CN103896280A - Operation method of polycrystalline silicon cold hydrogenation - Google Patents
Operation method of polycrystalline silicon cold hydrogenation Download PDFInfo
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- CN103896280A CN103896280A CN201410118505.8A CN201410118505A CN103896280A CN 103896280 A CN103896280 A CN 103896280A CN 201410118505 A CN201410118505 A CN 201410118505A CN 103896280 A CN103896280 A CN 103896280A
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Abstract
The invention discloses an operation method of polycrystalline silicon cold hydrogenation, and relates to the technical field of polycrystalline silicon production. The targets of impurity removal and hydrogen purification are achieved by a silicon power reaction step, a heat exchange step, a vaporization step, an electric heating step, a gas-solid separation step, a rinsing step, an impurity removal step, a refrigerant freezing step and a gas-liquid separation step. The energy of the material is fully utilized due to full exchange of cold and heat energy, the external energy consumption is greatly reduced, and the problem of pipe blockage of a purification tower is relieved by filtering and rinsing the system material in advance.
Description
Technical field
The invention belongs to technical field of polysilicon production, specifically the present invention relates to a kind of operation method of polysilicon cold hydrogenation.
Background technology
Known, cold hydrogenation is the important component part in polysilicon production process, cold hydrogenation is mainly the silicon tetrachloride as by-product in order to process and recycle polysilicon production process, thus reach improve raw material availability, realize the object that Matter Transfer uses, reduces production costs, reduces environmental pollution; Conventionally in cold hydrogenation operation operation, need silicon tetrachloride and hydrogen first to heat up, reach temperature of reaction, in reactor, react with silica flour, product gas is through the laggard row gas-liquid separation of lowering the temperature; And in current cold hydrogenation process, the needed energy of heating material and refrigerating process is directly to be provided by outside, and material in working cycle self cold and hot energy fully exchange utilize, energy consumption is larger, has caused unnecessary energy dissipation; In Matter Transfer process, the material that cold hydrogenation produces easily causes the problem of purification system line clogging in the time purifying, and has not only improved industrial accident rate and running cost simultaneously, and the problem of solution line clogging also comparatively bothers.
Summary of the invention
In order to overcome the deficiency in background technology, the invention provides a kind of operation method of polysilicon cold hydrogenation, realize material reasonable diffluence, circulation, and reached energy-saving and cost-reducing object.
Realize technical scheme of the present invention as follows:
An operation method for polysilicon cold hydrogenation, comprises silica flour reactions steps, heat exchange, pervaporation step, electrically heated step, gas solid separation step, drip washing, removal of impurity step, the freezing step of refrigerant and gas-liquid separating step, and concrete operation step is as follows:
(1) silica flour reactions steps: silica flour is sent into cold hydrogenation reactor by silica flour transport pipe, produce reactant gases;
(2) heat exchange, pervaporation step: by hydrogen and silicon tetrachloride in proportion respectively after hydrogen interchanger and silicon tetrachloride interchanger, the hot water transporting with vapor condensation waterpipe carries out heat exchange, hot water after heat exchange is discharged from waste pipe, and hydrogen and silicon tetrachloride mixture enter mixing vaporizing chamber and vaporize;
(3) electrically heated step: connect previous step, by previous step obtain hydrogen after vaporization and the mixed gas of silicon tetrachloride after first-class heat exchanger and secondary heat exchanger with cold hydrogenation reactor in the reactant gases heat exchange that produces, after then being heated by electric heater, enter cold hydrogenation reactor and react with silica flour;
(4) gas solid separation step: connect previous step, the reacted product that previous step is obtained by cyclonic separator by the silica flour in reactor product, catalyst solid and gas delivery, silica flour and catalyst solid are got back to cold hydrogenation reactor, gas is undertaken after dust removal by filtration by strainer, by secondary heat exchanger and first-class heat exchanger with from mixing the indoor gas converting heat out of vaporization;
(5) drip washing, removal of impurity step: connect previous step, will in previous step, enter eluting column drip washing from first-class heat exchanger gas out, the impurity under drip washing is discharged from the raffinate pipeline of eluting column bottom; Being lowered the temperature by one-level cold gas liquid/gas separator from eluting column top gas out, enter the gas-liquid separation of one-level water cooler gas-liquid separator, liquid under condensation directly enters purification tower, noncondensable gas enter secondary coolers cooling after, enter the gas-liquid separation of secondary coolers gas-liquid separator, liquid under condensation enters eluting column again, and spray enters the gas of eluting column out from first-class heat exchanger;
(6) the freezing step of refrigerant: connect previous step, enter gas-gas heat exchanger from secondary coolers gas-liquid separator gas out, carry out precooling, then enter the gas-liquid separation of gas-gas heat exchanger gas-liquid separator, it is freezing that isolated gas enters cryocooler;
(7) gas-liquid separation step: connect previous step, freezing previous step rear gas is entered to cryocooler gas-liquid separator to be reached gas-liquid and separates completely, isolated hydrogen enters gas-gas heat exchanger tube side and heats up, and from separating, Hydrogen Line enters systemic circulation use.
The operation method of described polysilicon cold hydrogenation, in heat exchange, pervaporation step, hydrogen and silicon tetrachloride pass through respectively hydrogen interchanger and silicon tetrachloride interchanger by the molar ratio of 1.8:1～3.0:1.
The operation method of described polysilicon cold hydrogenation, in heat exchange, pervaporation step, the temperature that the hot water transporting with vapor condensation waterpipe carries out heat exchange reaches 80～100 DEG C.
The operation method of described polysilicon cold hydrogenation, in electrically heated step, heat-exchange temperature reaches 400～490 DEG C.
The operation method of described polysilicon cold hydrogenation, in electrically heated step, the temperature being heated by electric heater reaches 500～600 DEG C.
The operation method of described polysilicon cold hydrogenation, in gas solid separation step, the temperature of heat exchange reaches 200～280 DEG C.
The operation method of described polysilicon cold hydrogenation, in drip washing, removal of impurity step, is lowered the temperature by one-level cold gas liquid/gas separator from eluting column top gas out, and the temperature of described cooling reaches 200～280 DEG C.
The operation method of described polysilicon cold hydrogenation, in drip washing, removal of impurity step, it is cooling that noncondensable gas enters secondary coolers, and described cooling temperature reaches 40～70 DEG C.
The operation method of described polysilicon cold hydrogenation, in the freezing step of refrigerant, freezing temperature reaches-40～-55 DEG C.
The operation method of described polysilicon cold hydrogenation, from one-level water cooler gas-liquid separator, secondary coolers gas-liquid separator, gas-gas heat exchanger gas-liquid separator, deep-cooling heat exchanger gas-liquid separator separates, liquid is all delivered to purification tower and is carried out component separation, and the required steam of described purification tower is provided by steam-pipe.
By above-mentioned disclosure, the invention has the beneficial effects as follows:
The operation method of polysilicon cold hydrogenation of the present invention, has the following advantages:
1, the present invention is in operation because cold and hot energy fully exchanges, and material self-energy is fully used, and has reduced by a relatively large margin outer energizing quantity consumption;
2, material reasonable diffluence, circulation, reduces unnecessary calorific loss;
3, by advance to system material filtering and drip washing, alleviated purification tower line clogging problem.
Brief description of the drawings
Fig. 1 is structural representation of the present invention;
Fig. 2 is schema of the present invention;
In the drawings: 1, silica flour transport pipe; 2, silicon tetrachloride interchanger; 3, hydrogen interchanger; 4, silicon tetrachloride pipeline; 5, Hydrogen Line; 6, waste pipe; 7, mix vaporizing chamber; 8, electric heater; 9, cold hydrogenation reactor; 10, eluting column; 11, one-level water cooler; 12, one-level water cooler gas-liquid separator; 13, secondary coolers; 14, secondary coolers gas-liquid separator; 15, cryocooler gas-liquid separator; 16, raffinate pipeline; 17, vapor condensation waterpipe; 18, steam-pipe; 19, purification tower; 20, cryocooler; 21, gas-gas heat exchanger gas-liquid separator; 22, separate rear Hydrogen Line; 23, gas-gas heat exchanger; 24, strainer; 25, cyclonic separator; 26, secondary heat exchanger; 27, first-class heat exchanger.
Embodiment
Can explain in more detail the present invention by the following examples, the present invention is not limited to the following examples; Disclose object of the present invention and be intended to protect all changes and improvements in the scope of the invention.
The operation method of described polysilicon cold hydrogenation, comprises silica flour reactions steps, heat exchange, pervaporation step, electrically heated step, gas solid separation step, drip washing, removal of impurity step, the freezing step of refrigerant and gas-liquid separating step, and concrete operation step is as follows:
(1) silica flour reactions steps: silica flour is sent into cold hydrogenation reactor 9 by silica flour transport pipe 1, produce reactant gases;
(2) heat exchange, pervaporation step: the molar ratio that hydrogen and silicon tetrachloride are pressed to 1.8:1～3.0:1 is respectively after hydrogen interchanger 3 and silicon tetrachloride interchanger 2, the hot water transporting with vapor condensation waterpipe 13 carries out heat exchange, and the temperature of described heat exchange reaches 80～100 DEG C; Hot water after heat exchange is discharged from waste pipe 6, and hydrogen and silicon tetrachloride mixture enter mixing vaporizing chamber 7 and vaporize;
(3) electrically heated step: connect previous step, by previous step obtain hydrogen after vaporization and the mixed gas of silicon tetrachloride after first-class heat exchanger 27 and secondary heat exchanger 26 with the reactant gases heat exchange of cold hydrogenation reactor 9 interior generations, described heat-exchange temperature reaches 400～490 DEG C; Then heated by electric heater 8, the temperature of described heating reaches after 500～600 DEG C, enters cold hydrogenation reactor 9 and reacts with silica flour;
(4) gas solid separation step: connect previous step, the reacted product that previous step is obtained passes through cyclonic separator 25 by the silica flour in reactor product, catalyst solid and gas delivery, silica flour and catalyst solid are got back to cold hydrogenation reactor 9, gas is undertaken after dust removal by filtration by strainer 24, by secondary heat exchanger 26 and first-class heat exchanger 27 with from mixing in vaporizing chamber 7 gas converting heat out; The temperature of described heat exchange reaches 200～280 DEG C;
(5) drip washing, removal of impurity step: connect previous step, will in previous step, enter eluting column 10 drip washing from first-class heat exchanger 27 gas out, the impurity under drip washing is discharged from the raffinate pipeline 16 of eluting column 10 bottoms; Being lowered the temperature by one-level cold gas liquid/gas separator 11 from eluting column 10 tops gas out, the temperature of described cooling reaches 70～90 DEG C; Enter 12 gas-liquid separations of one-level water cooler gas-liquid separator, the liquid under condensation directly enters purification tower 19, noncondensable gas enter secondary coolers 13 cooling after, described cooling temperature reaches 40～70 DEG C; Enter 14 gas-liquid separations of secondary coolers gas-liquid separator, the liquid under condensation enters eluting column 10 again, and spray enters the gas of eluting column 10 out from first-class heat exchanger 27;
(6) the freezing step of refrigerant: connect previous step, enter gas-gas heat exchanger 23 from secondary coolers gas-liquid separator 14 gas out, carry out precooling, enter again 21 gas-liquid separations of gas-gas heat exchanger gas-liquid separator, it is freezing that isolated gas enters cryocooler 20, and described freezing temperature reaches-40～-55 DEG C;
(7) gas-liquid separation step: connect previous step, freezing previous step rear gas is entered to cryocooler gas-liquid separator 15 to be reached gas-liquid and separates completely, isolated hydrogen enters gas-gas heat exchanger 23 tube sides and heats up, and from separating, Hydrogen Line 22 enters systemic circulation use.
The operation method of described polysilicon cold hydrogenation, from one-level water cooler gas-liquid separator 12, secondary coolers gas-liquid separator 14, gas-gas heat exchanger gas-liquid separator 21, deep-cooling heat exchanger gas-liquid separator 15 separates, liquid is all delivered to purification tower 19 and is carried out component separation, and the required steam of described purification tower 19 is provided by steam-pipe 18.
Implement the operation method of polysilicon cold hydrogenation of the present invention, in the time of operation, needed cold hydrogenation process silica flour is entered to cold hydrogenation reactor 9 by silica flour transport pipe 1, hydrogen and silicon tetrachloride are delivered to hydrogen interchanger 3 and silicon tetrachloride interchanger 2 by Hydrogen Line 5 and silicon tetrachloride pipeline 4 respectively by the molar ratio of 1.8:1～3.0:1, carry out heat exchange by the hot water transporting with vapor condensation waterpipe 17, temperature is by normal temperature heat exchange to 80～100 DEG C, hot water after heat exchange is discharged from waste pipe 6, hydrogen and silicon tetrachloride mixture enter and mix vaporizing chamber 7, heating vaporization, hydrogen after vaporization and silicon tetrachloride mixed gas are through first-class heat exchanger 27 and secondary heat exchanger 26, with cold hydrogenation reactor 9 gas converting heat out, temperature is raised to 400～490 DEG C, be heated to 500～600 DEG C by electric heater 8 again, entering cold hydrogenation reactor 9 reacts with silica flour, reacted product gas first passes through cyclonic separator 25, by silica flour in gas and catalyst solid particle separation, silica flour and granules of catalyst are got back to cold hydrogenation reactor 9, gas is again by the further dust removal by filtration of strainer 24, again carrying out gas-solid is separated, then gas by secondary heat exchanger 26 and first-class heat exchanger 27 with from mixing vaporizing chamber 7 gas converting heat out, temperature is down to 200～280 DEG C, enter eluting column 10 drip washing from first-class heat exchanger 27 gas out, in cooling, further remove impurity, impurity under drip washing is discharged from eluting column 10 bottom raffinate pipelines 16, individual curing, no longer enter in purification tower 19 and go, alleviate purification tower 19 line clogging problems, from eluting column 10 tops gas out, first be cooled to 70～90 DEG C by one-level water cooler 11, enter 12 gas-liquid separations of one-level water cooler gas-liquid separator, liquid under condensation directly enters purification tower 19, no longer further cooling, save purification tower 19 steam usage quantitys, gas enters secondary coolers 13, be cooled to 40～70 DEG C, enter 14 gas-liquid separations of secondary coolers gas-liquid separator, separate lower liquid and enter eluting column 10, gas in spray eluting column 10, enter gas-gas heat exchanger 23 from the isolated gas of secondary coolers gas-liquid separator 14, carry out precooling cooling, enter again 21 gas-liquid separations of gas-gas heat exchanger gas-liquid separator, isolated gas enters cryocooler 20 and is refrigerated to-40～-55 DEG C, realizing gas-liquid through cryocooler gas-liquid separator 15 separates completely, isolated hydrogen enters gas-gas heat exchanger 23 tube sides and heats up, from separating, Hydrogen Line 22 is delivered to elsewhere and recycles, from one-level water cooler gas-liquid separator 12, secondary coolers gas-liquid separator 14, gas-gas heat exchanger gas-liquid separator 21, the lower liquid of deep-cooling heat exchanger gas-liquid separator 15 separation is delivered to purification tower 19 and is carried out component separation, the required steam of purification tower 19 is provided by steam-pipe 18, the present invention, due to the abundant exchange of cold and hot energy, is fully used material self-energy, has reduced by a relatively large margin outer energizing quantity consumption, and by advance to system material filtering and drip washing, has alleviated purification tower line clogging problem.
Above-described embodiment is only for the invention example is clearly described; and the not restriction to the invention embodiment; for those of ordinary skill in the field; can also make other changes in different forms on the basis of the above description, and the apparent variation of being amplified out thus or variation are still among the protection domain in the invention claim.
Part not in the detailed description of the invention is prior art.
Claims (10)
1. the operation method of a polysilicon cold hydrogenation, it is characterized in that: comprise silica flour reactions steps, heat exchange, pervaporation step, electrically heated step, gas solid separation step, drip washing, removal of impurity step, the freezing step of refrigerant and gas-liquid separating step, concrete operation step is as follows:
(1) silica flour reactions steps: silica flour is sent into cold hydrogenation reactor (9) by silica flour transport pipe (1), produce reactant gases;
(2) heat exchange, pervaporation step: by hydrogen and silicon tetrachloride in proportion respectively after hydrogen interchanger (3) and silicon tetrachloride interchanger (2), the hot water transporting with vapor condensation waterpipe (13) carries out heat exchange, hot water after heat exchange is discharged from waste pipe (6), and hydrogen and silicon tetrachloride mixture enter mixing vaporizing chamber (7) and vaporize;
(3) electrically heated step: connect previous step, by previous step obtain hydrogen after vaporization and the mixed gas of silicon tetrachloride through first-class heat exchanger (27) and secondary heat exchanger (26) after with the reactant gases heat exchange of the interior generation of cold hydrogenation reactor (9), after then being heated by electric heater (8), enter cold hydrogenation reactor (9) and react with silica flour;
(4) gas solid separation step: connect previous step, the reacted product that previous step is obtained passes through cyclonic separator (25) by the silica flour in reactor product, catalyst solid and gas delivery, silica flour and catalyst solid are got back to cold hydrogenation reactor (9), gas is undertaken after dust removal by filtration by strainer (24), by secondary heat exchanger (26) and first-class heat exchanger (27) with from mixing in vaporizing chamber (7) gas converting heat out;
(5) drip washing, removal of impurity step: connect previous step, will in previous step, enter eluting column (10) drip washing from first-class heat exchanger (27) gas out, the impurity under drip washing is discharged from the raffinate pipeline (16) of eluting column (10) bottom; Being lowered the temperature by one-level cold gas liquid/gas separator (11) from eluting column (10) top gas out, enter one-level water cooler gas-liquid separator (12) gas-liquid separation, liquid under condensation directly enters purification tower (19), noncondensable gas enter secondary coolers (13) cooling after, enter secondary coolers gas-liquid separator (14) gas-liquid separation, liquid under condensation enters eluting column (10) again, and spray enters the gas of eluting column (10) out from first-class heat exchanger (27);
(6) the freezing step of refrigerant: connect previous step, enter gas-gas heat exchanger (23) from secondary coolers gas-liquid separator (14) gas out, carry out precooling, then enter gas-gas heat exchanger gas-liquid separator (21) gas-liquid separation, it is freezing that isolated gas enters cryocooler (20);
(7) gas-liquid separation step: connect previous step, freezing previous step rear gas is entered to cryocooler gas-liquid separator (15) to be reached gas-liquid and separates completely, isolated hydrogen enters gas-gas heat exchanger (23) tube side and heats up, and Hydrogen Line from separating (22) enters systemic circulation and uses.
2. the operation method of polysilicon cold hydrogenation according to claim 1, is characterized in that: in heat exchange, pervaporation step, hydrogen and silicon tetrachloride pass through respectively hydrogen interchanger (3) and silicon tetrachloride interchanger (2) by the molar ratio of 1.8:1～3.0:1.
3. the operation method of polysilicon cold hydrogenation according to claim 1, is characterized in that: in heat exchange, pervaporation step, the temperature that the hot water transporting with vapor condensation waterpipe (13) carries out heat exchange reaches 80～100 DEG C.
4. the operation method of polysilicon cold hydrogenation according to claim 1, is characterized in that: in electrically heated step, heat-exchange temperature reaches 400～490 DEG C.
5. the operation method of polysilicon cold hydrogenation according to claim 1, is characterized in that: in electrically heated step, reach 500～600 DEG C by the temperature of electric heater (8) heating.
6. the operation method of polysilicon cold hydrogenation according to claim 1, is characterized in that: in gas solid separation step, the temperature of heat exchange reaches 200～280 DEG C.
7. the operation method of polysilicon cold hydrogenation according to claim 1, it is characterized in that: in drip washing, removal of impurity step, from eluting column (10) top gas out, by one-level cold gas liquid/gas separator (11) cooling, the temperature of described cooling reaches 200～280 DEG C.
8. the operation method of polysilicon cold hydrogenation according to claim 1, is characterized in that: in drip washing, removal of impurity step, it is cooling that noncondensable gas enters secondary coolers (13), and described cooling temperature reaches 40～70 DEG C.
9. the operation method of polysilicon cold hydrogenation according to claim 1, is characterized in that: in the freezing step of refrigerant, freezing temperature reaches-40～-55 DEG C.
10. the operation method of polysilicon cold hydrogenation according to claim 1, it is characterized in that: described one-level water cooler gas-liquid separator (12), secondary coolers gas-liquid separator (14), gas-gas heat exchanger gas-liquid separator (21), the lower liquid of deep-cooling heat exchanger gas-liquid separator (15) separation are all delivered to purification tower (19) and carried out component separation, and the required steam of described purification tower (19) is provided by steam-pipe (18).
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106315586A (en) * | 2015-06-15 | 2017-01-11 | 内蒙古盾安光伏科技有限公司 | Polycrystalline silicon production system |
| CN106554018A (en) * | 2015-09-28 | 2017-04-05 | 新特能源股份有限公司 | A kind of cold hydrogenation dust pelletizing system and technique |
| CN107337211A (en) * | 2016-05-03 | 2017-11-10 | 新特能源股份有限公司 | The gasification method and vapourizing unit of silicon tetrachloride in a kind of polysilicon cold hydrogenization method |
| CN110422847A (en) * | 2019-08-30 | 2019-11-08 | 中石化南京工程有限公司 | A kind of silicon tetrachloride vaporization and heat recovery system and method |
| WO2022041699A1 (en) * | 2020-08-24 | 2022-03-03 | 中国恩菲工程技术有限公司 | Silicon tetrachloride cold hydrogenation system |
| CN115414771A (en) * | 2022-08-11 | 2022-12-02 | 中国恩菲工程技术有限公司 | Tail gas treatment system and method for silicon-based electronic product production process |
| CN115744915A (en) * | 2022-12-01 | 2023-03-07 | 华陆工程科技有限责任公司 | Chlorosilane liquid treatment method and treatment device |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106315586A (en) * | 2015-06-15 | 2017-01-11 | 内蒙古盾安光伏科技有限公司 | Polycrystalline silicon production system |
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| CN106554018A (en) * | 2015-09-28 | 2017-04-05 | 新特能源股份有限公司 | A kind of cold hydrogenation dust pelletizing system and technique |
| CN106554018B (en) * | 2015-09-28 | 2018-12-25 | 新特能源股份有限公司 | The cold hydrogenation dust pelletizing system of one kind and technique |
| CN107337211A (en) * | 2016-05-03 | 2017-11-10 | 新特能源股份有限公司 | The gasification method and vapourizing unit of silicon tetrachloride in a kind of polysilicon cold hydrogenization method |
| CN107337211B (en) * | 2016-05-03 | 2020-06-16 | 新特能源股份有限公司 | Method and device for vaporizing silicon tetrachloride in cold hydrogenation of polycrystalline silicon |
| CN110422847A (en) * | 2019-08-30 | 2019-11-08 | 中石化南京工程有限公司 | A kind of silicon tetrachloride vaporization and heat recovery system and method |
| WO2022041699A1 (en) * | 2020-08-24 | 2022-03-03 | 中国恩菲工程技术有限公司 | Silicon tetrachloride cold hydrogenation system |
| CN115414771A (en) * | 2022-08-11 | 2022-12-02 | 中国恩菲工程技术有限公司 | Tail gas treatment system and method for silicon-based electronic product production process |
| CN115744915A (en) * | 2022-12-01 | 2023-03-07 | 华陆工程科技有限责任公司 | Chlorosilane liquid treatment method and treatment device |
| CN115744915B (en) * | 2022-12-01 | 2024-01-23 | 华陆工程科技有限责任公司 | Treatment method and treatment device for chlorosilane liquid |
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Address after: 471322 Baisha Town Industrial Agglomeration Area, Yichuan County, Luoyang City, Henan Province Patentee after: Luoyang Lier Functional Materials Co., Ltd. Address before: 471322 Baisha Town Industrial Agglomeration Area, Yichuan County, Luoyang City, Henan Province Patentee before: LUOYANG LIER ZHONGJING PHOTOVOLTAIC MATERIAL CO., LTD. |