CN102174674A - Processing and recycling process for silicon slurry - Google Patents
Processing and recycling process for silicon slurry Download PDFInfo
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- CN102174674A CN102174674A CN2011100587360A CN201110058736A CN102174674A CN 102174674 A CN102174674 A CN 102174674A CN 2011100587360 A CN2011100587360 A CN 2011100587360A CN 201110058736 A CN201110058736 A CN 201110058736A CN 102174674 A CN102174674 A CN 102174674A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a processing and recycling process for silicon slurry, which comprises the steps as follows: silicon slurry is evaporated for gas and solid separation; high boiling point substances are obtained after the gas phase is condensed; the high boiling point substances react with hydrogen chloride to be cracked into mixed monomers such as methyl trichloro silicane, trimethyl chloro silicane, methyl silane, dimethyl dichloro silicane and the like; and after the fractionation, each pure monomer product can be obtained. The solid phase separated through evaporation mainly contains cuprous oxide, silicon, silicon dioxide and the like; hydrochloric acid (or sulfuric acid) is added into the solid phase to extract copper chloride (or copper sulfate, which can be sold directly) by a chemical method; and silicon and silicon dioxide are separated out. Iron powder is added into a copper chloride solution for extracting copper and ferrous chloride, and sodium hydroxide is added into the ferrous chloride solution for extracting ferrous oxide. The processing and recycling process is environment-friendly and can eliminate pollution, and meanwhile can recover various by-products from silicon slurry, thereby having well economic benefits.
Description
Technical field
The present invention relates to chemical technique, technology is reclaimed in particularly a kind of processing of white residue slurry.
Background technology
The organosilicon device with by-product high boiling material, azeotrope and white residue slurry, wherein contains useful matter and other objectionable constituent such as Si, Cu and organosilane monomer in the synthetic production process of monomer.Organosilicon device by 70,000 tons of/year scales calculates, and annual quantum of output is about respectively :～4000 tons of rectifying high boiling material, about 1200 tons of azeotropes, 3000 tons of white residues are starched.These byproducts can not directly discharge owing to contain harmful ingredients; But the channel of direct marketing is limited, has restricted the normal operation of organosilane monomer device.
Summary of the invention
Purpose of the present invention exactly in order to solve the problems referred to above that prior art exists, provides a kind of processing of white residue slurry to reclaim technology.
To achieve these goals, the present invention has adopted following technical scheme: technology is reclaimed in a kind of processing of white residue slurry, may further comprise the steps:
A, white residue slurry is delivered in the airtight equipment evaporates, carry out gas solid separation, obtain gaseous phase materials and solid-phase material;
B, will obtain high boiling material after the condensation of step a gained gaseous phase materials;
C, high boiling material is carried out catalytic pyrolysis, high boiling material and hydrogenchloride generation scission reaction under the effect of catalyzer will obtain monomethyl trichlorosilane, tri-methyl-chlorosilane, monomethyl hydrogen silane and dimethyldichlorosilane(DMCS) product after the split product fractionation;
D, step a gained solid-phase material is added hydrochloric acid reaction, separate obtaining the mixture that solid phase is silicon and silicon-dioxide, liquid phase is a Cupric Chloride Solution;
E, adding iron powder reaction in Cupric Chloride Solution, it is copper that separation obtains solid phase, liquid phase is a solution of ferrous chloride;
F, adding sodium hydroxide reaction in solution of ferrous chloride, it is ferrous hydroxide that separation obtains solid phase;
G, ferrous hydroxide is cured the back obtain iron protoxide powder product;
H, step e gained solid phase copper is cured the back obtain the copper powder product;
J, the mixture of steps d gained silicon and silicon-dioxide is cured the back obtain the silica flour product.
Steps d changes the adding sulfuric acid reaction into, separates to obtain the mixture that solid phase is silicon and silicon-dioxide, and liquid phase is a copper-bath; The copper sulfate product will be obtained after the copper-bath evaporation drying; The mixture of silicon and silicon-dioxide is cured back acquisition silica flour product.
Catalyzer described in the step c is an iron powder.
After the white residue slurry that the processing recovery technology of white residue slurry of the present invention produces the organosilane monomer device carries out harmless treatment, both can guarantee the normal driving of organosilane monomer device, and can reclaim monomethyl trichlorosilane, tri-methyl-chlorosilane, monomethyl hydrogen silane, dimethyldichlorosilane(DMCS), copper powder, silica flour and iron protoxide again.The dimethyl chloride disilane is sold with intermediate, or and then synthetic expensive hexamethyldisilane.Copper powder, silica flour and iron protoxide can sell.In protection environment, decontamination, can bring good economic benefits again.Thoroughly solved the bottleneck problem of domestic and international organosilicon long-term sustainable development.
Description of drawings
Fig. 1, Fig. 2 reclaim the process flow sheet of technology for the processing of white residue slurry of the present invention.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
Referring to Fig. 1, Fig. 2, the concrete steps that technology is reclaimed in the processing of white residue of the present invention slurry are, the white residue slurry is delivered to an airtight equipment (available rotary kiln realization) evaporation carries out gas solid separation, and the gas that evaporation is produced obtains high boiling material after condensation.High boiling material adopts the cracking and catalyzing technology, the cracking that reacts of high boiling material and hydrogenchloride goes out mix monomers such as monomethyl trichlorosilane, tri-methyl-chlorosilane, monomethyl hydrogen silane, dimethyldichlorosilane(DMCS) under the effect of iron powder catalyzer, obtains each pure monomer product through fractionation.And the solid separated of evaporation mainly contains Red copper oxide, silicon and silicon-dioxide etc., adds hydrochloric acid (or sulfuric acid) with chemical method in solid phase and extracts cupric chloride (or copper sulfate, copper sulfate can sell), isolates silicon and silicon-dioxide.In Cupric Chloride Solution, add iron powder and extract copper and iron protochloride, in solution of ferrous chloride, add sodium hydroxide extraction and go out iron protoxide.Iron protoxide obtains iron protoxide powder product after curing.Silicon and silicon-dioxide obtain the silica flour product after curing.
Claims (3)
1. technology is reclaimed in the processing of a white residue slurry, it is characterized in that, may further comprise the steps:
A, white residue slurry is delivered in the airtight equipment evaporates, carry out gas solid separation, obtain gaseous phase materials and solid-phase material;
B, will obtain high boiling material after the condensation of step a gained gaseous phase materials;
C, high boiling material is carried out catalytic pyrolysis, high boiling material and hydrogenchloride generation scission reaction under the effect of catalyzer will obtain monomethyl trichlorosilane, tri-methyl-chlorosilane, monomethyl hydrogen silane and dimethyldichlorosilane(DMCS) product after the split product fractionation;
D, step a gained solid-phase material is added hydrochloric acid reaction, separate obtaining the mixture that solid phase is silicon and silicon-dioxide, liquid phase is a Cupric Chloride Solution;
E, adding iron powder reaction in Cupric Chloride Solution, it is copper that separation obtains solid phase, liquid phase is a solution of ferrous chloride;
F, adding sodium hydroxide reaction in solution of ferrous chloride, it is ferrous hydroxide that separation obtains solid phase;
G, ferrous hydroxide is cured the back obtain iron protoxide powder product;
H, step e gained solid phase copper is cured the back obtain the copper powder product;
J, the mixture of steps d gained silicon and silicon-dioxide is cured the back obtain the silica flour product.
2. technology is reclaimed in the processing of white residue slurry as claimed in claim 1, and it is characterized in that: steps d changes the adding sulfuric acid reaction into, separates obtaining the mixture that solid phase is silicon and silicon-dioxide, and liquid phase is a copper-bath; The copper sulfate product will be obtained after the copper-bath evaporation drying; The mixture of silicon and silicon-dioxide is cured back acquisition silica flour product.
3. technology is reclaimed in the processing of white residue slurry as claimed in claim 2, and it is characterized in that: the catalyzer described in the step c is an iron powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2011100587360A CN102174674A (en) | 2011-03-11 | 2011-03-11 | Processing and recycling process for silicon slurry |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100587360A CN102174674A (en) | 2011-03-11 | 2011-03-11 | Processing and recycling process for silicon slurry |
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| CN102174674A true CN102174674A (en) | 2011-09-07 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420381A (en) * | 2012-05-15 | 2013-12-04 | 天华化工机械及自动化研究设计院有限公司 | Method for recycling disposal of silicon tetrachloride slag slurry produced in polycrystalline silicon production and device thereof |
| CN103555951A (en) * | 2013-10-23 | 2014-02-05 | 泸州北方化学工业有限公司 | Method for extracting copper from organic silicon scrap |
| CN104262379A (en) * | 2014-08-29 | 2015-01-07 | 浙江恒业成有机硅有限公司 | Organic silicon residue slurry treatment device and treatment method |
| CN105439504A (en) * | 2015-11-16 | 2016-03-30 | 卢连伟 | Method for recycling organic silicon slurry |
| CN105921257A (en) * | 2016-04-20 | 2016-09-07 | 昌邑市龙港无机硅有限公司 | Treating method for silicon slag produced during production of liquid sodium silicate |
| CN106220666A (en) * | 2016-07-18 | 2016-12-14 | 聊城市鲁西化工工程设计有限责任公司 | The processing system of a kind of organic silicon slurry slag and processing method |
| CN108558928A (en) * | 2018-05-09 | 2018-09-21 | 成都斯力康科技股份有限公司 | A kind of method and apparatus of organosilicon slag slurry synthetical recovery processing |
| CN110330521A (en) * | 2019-06-05 | 2019-10-15 | 江苏明珠硅橡胶材料有限公司 | A kind of organosilicon slag slurry processing method |
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| CN101386626A (en) * | 2008-10-31 | 2009-03-18 | 江苏宏达新材料股份有限公司 | Organosilicon slag slurry treatment method and apparatus thereof |
| CN101659672A (en) * | 2008-08-29 | 2010-03-03 | 中国石油天然气股份有限公司 | Method for cracking treatment of organic silicon waste residue slurry |
| CN101824047A (en) * | 2010-05-31 | 2010-09-08 | 山东中创钢构有限公司 | Method for preparing methyl chlorosilane by cracking organic silicon high boiling point substance |
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| CN101659672A (en) * | 2008-08-29 | 2010-03-03 | 中国石油天然气股份有限公司 | Method for cracking treatment of organic silicon waste residue slurry |
| CN101386626A (en) * | 2008-10-31 | 2009-03-18 | 江苏宏达新材料股份有限公司 | Organosilicon slag slurry treatment method and apparatus thereof |
| CN101824047A (en) * | 2010-05-31 | 2010-09-08 | 山东中创钢构有限公司 | Method for preparing methyl chlorosilane by cracking organic silicon high boiling point substance |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420381A (en) * | 2012-05-15 | 2013-12-04 | 天华化工机械及自动化研究设计院有限公司 | Method for recycling disposal of silicon tetrachloride slag slurry produced in polycrystalline silicon production and device thereof |
| CN103555951A (en) * | 2013-10-23 | 2014-02-05 | 泸州北方化学工业有限公司 | Method for extracting copper from organic silicon scrap |
| CN103555951B (en) * | 2013-10-23 | 2015-11-04 | 泸州北方化学工业有限公司 | The method of copper is put forward from organic silicon scrap |
| CN104262379A (en) * | 2014-08-29 | 2015-01-07 | 浙江恒业成有机硅有限公司 | Organic silicon residue slurry treatment device and treatment method |
| CN105439504A (en) * | 2015-11-16 | 2016-03-30 | 卢连伟 | Method for recycling organic silicon slurry |
| CN105921257A (en) * | 2016-04-20 | 2016-09-07 | 昌邑市龙港无机硅有限公司 | Treating method for silicon slag produced during production of liquid sodium silicate |
| CN105921257B (en) * | 2016-04-20 | 2018-07-17 | 昌邑市龙港无机硅有限公司 | A kind of processing method for producing liquid sodium silicate and generating white residue |
| CN106220666A (en) * | 2016-07-18 | 2016-12-14 | 聊城市鲁西化工工程设计有限责任公司 | The processing system of a kind of organic silicon slurry slag and processing method |
| CN108558928A (en) * | 2018-05-09 | 2018-09-21 | 成都斯力康科技股份有限公司 | A kind of method and apparatus of organosilicon slag slurry synthetical recovery processing |
| CN108558928B (en) * | 2018-05-09 | 2020-08-18 | 成都斯力康科技股份有限公司 | Method and equipment for comprehensively recycling organic silicon slag slurry |
| CN110330521A (en) * | 2019-06-05 | 2019-10-15 | 江苏明珠硅橡胶材料有限公司 | A kind of organosilicon slag slurry processing method |
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