oil to regulate and control adsorption temp, and adsorption temp is 20～150 DEG C.
7. method as claimed in claim 2, it is characterized in that immobilized chemical reaction chelating agent on adsorbent, chemical reaction chelating agent does not react with chlorosilane, can be formed chemically with impurity and thermodynamically high stability complex, this complex and chlorosilane can be easily separated.
8. method as claimed in claim 7, is characterized in that the difficult volatilization of adsorbent and has chemical inertness, and uniform particle sizes has big specific surface area, wraps or their combination a kind of into active silica-alumina oxide, permutite, molecular sieve, activated carbon, silica gel, resin.
9. method as claimed in claim 7, is characterized in that chemical reaction chelating agent includes ammonium pyrrolidine dithiocarboxylate, p-hydroxyazobenzene, triphenylchloromethane, capryl alcohol, benzene-azo-α-naphthalene, AlCl3Chelating agent, nitrile, thioglycolic acid (β naphthalene)-amide be a kind of or their combination or their homologue.
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| CN201610112604.4A CN105731465A (en) | 2016-02-29 | 2016-02-29 | Method and equipment for removing boron and phosphorous by utilizing chlorosilane fixed bed chemical adsorption reaction method |
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Cited By (8)
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| CN110156026A (en) * | 2019-04-26 | 2019-08-23 | 新疆大全新能源股份有限公司 | A kind of purifying technique of polycrystalline silicon raw material |
| CN110743199A (en) * | 2019-11-12 | 2020-02-04 | 新疆东方希望新能源有限公司 | Adsorption equipment for reducing content of boron and phosphorus impurities in chlorosilane |
| CN111036029A (en) * | 2018-10-15 | 2020-04-21 | 新特能源股份有限公司 | Method for recovering waste gas in polycrystalline silicon production process |
| CN111097194A (en) * | 2020-01-05 | 2020-05-05 | 天津大学 | Selective adsorption method and device for purifying dimethyldichlorosilane |
| CN112250073A (en) * | 2020-11-16 | 2021-01-22 | 天津大学 | Method and device of chlorosilane purification system |
| CN113603096A (en) * | 2021-05-26 | 2021-11-05 | 中国科学院过程工程研究所 | Method for adsorbing trace boron and phosphorus impurities in chlorosilane system |
| CN114588877A (en) * | 2022-02-23 | 2022-06-07 | 木林森活性炭江苏有限公司 | Modified activated carbon carrier, liquid-phase chlorosilane impurity-removing adsorbent and production process of adsorbent |
| CN115023407A (en) * | 2020-11-05 | 2022-09-06 | 瓦克化学股份公司 | Process for removing impurities from chlorosilane mixtures |
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| CN114588877A (en) * | 2022-02-23 | 2022-06-07 | 木林森活性炭江苏有限公司 | Modified activated carbon carrier, liquid-phase chlorosilane impurity-removing adsorbent and production process of adsorbent |
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