CN106430221B - A kind of resource utilization method of silicon tetrachloride as by-product of polysilicon - Google Patents
A kind of resource utilization method of silicon tetrachloride as by-product of polysilicon Download PDFInfo
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- CN106430221B CN106430221B CN201610794942.0A CN201610794942A CN106430221B CN 106430221 B CN106430221 B CN 106430221B CN 201610794942 A CN201610794942 A CN 201610794942A CN 106430221 B CN106430221 B CN 106430221B
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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
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
- C01B33/183—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The present invention relates to a kind of resource utilization methods of silicon tetrachloride as by-product of polysilicon, comprising steps of the silicon tetrachloride liquid in silicon tetrachloride storage tank to be added to the entrance of venturi tube inlet cylindrical section by mechanical pump, the mixed solution of deionized water and dispersing agent is introduced from Venturi tube cylindrical throat, silicon tetrachloride and deionized water is set to react in Venturi tube, the mixture of Venturi tube circular cone diffuser opening discharge flows back into silicon tetrachloride storage tank, carries out circular response；Until the mixed solution of deionized water and dispersing agent all adds, it is aged；It is filtered, washed, dries and collects.The beneficial effects of the present invention are: reaction condition is mild, safely controllable, properties of product can be controlled by the control parameters such as four silica flow velocitys and deionized water velocity ratio, dispersant dosage and spray drying temperature, obtain the silica product of different aggregation partial sizes and specific surface area；The rapid development of polysilicon industry health is promoted, is reduced environmental pollution, energy-saving and emission-reduction.
Description
Technical field
The present invention relates to a kind of resource utilization methods of silicon tetrachloride as by-product of polysilicon.
Background technique
In recent years, with the development of polysilicon industry, the processing problem of silicon tetrachloride as by-product becomes increasingly conspicuous.According to system
Meter, every 1 ton about 10~15 tons of polysilicon by-produced tetrachlorosilane of production.Silicon tetrachloride is a kind of with the poisonous and harmful of strong corrosive
Liquid, to safety and environmental protection it is very harmful, how effective solution polysilicon industry silicon tetrachloride as by-product processing asks
Topic has great significance for the development and the Implement of sustainable development strategy that promote photovoltaic industry.
Currently, mainly having two approach to the processing of silicon tetrachloride as by-product of polysilicon: first is that by polysilicon by-product four
The products such as silester, organosilicon are made in silicon chloride, but these methods are too small to the digestion amount of silicon tetrachloride, and are often consuming
New environmental pollution is generated while waste again；Another way is hydrogenated silicon tetrachloride as by-product of polysilicon as trichlorine hydrogen
Silicon is recycled back to synthesis procedure, and this processing mode has investment big, energy consumption height, the low, complex procedures of conversion ratio etc.
Disadvantage.Processing silicon tetrachloride is mainly also there are two types of method in the world: method first is that being gone back at high temperature under high pressure using hydrogen
Originally be the primary raw material trichlorosilane of polysilicon, method second is that using silicon tetrachloride production high added value gas-phase silica.
Such as German watt gram, day the Bender mountain of external main polysilicon company not only produces polysilicon but also raw using later approach
White carbon black is produced, gas-phase silica and production of polysilicon are combined closely, the circulating economy chain that a resource utilizes mutually is formed, it is real
Existing resource circulation utilization.
The country is in the starting stage by the technique that raw material produces gas-phase silica of silicon tetrachloride, and certain critical process are grasped
In external a small number of major companies hand.And the method equipment investment is big, production higher cost constrains its product promotion.Therefore,
Find a kind of simple production process, equipment investment is small, product cost is low new method solves the resource utilization of silicon tetrachloride
Problem is imperative.
In recent years precipitated silica due to simple production process, equipment investment is small, product cost is low and to environment without dirt
The features such as dye is considered as the new way for solving the problems, such as silicon tetrachloride resource utilization.Preparing white carbon black by precipitation method is with industry water
Glass and sulfuric acid (or hydrochloric acid) are raw material to prepare white carbon black.If Chinese invention patent ZL 200910227609.1 is by four chlorinations
Silicon is slowly added in water, and reaction is hydrolyzed, while appropriate dispersing agent is added, and is prepared precipitated silica, in reaction process
The hydrogen chloride of generation can be used for producing polyvinyl chloride or trichlorosilane after carrying out gas phase recycling；Chinese invention patent CN
Silicon tetrachloride is added dropwise in Yu Yushui or alkaline solution 101712476A reacts, and precipitated silica is prepared；Middle promulgated by the State Council
Bright patent ZL201110086493.1 mixes silicon tetrachloride with solvent naphtha and water, and reaction generates precipitated silica；Chinese invention
Silicon tetrachloride is added dropwise in the water glass solution after dilution patent CN 102659118A, and reaction generates precipitated silica.It is above-mentioned
Although patent can prepare precipitated silica, exists and react the too drastic white carbon black partial size for being difficult to control, being prepared
Greatly, the disadvantages of poor activity, how to make that reaction is mild, white carbon black partial size is small and it is active it is big be always the difficulty for preparing precipitated silica
Topic.
The present invention uses venturi-type method, white by the way that precipitating is prepared with deionized water hybrid reaction in silicon tetrachloride
Carbon black has reaction mild controllable, and white carbon black partial size obtained is small, large specific surface area, the features such as activity is big.
Summary of the invention
The technical problem to be solved by the present invention is based on the above issues, the present invention provides a kind of polysilicon by-product tetrachloro
The resource utilization method of SiClx.
The present invention solves a technical solution used by its technical problem: a kind of silicon tetrachloride as by-product of polysilicon
Resource utilization method, comprising the following steps:
(1) at room temperature, dispersing agent is added in deionized water, is uniformly mixed, it is spare；
(2) entering for venturi tube inlet cylindrical section is added by mechanical pump in the silicon tetrachloride liquid in silicon tetrachloride storage tank
Mouthful, the mixed solution of deionized water and dispersing agent is introduced from Venturi tube cylindrical throat, makes silicon tetrachloride and deionized water
It reacting in Venturi tube, the mixture of Venturi tube circular cone diffuser opening discharge flows back into silicon tetrachloride storage tank,
Carry out circular response, the chemical equation of silicon tetrachloride and deionized water are as follows: SiCl4+2H2O=SiO2+4HCl；
(3) until the mixed solution of deionized water and dispersing agent all adds, mixture is aged in silicon tetrachloride storage tank,
Obtain solidliquid mixture；
(4) solidliquid mixture that step (3) obtains is sent to storage tank, is washed by box filter filtering, deionization
It washs, obtains filter cake and raffinate；
(5) deionized water is added in the filter cake for obtaining step (4), is made into slurry, and slurry is sent by pumping to spray drying tower,
It after heated-air drying, is collected by filtration by bag filter, obtains white carbon black.
Further, in step (1) and step (2) dispersing agent be one of both dehydrated alcohol, polyethylene glycol or
Two kinds, dehydrated alcohol dosage be silicon tetrachloride volume 200~1000%, polyethylene glycol dosage be silicon tetrachloride volume 0~
100%, the volume ratio of deionized water and silicon tetrachloride is 15~30:1.
Further, dehydrated alcohol dosage is the 400~750% of silicon tetrachloride volume in step (1) and step (2), is gathered
Ethylene glycol dosage is the 60~80% of silicon tetrachloride volume, and the volume ratio of deionized water and silicon tetrachloride is 20~25:1.
Further, the flow velocity of the mixed solution of deionized water and dispersing agent is silicon tetrachloride liquid flow velocity in step (2)
0.05~0.5, the flow velocity of silicon tetrachloride liquid is 3~5L/min.
Further, the flow velocity of the mixed solution of deionized water and dispersing agent is silicon tetrachloride liquid flow velocity in step (2)
0.08~0.12.
Further, digestion time is 0.5~3 hour in step (3).
Further, digestion time is 1~1.5 hour in step (3).
Further, the temperature of heated-air drying is 110~200 DEG C in step (5).
Further, the temperature of heated-air drying is 150~160 DEG C in step (5).
The beneficial effects of the present invention are: (1) directlys adopt deionized water as raw material, rather than traditional alkali generates water,
Energy consumption of reaction reduces, and safety greatly improves；(2) reaction condition is mild, safely controllable, can by control four silica flow velocitys and
The parameters such as deionized water velocity ratio, dispersant dosage and spray drying temperature control properties of product, obtain different aggregation partial sizes
With the silica product of specific surface area；(3) it is prepared as a raw material for production using four silica of by-product in production of polysilicon
Precipitated silica, efficiently solves that four silica of by-product in polysilicon industry is difficult to handle, resource utilization is low, pollution is big
The problem of, the health for promoting polysilicon industry rapidly develops, and reduces environmental pollution, energy-saving and emission-reduction.
Detailed description of the invention
The following further describes the present invention with reference to the drawings.
Fig. 1 is the structural block diagram for the equipment that the present invention uses；
Wherein: 1. silicon tetrachloride storage tanks, 2. deionized water dispersing agent storage tanks, 3. Venturi tubes, 3-1. inlet cylinders section, 3-
2. circular cone contraction section, 3-3. cylindrical throat, 3-4. circular cone diffuser, 4. circular cone diffusers, 5. box filters, 6. is spraying dry
Dry tower, 7. bag filters, 8. control valves.
Specific embodiment
Presently in connection with specific embodiment, the invention will be further described, following embodiment be intended to illustrate invention rather than
Limitation of the invention further.
Such as a kind of resource utilization equipment of Fig. 1 silicon tetrachloride as by-product of polysilicon shown, including consersion unit and rear place
Equipment is managed, consersion unit includes silicon tetrachloride storage tank 1, deionized water dispersing agent storage tank 2, Venturi tube 3, and Venturi tube 3 includes
Sequentially connected inlet cylinders section 3-1, circular cone contraction section 3-2, cylindrical throat 3-3 and circular cone diffuser 3-4, silicon tetrachloride storage
The output end of tank 1 and the input terminal pipeline connection of inlet cylinders section 3-1, the output end and cylinder of deionized water dispersing agent storage tank 2
The input terminal piping connection of shape throat 3-3, the output end of circular cone diffuser 3-4 and the input terminal pipeline of silicon tetrachloride storage tank 1 connect
It connects, the mechanical pump 4 for controlling its flow velocity, post-processing is installed on the pipeline between the output end and input terminal of silicon tetrachloride storage tank 1
Equipment includes box filter 5, spray drying tower 6 and bag filter 7.
Deionized water dispersing agent storage tank 2 is provided with the mixed solution of deionized water and dispersing agent, the storage of deionized water dispersing agent
Pipeline between tank 2 and cylindrical throat 3-3 is equipped with control valve 8.
Embodiment 1
By polyethylene glycol: dehydrated alcohol: deionized water is made into mixed solution according to volume ratio 0.8:6:20, stirs evenly,
It is spare.Silicon tetrachloride liquid is recycled with the rate of 5L/min by Venturi tube under the action of mechanical pump, into venturi
The volume ratio of the entrance of tube inlet cylindrical section, deionized water and silicon tetrachloride is 20:1.Control valve controls mixed solution flow velocity
The 0.1 of silicon tetrachloride liquid flow velocity, is slowly added to, and reacts silicon tetrachloride with water.After solution to be mixed all adds, control is closed
Valve processed continues at the ageing of silicon tetrachloride storage tank reaction 1 hour.By the mixture in silicon tetrachloride storage tank be put into after storage tank by
Box filter filtering and washing, obtain filter cake.Deionized water is added in filter cake and forms slurry, slurry is conveyed by mechanical pump
Dry in spray drying tower, control intake air temperature is 155 DEG C, and the powder after drying is collected by filtration by bag filter,
Obtain precipitated silica.Measuring its specific surface area is 507m2/ g, partial size are 326 ± 3nm, and analysis of components is detected such as 1 institute of table
Show, meets People's Republic of China's light industry food white carbon black QB/T2346-2007 standard.
Embodiment 2
By polyethylene glycol: dehydrated alcohol: deionized water is made into mixed solution according to volume ratio 0.6:5:25, stirs evenly,
It is spare.By silicon tetrachloride liquid to be recycled with the rate of 4L/min by Venturi tube under the action of mechanical pump, into literary mound
In tube inlet cylindrical section entrance, the volume ratio of deionized water and silicon tetrachloride is 25:1.Control valve controls mixed solution flow velocity
It is the 0.12 of silicon tetrachloride liquid flow velocity, is slowly added to, reacts silicon tetrachloride with water.After solution to be mixed all adds, close
Control valve is closed, is continued at the ageing of silicon tetrachloride storage tank reaction 1.5 hours.Mixture in silicon tetrachloride storage tank is put into storage tank
It filters and washs by box filter afterwards, obtain filter cake.Deionized water is added in filter cake and forms slurry, slurry is passed through into machinery
Pump is delivered to drying in spray drying tower, and control intake air temperature is 160 DEG C, and the powder after drying is filtered by bag filter
It collects, obtains precipitated silica.Measuring its specific surface area is 752m2/ g, partial size are 202 ± 5nm, and analysis of components detection is as follows
Shown in table, meet People's Republic of China's light industry food white carbon black QB/T2346-2007 standard.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (10)
1. a kind of resource utilization system of silicon tetrachloride as by-product of polysilicon, it is characterised in that: including consersion unit and rear place
Equipment is managed, the consersion unit includes: silicon tetrachloride storage tank, deionized water dispersing agent storage tank and Venturi tube, wherein institute
Silicon tetrachloride storage tank is stated for storing silicon tetrachloride liquid；The deionized water dispersing agent storage tank is for storing deionized water and dividing
The mixed solution of powder；The Venturi tube includes sequentially connected inlet cylinders section, circular cone contraction section, cylindrical throat and circle
Bore diffuser；
The input terminal pipeline connection of the output end of the silicon tetrachloride storage tank and the inlet cylinders section, by the silicon tetrachloride
Silicon tetrachloride liquid in storage tank is added by mechanical pump to the entrance of the inlet cylinders section of the Venturi tube, described to go
The output end of ion water dispersant storage tank and the input terminal piping connection of the cylindrical throat, the deionized water is dispersed
The mixed solution of deionized water and dispersing agent in agent storage tank is introduced from the cylindrical throat of the Venturi tube, so that four
Silicon chloride and deionized water react in the Venturi tube, the output end and the silicon tetrachloride of the circular cone diffuser
The input terminal piping connection of storage tank flows back into the mixture of the opening discharge of the circular cone diffuser of the Venturi tube
In the silicon tetrachloride storage tank, circular response is carried out, until the mixed solution of deionized water and dispersing agent all adds, mixture
It is aged in the silicon tetrachloride storage tank, obtains solidliquid mixture；
The equipment for after-treatment includes box filter, spray drying tower and bag filter；
Wherein, the box filter be used for in the silicon tetrachloride storage tank ageing obtain solidliquid mixture be filtered,
Deionized water washing, to obtain filter cake and raffinate；
The spray drying tower is used for the slurry being made into the filter cake obtained by the box filter by the way that deionized water is added
Heated-air drying is carried out, wherein the slurry is sent by pumping to the spray drying tower；
The bag filter is for being collected by filtration the slurry after the spray drying tower heated-air drying, to obtain white carbon black.
2. the resource utilization system of silicon tetrachloride as by-product of polysilicon according to claim 1, it is characterised in that: described
Mechanical pump is set on the pipeline between the output end and input terminal of the silicon tetrachloride storage tank to control its flow velocity；The deionization
Pipeline between water dispersant storage tank and the cylindrical throat is equipped with control valve.
3. a kind of resource utilization system of silicon tetrachloride as by-product of polysilicon according to claim 1, it is characterised in that:
The dispersing agent in the deionized water dispersing agent storage tank is one of both dehydrated alcohol, polyethylene glycol or two kinds,
Dehydrated alcohol dosage is the 200~1000% of silicon tetrachloride volume, and polyethylene glycol dosage is the 0~100% of silicon tetrachloride volume,
Deionized water and the volume ratio of silicon tetrachloride are 15~30:1.
4. the resource utilization system of silicon tetrachloride as by-product of polysilicon according to claim 3, it is characterised in that: anhydrous
Ethanol consumption be silicon tetrachloride volume 400~750%, polyethylene glycol dosage be silicon tetrachloride volume 60~80%, go from
The volume ratio of sub- water and silicon tetrachloride is 20~25:1.
5. the resource utilization system of silicon tetrachloride as by-product of polysilicon according to claim 2, it is characterised in that: described
The flow velocity of the mixed solution of control valve control deionized water and dispersing agent makes the 0.05~0.5 of its silicon tetrachloride liquid flow velocity,
It is 3~5L/min by the flow velocity that the mechanical pump controls silicon tetrachloride liquid.
6. the resource utilization system of silicon tetrachloride as by-product of polysilicon according to claim 5, it is characterised in that: described
The flow velocity of the mixed solution of control valve control deionized water and dispersing agent makes the 0.08~0.12 of its silicon tetrachloride liquid flow velocity.
7. the resource utilization system of silicon tetrachloride as by-product of polysilicon according to claim 1, it is characterised in that: mixing
Object digestion time in the silicon tetrachloride storage tank is set as 0.5~3 hour.
8. the resource utilization system of silicon tetrachloride as by-product of polysilicon according to claim 7, it is characterised in that: mixing
Object digestion time in the silicon tetrachloride storage tank is set as 1~1.5 hour.
9. the resource utilization system of silicon tetrachloride as by-product of polysilicon according to claim 1, it is characterised in that: described
The temperature of the heated-air drying of spray drying tower is set as 110~200 DEG C.
10. the resource utilization system of silicon tetrachloride as by-product of polysilicon according to claim 9, it is characterised in that: institute
The temperature for stating the heated-air drying of spray drying tower is set as 150~160 DEG C.
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| CN201610794942.0A CN106430221B (en) | 2016-08-31 | 2016-08-31 | A kind of resource utilization method of silicon tetrachloride as by-product of polysilicon |
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| CN201610794942.0A CN106430221B (en) | 2016-08-31 | 2016-08-31 | A kind of resource utilization method of silicon tetrachloride as by-product of polysilicon |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798088A (en) * | 2009-12-25 | 2010-08-11 | 河南科技大学 | Method for preparing white carbon black by utilizing silicon tetrachloride |
| CN102180470A (en) * | 2011-04-07 | 2011-09-14 | 赵志军 | Method for recycling silicon tetrachloride as by-product of polycrystalline silicon |
| CN102432026A (en) * | 2011-10-21 | 2012-05-02 | 安徽祥源安全环境科学技术有限公司 | Method for preparing white carbon black from polysilicon byproduct silicon tetrachloride |
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2016
- 2016-08-31 CN CN201610794942.0A patent/CN106430221B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798088A (en) * | 2009-12-25 | 2010-08-11 | 河南科技大学 | Method for preparing white carbon black by utilizing silicon tetrachloride |
| CN102180470A (en) * | 2011-04-07 | 2011-09-14 | 赵志军 | Method for recycling silicon tetrachloride as by-product of polycrystalline silicon |
| CN102432026A (en) * | 2011-10-21 | 2012-05-02 | 安徽祥源安全环境科学技术有限公司 | Method for preparing white carbon black from polysilicon byproduct silicon tetrachloride |
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