CN102267697A - Process for producing solar grade polysilicon with sodium circulation method - Google Patents
Process for producing solar grade polysilicon with sodium circulation method Download PDFInfo
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- CN102267697A CN102267697A CN2010101980973A CN201010198097A CN102267697A CN 102267697 A CN102267697 A CN 102267697A CN 2010101980973 A CN2010101980973 A CN 2010101980973A CN 201010198097 A CN201010198097 A CN 201010198097A CN 102267697 A CN102267697 A CN 102267697A
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Abstract
The invention relates to a process for producing solar grade polysilicon with a sodium circulation method. The process comprises the following steps: heating sodium fluosilicate Na2SiF6 to decompose to a silicon tetrafluoride (SiF4) gas and sodium fluoride NaF; vaporizing metallic sodium Na to a sodium (Na) steam at a high temperature; allowing the silicon tetrafluoride (SiF4) gas and the sodium (Na) steam to enter a reaction furnace to generate high purity silicon powder, allowing the high purity silicon powder to enter a first collector, and carrying out high temperature fusion to prepare finished products of polysilicon; allowing other mixed gases to enter a second collector, allowing sodium fluoride NaF to deposit with unreacted sodium Na, and carrying out heating separation on sodium fluoride NaF and sodium Na; allowing the other gases to enter a third collector, cooling, collecting the residual silicon tetrafluoride (SiF4) gas, adding water to dissolve into a solution of fluosilicic acid (H2SiF6); and carrying out spray processing on residual substances. The process for producing solar grade polysilicon with the sodium circulation method, which has the advantages of simple production technology, no discharge of toxic gases, wide source and cheapness of raw materials, and accordance of the concept of Chinese circular economy, allows generated byproducts to be effectively utilized, the production cost to be substantially saved, and the development of the solar photovoltaic industry to be effectively promoted.
Description
Technical field
The present invention relates to a kind of processing method of producing polysilicon, especially a kind of sodium circulation method is produced the processing method of solar-grade polysilicon.
Background technology
Because sun power has the fast development and the newly increased requirement of impayable environmental protection, low-carbon (LC), advantage such as inexhaustible and photovoltaic industry, the current upsurge that has formed developing low-cost, low consumption sun power and polysilicon in the world, emerge the new technology of many special production solar-grade polysilicons, the normal at present polysilicon reduction method that adopts has Siemens Method, silane thermal decomposition process, sulfuration bed method etc., but, existing polysilicon reduction method cost height, energy consumption is big, seriously polluted, increased production cost and environmental pollution.
Summary of the invention
In order to solve the problem that existing polysilicon reduction method exists, the present invention proposes a kind of sodium circulation method and produce the processing method of solar-grade polysilicon, this kind processing method adopts the chemical physics conversion method, production technique is simple, no toxic gas discharging, and the byproduct that produces effectively can be utilized, saved production cost and energy consumption greatly, effectively promoted the development of photovoltaic industry.
The technical solution adopted for the present invention to solve the technical problems is: the processing method that this a kind of sodium circulation method is produced solar-grade polysilicon is: Na2SiF6 puts into reactor with Sodium Silicofluoride, with 300 ℃-800 ℃ temperature thermal degradation 1-5 hour, generate silicon tetrafluoride SiF4 gas and byproduct Sodium Fluoride NaF, can sell after Sodium Fluoride NaF cooling becomes solid; High purity metal sodium Na in reactor, is increased temperature 800 ℃-1000 ℃ and is vaporized into sodium Na steam; Make silicon tetrafluoride SiF4 gas and high purity sodium Na steam enter Reaktionsofen than along pipeline simultaneously, generate the high purity silica flour by 1: 4 reaction formula weight; The high purity silica flour enters first collector, and controlled temperature becomes piece with Powdered high purity silicon Si high-temperature fusion between 1000 ℃-1600 ℃, make the polysilicon finished product; Other mixed gas enters second collector, at 800 ℃-100 ℃, makes Sodium Fluoride NaF and unreacted sodium Na deposition by controlled temperature, and with Sodium Fluoride NaF and sodium Na heating and separating, sodium Na recycles again, and Sodium Fluoride NaF sells as byproduct; Other mixed gas enters the 3rd collector, cools to 10 ℃ of-0 ℃ of coolings, collects remaining silicon tetrafluoride SiF4 gas, is dissolved in water into silicofluoric acid H2SiF6 solution and sells; Remaining material spray is handled.
The invention has the beneficial effects as follows: the processing method production technique that this a kind of sodium circulation method is produced solar-grade polysilicon is simple, no toxic gas discharging, raw material sources are extensively cheap, the notion that meets national recycling economy, and the byproduct that produces effectively can be utilized, save production cost greatly, effectively promoted the development of photovoltaic industry.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples.
Accompanying drawing 1 is that this a kind of sodium circulation method is produced the process flow sheet of the processing method of solar-grade polysilicon.
Tool is stopped embodiment
In accompanying drawing 1, the processing method that this a kind of sodium circulation method is produced solar-grade polysilicon is: Na2SiF6 puts into reactor with Sodium Silicofluoride, with 300 ℃-800 ℃ temperature thermal degradation 1-5 hour, generate silicon tetrafluoride SiF4 gas and byproduct Sodium Fluoride NaF, can sell after Sodium Fluoride NaF cooling becomes solid; High purity metal sodium Na in reactor, is increased temperature 800 ℃-1000 ℃ and is vaporized into sodium Na steam; Make silicon tetrafluoride SiF4 gas and high purity sodium Na steam enter Reaktionsofen than along pipeline simultaneously, generate the high purity silica flour by 1: 4 reaction formula weight; The high purity silica flour enters first collector, and controlled temperature becomes piece with Powdered high purity silicon Si high-temperature fusion between 1000 ℃-1600 ℃, make the polysilicon finished product; Other mixed gas enters second collector, at 800 ℃-100 ℃, makes Sodium Fluoride NaF and unreacted sodium Na deposition by controlled temperature, and with Sodium Fluoride NaF and sodium Na heating and separating, sodium Na recycles again, and Sodium Fluoride NaF sells as byproduct; Other mixed gas enters the 3rd collector, cools to 10 ℃ of-0 ℃ of coolings, collects remaining silicon tetrafluoride SiF4 gas, is dissolved in water into silicofluoric acid H2SiF6 solution and sells; Remaining material spray is handled.
Impurity concentration＜the 0.02ppm (7N) of the silica flour that generates.
Raw material Sodium Silicofluoride Na2SiF6 is the byproduct in the phosphate fertilizer making processes, and the source is cheap and extensive; The byproduct Sodium Fluoride NaF that produces in the anti-process is the fine industrial chemicals, is used for Aluminium industry and toothpaste production, and silicofluoric acid H2SiF6 solution can be used for Metal plating, wood preservation, has disinfectant properties, can make the sterilizing agent in the brewage.
Claims (2)
1. a sodium circulation method is produced the processing method of solar-grade polysilicon, it is characterized in that: Na2SiF6 puts into reactor with Sodium Silicofluoride, with 300 ℃-800 ℃ temperature thermal degradation 1-5 hour, generate silicon tetrafluoride SiF4 gas and byproduct Sodium Fluoride NaF, can sell after Sodium Fluoride NaF cooling becomes solid; High purity metal sodium Na in reactor, is increased temperature 800 ℃-1000 ℃ and is vaporized into sodium Na steam; Make silicon tetrafluoride SiF4 gas and high purity sodium Na steam enter Reaktionsofen than along pipeline simultaneously, generate the high purity silica flour by 1: 4 reaction formula weight; The high purity silica flour enters first collector, and controlled temperature becomes piece with Powdered high purity silicon Si high-temperature fusion between 1000 ℃-1600 ℃, make the polysilicon finished product; Other mixed gas enters second collector, at 800 ℃-100 ℃, makes Sodium Fluoride NaF and unreacted sodium Na deposition by controlled temperature, and with Sodium Fluoride NaF and sodium Na heating and separating, Sodium Fluoride NaF sells as byproduct again; Other mixed gas enters the 3rd collector, cools to 10 ℃ of-0 ℃ of coolings, collects remaining silicon tetrafluoride SiF4 gas, is dissolved in water into silicofluoric acid H2SiF6 solution and sells; Remaining material spray is handled.
2. according to the processing method of the described a kind of sodium circulation method production solar-grade polysilicon of claim 1, it is characterized in that: sodium Na recycles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2010101980973A CN102267697B (en) | 2010-06-04 | 2010-06-04 | Process for producing solar grade polysilicon with sodium circulation method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101980973A CN102267697B (en) | 2010-06-04 | 2010-06-04 | Process for producing solar grade polysilicon with sodium circulation method |
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| CN102267697A true CN102267697A (en) | 2011-12-07 |
| CN102267697B CN102267697B (en) | 2013-01-02 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288088A (en) * | 2012-02-23 | 2013-09-11 | 苏州宝时得电动工具有限公司 | Preparation method of polycrystalline silicon |
| CN103395785A (en) * | 2013-07-18 | 2013-11-20 | 贵州省产品质量监督检验院 | Method for preparing polycrystalline silicon by reducing sodium fluosilicate with sodium |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4446120A (en) * | 1982-01-29 | 1984-05-01 | The United States Of America As Represented By The United States Department Of Energy | Method of preparing silicon from sodium fluosilicate |
| CN101134562A (en) * | 2006-09-01 | 2008-03-05 | 多氟多化工股份有限公司 | Method for producing hydrofluoric acid |
| US20090263307A1 (en) * | 2008-04-17 | 2009-10-22 | Circulon Hungary Ltd. | Silicon Production Process |
-
2010
- 2010-06-04 CN CN2010101980973A patent/CN102267697B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4446120A (en) * | 1982-01-29 | 1984-05-01 | The United States Of America As Represented By The United States Department Of Energy | Method of preparing silicon from sodium fluosilicate |
| CN101134562A (en) * | 2006-09-01 | 2008-03-05 | 多氟多化工股份有限公司 | Method for producing hydrofluoric acid |
| US20090263307A1 (en) * | 2008-04-17 | 2009-10-22 | Circulon Hungary Ltd. | Silicon Production Process |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288088A (en) * | 2012-02-23 | 2013-09-11 | 苏州宝时得电动工具有限公司 | Preparation method of polycrystalline silicon |
| CN103288088B (en) * | 2012-02-23 | 2016-02-17 | 苏州宝时得电动工具有限公司 | A kind of preparation method of polysilicon |
| CN103395785A (en) * | 2013-07-18 | 2013-11-20 | 贵州省产品质量监督检验院 | Method for preparing polycrystalline silicon by reducing sodium fluosilicate with sodium |
| CN103395785B (en) * | 2013-07-18 | 2014-12-31 | 贵州省产品质量监督检验院 | Method for preparing polycrystalline silicon by reducing sodium fluosilicate with sodium |
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