CN110371985A - A kind of synthetic method of silicon tetrachloride - Google Patents
A kind of synthetic method of silicon tetrachloride Download PDFInfo
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- CN110371985A CN110371985A CN201910798604.8A CN201910798604A CN110371985A CN 110371985 A CN110371985 A CN 110371985A CN 201910798604 A CN201910798604 A CN 201910798604A CN 110371985 A CN110371985 A CN 110371985A
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- silicon tetrachloride
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- chlorine
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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
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10715—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material
- C01B33/10721—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material with the preferential formation of tetrachloride
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- Inorganic Chemistry (AREA)
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Abstract
The present invention relates to a kind of synthetic methods of silicon tetrachloride, silicon powder and the uncooled hydrogen chloride of cryogenic system react in fluidized bed reactor, and the trichlorosilane and silicon tetrachloride for reacting production successively enter cyclone separator, bag filter and hydrofilter and be dusted；Trichlorosilane and after wet dedusting reaction product mixing after enter photo catalysis reactor, chlorine and hydrogen are filled with from photo catalysis reactor bottom, trichlorosilane sufficiently reacts under light illumination with chlorine generates silicon tetrachloride and hydrogen chloride, and chlorine and hydrogen react under light illumination generates hydrogen chloride；The extraction at the top of photo catalysis reactor of light-catalyzed reaction product enters cryogenic system；For light-catalyzed reaction product after cryogenic system condensation is cooling, condensation liquid phase is crude product silicon tetrachloride, and crude product silicon tetrachloride enters subsequent refining system；Converting silicon tetrachloride rate >=98%.Reactor takes hot mode using outside, and whole process is generated without waste, environmentally protective.
Description
Technical field
The invention belongs to field polysilicons, are related to a kind of synthetic method of silicon tetrachloride, in particular to it is a kind of with chlorine and
Si powder is the method for Material synthesis silicon tetrachloride.
Background technique
High purity silicon tetrachloride is colourless transparent liquid, and the slightly lower presentation of purity is micro- yellow or faint yellow, there is stinkpot
It is corrosive to skin, is usually used in silicate class processed, organic silicon monomer, organic silicone oil, high-temperature insulation paint, silicone resin, silicon rubber
Deng also serving as screening smoke.Silicon tetrachloride is the by-product in polysilicon production process, but due to the influence of photovoltaic market, polycrystalline
Silicon raw materials for production trichlorosilane device majority stops production, and causes by-produced tetrachlorosilane fewer and fewer, silicon tetrachloride market is well sold and in short supply therewith.
Synthesis silicon tetrachloride is industrially directly reacted with hydrogen chloride frequently with silicon powder high temperature, this method reactive moieties are using boiling
Rise bed, converting silicon tetrachloride rate is 10-25%, trichlorosilane conversion ratio 75-90% at 300-400 DEG C of bubbling bed temperature, and is
The conversion ratio for improving silicon tetrachloride, generally requires for bubbling bed temperature to be increased to 800 DEG C or more, and silicon tetrachloride turns at this time
Rate 70-80%, the conversion ratio 20-30% of trichlorosilane improve although conversion that temperature is conducive to silicon tetrachloride, but four chlorinations
Silicon conversion is not still high, and requirement of the high temperature to equipment is harsh, and equipment cost is high.
Chinese patent CN201310360305.9 proposes the synthetic method and its production system of a kind of silicon tetrachloride, the party
Method includes the production stage and rectification step of silicon tetrachloride crude product, and the production stage of the silicon tetrachloride crude product is with silicon powder
Gas-solid direct synthesis is carried out with chlorine and reacts four chlorinations of preparation under the situation for not adding any catalyst for primary raw material
Silicon, reactor are fluidized bed；Controlling reaction temperature is 250-450 DEG C, and the fluidizing gas velocity of pressure 0.05-0.5MPa, chlorine are
0.05~0.15m/s；Silicon tetrachloride selectivity is 95% or more in crude product.However this method is not related to the recycling benefit of heat
With, it is more demanding to silicon powder and quality of chlorine gas, and fluidized bed control temperature is higher than 250 DEG C, chlorine has very when being higher than 250 DEG C
Strong corrosivity, the high requirements on the equipment.
Chinese patent CN201711066944.9 proposes the preparation method and reaction temperature controlling party of a kind of silicon tetrachloride
Method uses the silicon source containing silica and silicon carbide, the chlorine source containing chlorine and nitrogen for raw material, and temperature is controlled in reactor
Degree maintains 800-1500 DEG C and is reacted, and can control temperature by adjusting the content of chlorine and nitrogen.However this method is not
It is related to the recycling of heat, and temperature of reactor is higher than 800 DEG C, chlorine has very strong corrosivity when being higher than 250 DEG C, right
Equipment requirement is high.
It for the composition problem of silicon tetrachloride, needs to invent a kind of process, reaction can be reduced to material quality
It is required that effectively solving the conversion ratio of raising silicon tetrachloride, and the reaction temperature of silicon tetrachloride synthesis process can be reduced, reduce and close
Requirement at process to equipment material, and the heat in silicon tetrachloride synthesis process can all be recycled.
Summary of the invention
In order to solve problems in the prior art, the invention proposes a kind of silicon tetrachloride synthetic methods, with chlorine and silicon powder
For raw material, the device temperature contacted with chlorine is lower than 200 DEG C, and chlorine corrosivity when being lower than 200 DEG C is lower, thus to equipment material
Matter requires low；It is refrigerant using water in such a way that outside takes heat, steam is occurred into for the heat in reaction process, thus into one
Step recycles.The synthetic method of a kind of silicon tetrachloride of the invention, using fluidized bed reactor and two kinds of photo catalysis reactor
Reaction step synthesizes silicon tetrachloride, lower to raw material chlorine and silicon powder quality requirement, and converting silicon tetrachloride rate >=98%.
To achieve the above object, the present invention adopts the following technical scheme that realize:
A kind of silicon tetrachloride synthetic method, comprises the following steps that
(1) silicon powder and the uncooled hydrogen chloride of cryogenic system react in fluidized bed reactor, react the three of production
Chlorine hydrogen silicon and silicon tetrachloride produce at the top of fluidized bed reactor and successively enter cyclone separator, bag filter and wet process and remove
Dirt device is dusted；
(2) enter photo catalysis reactor, chlorine after reaction product mixing from extraneous trichlorosilane and after wet dedusting
Gas and hydrogen are filled with from photo catalysis reactor bottom, and in photo catalysis reactor, trichlorosilane and chlorine are sufficiently anti-under light illumination
Silicon tetrachloride and hydrogen chloride should be generated, chlorine and hydrogen react under light illumination generates hydrogen chloride；Light-catalyzed reaction product is urged from light
Change reactor head extraction and enters cryogenic system；
(3) for light-catalyzed reaction product after cryogenic system condensation is cooling, condensation liquid phase is crude product silicon tetrachloride, crude product four
Silicon chloride enters subsequent refining system；Uncooled gas phase is the hydrogen chloride and unreacted hydrogen that reaction generates, which returns
Fluidized bed reactor bottom.
Step (1) fluidized bed reactor controls 200-400 DEG C of reaction temperature.
Step (2) photo catalysis reactor controls 120-200 DEG C of reaction temperature.
Step (2) the photo catalysis reactor material is carbon steel or 304 stainless steels.
Step (1) (2) fluidized bed reactor and photo catalysis reactor are all made of external coil pipe and carry out taking heat, take heat
Medium is deionized water.
The step (2) can arbitrary proportion into trichlorosilane in the material of photo catalysis reactor and silicon tetrachloride.
It is 2:1-10:1 that the step (2), which enters photo catalysis reactor chlorine and the molar ratio of hydrogen,.
A kind of silicon tetrachloride synthetic method of the present invention, major advantage are as follows:
1, silicon tetrachloride is synthesized using two kinds of reaction steps of fluidized bed reactor and photo catalysis reactor, reaction process is secondary anti-
It should lack, the selectivity of silicon tetrachloride is high, and converting silicon tetrachloride rate >=98%.
2, reaction temperature is low, and required equipment material requirement is low, and photo catalysis reactor can be met the requirements using carbon steel material,
Reaction process is more safe and reliable.
3, into trichlorosilane in photo catalysis reactor material and silicon tetrachloride can arbitrary proportion, city can be well adapted to
Field demand.
4, the hydrogen chloride and unreacted hydrogen that reaction generates directly recycle, and avoid the SPA hydrogen manufacturing of traditional handicraft
Link avoids the accumulation of hydrogen in SPA hydrogen production process.
5, by the way of reactor takes heat using outside, heat of reaction is recycled from hair, and entire reaction process is without waste
It generates, it is environmentally protective.
Detailed description of the invention
A kind of silicon tetrachloride synthesis technology flow diagram of the invention is as shown in Figure 1.
Specific embodiment
The present invention is described in further detail in the following with reference to the drawings and specific embodiments:
Be described as follows according to Fig. 1: to achieve the above object, the following technical solution is realized:
A kind of device of the synthesis of silicon tetrachloride, mainly include fluidized bed reactor, cyclone separator, bag filter,
Hydrofilter, photo catalysis reactor, cryogenic system；Extraction mouth is sequentially connected cyclone separator, cloth at the top of fluidized bed reactor
Bag dust collector, hydrofilter；Hydrofilter produces mouth and connects photo catalysis reactor, sets and adds from photo catalysis reactor bottom
It is equipped with the entrance of chlorine and hydrogen, extraction mouth connects cryogenic system at the top of photo catalysis reactor；Cryogenic system gas phase produces mouth and connects
Fluidized bed reactor bottom is connect, cryogenic system is provided with silicon tetrachloride crude product liquid phase extraction mouth.
The fluidized bed reactor, for silicon powder and hcl reaction to be synthesized silicon tetrachloride, tower body uses external coil pipe
It carries out taking heat, produces reaction product at the top of fluidized bed reactor.
The cyclone separator is connect with the fluidized bed reactor, for unreacted silicon powder and gas phase reaction product
Separation.
The bag filter is connect with the cyclone separator, for the solid impurity in effective elimination reaction product.
The hydrofilter is connect with the bag filter, miscellaneous for the solid in further elimination reaction product
Matter.
The photo catalysis reactor is connect with the hydrofilter, for by the trichlorosilane in reaction product into one
Step reaction obtains silicon tetrachloride, while photo catalysis reactor bottom being provided with the entrance of chlorine and hydrogen, and hydrogen and chlorine exist
Reaction obtains hydrogen chloride in photo catalysis reactor, produces reaction product at the top of photo catalysis reactor.
The cryogenic system is connect with the photo catalysis reactor, and the reaction for will produce from photo catalysis reactor produces
Object condensation cooling, cryogenic system is equipped with gas phase extraction mouth and liquid phase produces mouth, and wherein gas phase extraction mouth connects fluidized bed reactor,
Liquid phase produces mouth and produces crude product silicon tetrachloride.
The uncooled hydrogen chloride of cryogenic system reacts with raw material Si powder in fluidized bed reactor and generates trichlorosilane
And silicon tetrachloride, water management temperature of reactor is added in the external heat collector of fluidized bed reactor, while steam occurs, by reaction heat
Amount sufficiently recycles；Extraction reaction product is through cyclone separator, bag filter, hydrofilter at the top of fluidized bed reactor
After dedusting, photo catalysis reactor, hydrogen and chlorine are mixed into from photo catalysis reactor bottom with from extraneous trichlorosilane
It is added, under the catalytic action of ultraviolet light, trichlorosilane is sufficiently reacted with chlorine generates silicon tetrachloride, and hydrogen and chlorine reaction are raw
At hydrogen chloride, water management temperature of reactor is added in the external heat collector of photo catalysis reactor, while steam occurs, by heat of reaction
Sufficiently recycle；After extraction reaction product enters cryogenic system condensation cooling at the top of photo catalysis reactor, gas phase is hydrogen chloride
And unreacted hydrogen returns to fluidized bed reactor, liquid phase is that silicon tetrachloride crude product enters subsequent fine processing procedure sequence.
The fluidized bed reactor controls 200-400 DEG C of reaction temperature.
The photo catalysis reactor controls 120-200 DEG C of reaction temperature.
The photo catalysis reactor material is carbon steel or S304 stainless steel.
The fluidized bed reactor and photo catalysis reactor is all made of external coil pipe and carries out taking heat, take thermal medium be go from
Sub- water.
Trichlorosilane and silicon tetrachloride can arbitrary proportions in the material into photo catalysis reactor.
It is described into the molar ratio of photo catalysis reactor chlorine and hydrogen be 2:1-10:1.
Embodiment 1
The uncooled hydrogen chloride of cryogenic system reacts with raw material Si powder in fluidized bed reactor and generates trichlorosilane
And silicon tetrachloride, it is 200 DEG C that water management temperature of reactor is added in the external heat collector of fluidized bed reactor, while steam occurs,
Heat of reaction is sufficiently recycled；Extraction reaction product is through cyclone separator, bag filter, wet at the top of fluidized bed reactor
After method deduster dedusting, it is mixed into photo catalysis reactor with from extraneous trichlorosilane, hydrogen and chlorine are anti-from photocatalysis
Answer device bottom be added, it is described into the molar ratio of photo catalysis reactor chlorine and hydrogen be 10:1, ultraviolet light catalysis make
Under, trichlorosilane is sufficiently reacted with chlorine generates silicon tetrachloride, and hydrogen and chlorine reaction generate hydrogen chloride, photo catalysis reactor
It is 120 DEG C that water management temperature of reactor is added in external heat collector, while steam occurs, and heat of reaction is sufficiently recycled；
After extraction reaction product enters cryogenic system condensation cooling at the top of photo catalysis reactor, gas phase is hydrogen chloride and unreacted hydrogen
Fluidized bed reactor is returned to, liquid phase is that silicon tetrachloride crude product enters subsequent fine processing procedure sequence.
After fluidized bed reactor and photo catalysis reactor effect, converting silicon tetrachloride rate >=98%
Embodiment 2
The uncooled hydrogen chloride of cryogenic system reacts with raw material Si powder in fluidized bed reactor and generates trichlorosilane
And silicon tetrachloride, it is 300 DEG C that water management temperature of reactor is added in the external heat collector of fluidized bed reactor, while steam occurs,
Heat of reaction is sufficiently recycled；Extraction reaction product is through cyclone separator, bag filter, wet at the top of fluidized bed reactor
After method deduster dedusting, it is mixed into photo catalysis reactor with from extraneous trichlorosilane, hydrogen and chlorine are anti-from photocatalysis
Answer device bottom be added, it is described into the molar ratio of photo catalysis reactor chlorine and hydrogen be 5:1, in the catalytic action of ultraviolet light
Under, trichlorosilane is sufficiently reacted with chlorine generates silicon tetrachloride, hydrogen and chlorine reaction generation hydrogen chloride, outside photo catalysis reactor
Setting and water management temperature of reactor is added in heat collector is 150 DEG C, while steam occurs, and heat of reaction is sufficiently recycled；Light
After extraction reaction product enters cryogenic system condensation cooling at the top of catalytic reactor, gas phase is that hydrogen chloride and unreacted hydrogen return
Fluidized bed reactor is returned, liquid phase is that silicon tetrachloride crude product enters subsequent fine processing procedure sequence.
After fluidized bed reactor and photo catalysis reactor effect, converting silicon tetrachloride rate >=98%
Embodiment 3
The uncooled hydrogen chloride of cryogenic system reacts with raw material Si powder in fluidized bed reactor and generates trichlorosilane
And silicon tetrachloride, it is 400 DEG C that water management temperature of reactor is added in the external heat collector of fluidized bed reactor, while steam occurs,
Heat of reaction is sufficiently recycled；Extraction reaction product is through cyclone separator, bag filter, wet at the top of fluidized bed reactor
After method deduster dedusting, it is mixed into photo catalysis reactor with from extraneous trichlorosilane, hydrogen and chlorine are anti-from photocatalysis
Answer device bottom be added, it is described into the molar ratio of photo catalysis reactor chlorine and hydrogen be 2:1, in the catalytic action of ultraviolet light
Under, trichlorosilane is sufficiently reacted with chlorine generates silicon tetrachloride, hydrogen and chlorine reaction generation hydrogen chloride, outside photo catalysis reactor
Setting and water management temperature of reactor is added in heat collector is 200 DEG C, while steam occurs, and heat of reaction is sufficiently recycled；Light
After extraction reaction product enters cryogenic system condensation cooling at the top of catalytic reactor, gas phase is that hydrogen chloride and unreacted hydrogen return
Fluidized bed reactor is returned, liquid phase is that silicon tetrachloride crude product enters subsequent fine processing procedure sequence.
After fluidized bed reactor and photo catalysis reactor effect, converting silicon tetrachloride rate >=98%.
A kind of silicon tetrachloride synthetic method of the present invention synthesizes silicon tetrachloride using two-step method, to raw material chlorine and silicon powder matter
Amount requires lower, and converting silicon tetrachloride rate >=98%；Reaction temperature is low, and required equipment material requires low, photo catalysis reactor
It can be met the requirements using carbon steel material, reaction process is more safe and reliable；Into trichlorosilane in photo catalysis reactor material
With the ratio of silicon tetrachloride can arbitrary proportion allotment, the market demand can be well adapted to；React generate hydrogen chloride and not instead
The hydrogen answered directly recycles, and avoids the SPA hydrogen manufacturing link of traditional handicraft, avoids the tired of hydrogen in SPA hydrogen production process
Product；By the way of reactor is reduced phlegm and internal heat using outside, heat of reaction is recycled from hair, and entire reaction process is generated without waste, green
Colour circle is protected.
Claims (7)
1. a kind of synthetic method of silicon tetrachloride, it is characterized in that comprising the following steps that
(1) silicon powder and the uncooled hydrogen chloride of cryogenic system react in fluidized bed reactor, react the trichlorine hydrogen of production
Silicon and silicon tetrachloride produce at the top of fluidized bed reactor and successively enter cyclone separator, bag filter and hydrofilter
It is dusted；
(2) enter photo catalysis reactor after reaction product mixing from extraneous trichlorosilane and after wet dedusting, chlorine and
Hydrogen is filled with from photo catalysis reactor bottom, and in photo catalysis reactor, trichlorosilane sufficiently reacts life with chlorine under light illumination
At silicon tetrachloride and hydrogen chloride, chlorine and hydrogen react generate hydrogen chloride under light illumination；Light-catalyzed reaction product is anti-from photocatalysis
Extraction at the top of device is answered to enter cryogenic system；
(3) for light-catalyzed reaction product after cryogenic system condensation is cooling, condensation liquid phase is crude product silicon tetrachloride, four chlorination of crude product
Silicon enters subsequent refining system；Uncooled gas phase is the hydrogen chloride and unreacted hydrogen that reaction generates, which returns to boiling
Bed reactor bottom.
2. the method as described in claim 1, it is characterized in that step (1) fluidized bed reactor controls reaction temperature 200-
400℃。
3. the method as described in claim 1, it is characterized in that step (2) photo catalysis reactor controls reaction temperature 120-
200℃。
4. the method as described in claim 1, it is characterized in that step (2) the photo catalysis reactor material is carbon steel or 304
Stainless steel.
5. the method as described in claim 1, it is characterized in that the step (1) or (2) fluidized bed reactor and photocatalysis are anti-
It answers device to be all made of external coil pipe to carry out taking heat, taking thermal medium is deionized water.
6. the method as described in claim 1, it is characterized in that the step (2) enters trichlorine in the material of photo catalysis reactor
Hydrogen silicon and silicon tetrachloride can arbitrary proportions.
7. the method as described in claim 1, it is characterized in that the step (2) enters photo catalysis reactor chlorine and hydrogen
Molar ratio is 2:1-10:1.
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| RU2457178C1 (en) * | 2011-01-11 | 2012-07-27 | ФГУП "Российский научный центр "Прикладная химия" | Method of producing high-purity monosilane and silicon tetrachloride |
| CN105800618A (en) * | 2016-02-29 | 2016-07-27 | 天津大学 | Method and device for producing optical fiber-grade silicon tetrachloride |
| CN108101065A (en) * | 2017-11-29 | 2018-06-01 | 天津中科拓新科技有限公司 | A kind of method for preparing industrial grade silicon tetrachloride |
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2019
- 2019-08-27 CN CN201910798604.8A patent/CN110371985A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2254291C1 (en) * | 2003-11-11 | 2005-06-20 | Открытое акционерное общество "Подольский химико-металлургический завод" | Method of production of trichlorosilane |
| CN101638233A (en) * | 2009-08-24 | 2010-02-03 | 洛阳中硅高科技有限公司 | Dry method recovery technique of trichlorosilane synthetic tail gas |
| CN102557042A (en) * | 2010-12-24 | 2012-07-11 | 北京有色金属研究总院 | Method for removing impurity trichlorosilane from silicon tetrachloride |
| RU2457178C1 (en) * | 2011-01-11 | 2012-07-27 | ФГУП "Российский научный центр "Прикладная химия" | Method of producing high-purity monosilane and silicon tetrachloride |
| CN105800618A (en) * | 2016-02-29 | 2016-07-27 | 天津大学 | Method and device for producing optical fiber-grade silicon tetrachloride |
| CN108101065A (en) * | 2017-11-29 | 2018-06-01 | 天津中科拓新科技有限公司 | A kind of method for preparing industrial grade silicon tetrachloride |
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