CN85107465A - New process for hydrogenation of silicon tetrachloride - Google Patents
New process for hydrogenation of silicon tetrachloride Download PDFInfo
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- CN85107465A CN85107465A CN 85107465 CN85107465A CN85107465A CN 85107465 A CN85107465 A CN 85107465A CN 85107465 CN85107465 CN 85107465 CN 85107465 A CN85107465 A CN 85107465A CN 85107465 A CN85107465 A CN 85107465A
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- hydrogenation
- sicl
- catalyst
- carry out
- temperature
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Abstract
SiCl
4New process for hydrogenation is that Powdered nickel accelerant is mixed by a certain percentage with silica flour, in the reactor of packing into, in nitrogen atmosphere and under 430 ℃ of temperature it is carried out 4 hours activation treatment after, can feed SiCl
4With H
2Mixed gas, carry out hydrogenation, temperature of reaction is 400～500 ℃, pressure 10～20kg/cm
2In the life-span of catalyst validity period, needn't add, hydrogenation can carry out continuously.
This novel process, simple to operate, SiCl
4Transformation efficiency height, energy consumption are lower.
Description
The invention belongs to hydrogenation of silicon tetrachloride technology.
At present, polysilicon factory all adopts silica flour and the synthetic SiHCl that produces of hydrogenchloride both at home and abroad
3In synthetic product, SiHCl
3Account for 80%, SiO
4Account for 20%.The exhaust condensate of this synthetic product and polysilicon reactor by slightly heat up in a steamer, after the rectifying, SiCl
4Go out SiHCl so that impurity is separated
3Then be used to produce polysilicon.
Domestic each silicon factory is for the SiCl that fractionates out
4, reasonably do not reclaim technology because of still having, and it is sold with chemical industry department or as waste disposal, thereby SiHCl
3Output capacity is low, has caused raw-material waste.
External silicon factory is to the SiCl of institute's output in producing
4, generally be to be catalyst with hydrogenchloride, cuprous chloride, or with diatomite, gac, Al
2O
3Under the condition that exists for the granular nickel salt of carrier, mantoquita catalyst, control certain temperature, pressure, make H
2, SiCl
4Mixed gas and silica flour contact with boiling state in reactor and carry out hydrogenation, make part of SiC l
4Change into SiHCl
3, the SiCl in its product
4Make after separating that it circulates repeatedly, hydrocracking reclaims.Its reaction formula is:
Above-mentioned SiCl
4The principal feature of hydroconversion process is mixed HCl or CuCl continuously with the fixed proportioning in hydrogenation process and is carried out with reactant.In order to strengthen reaction process, the reactor of a kind of multilayer insulating panel of employing that has is all put into silica flour and granular catalyst respectively, is made H for every layer
2, SiCl
4, HCl mixed gas by this multi-layered reactors to improve SiCl
4Transformation efficiency.
The shortcoming of above-mentioned technology is:
1. owing in technological process, need continuously HCl or CuCl to be mixed with reactant with fixed mixing ratio (being generally 5%), and SiCl
4A transformation efficiency lower (being generally 15%～18%) is so raw materials consumption is higher, plant efficiency is low.
2.HCl, CuCl and granular nickel salt, mantoquita catalyst activity be less, so the reaction conditions that requires is higher, pressure needs 21～35kg/cm
2, temperature is more than 500 ℃, so the energy energy consumption height of process, also high to the requirement of reactor.
Task of the present invention is sought a SiCl preferably exactly
4Hydrogenation process is to overcome the existing shortcoming of above-mentioned technology.Be characterized in adopting Powdered nickel accelerant of homemade NC-9-2 type and silica flour to be mixed in proportion, the individual layer gas of once packing into divides in the Fabric plate reactor, under nitrogen atmosphere, be heated to 430 ℃ of activation after, can carry out SiCl continuously
4Hydroconversion reactions.Its technological process is described below in conjunction with the accompanying drawings:
The Powdered nickel accelerant of NC-9-2 type and silica flour are packed into after by 2～4% mixed in the reactor III, feed the hydrogen that is heated to 430 ℃ through the preheater II then, the activation treatment that catalyst was carried out 4 hours under this temperature.The liquid SiCl of slightly, rectifying output
4Be heated to 90～129 ℃ and gasify in the volatilizer I, hydrogen is by mole ratio H
2: SiCl
4Enter volatilizer at=1～4: 1, with the SiCl that has been gasified
4Enter the preheater II after the mixing, enter continuously in the reactor III after mixed gas is heated to 300～400 ℃, the hydrogenation temperature is 400～500 ℃, pressure 10～20kg/cm
2The SiHCl of hydrogenation output
3With SiCl
4, and in the condenser VI, be condensed into liquid and enter in the phlegma storage tank VII through filter IV, pre-cooler V Deng mixed gas.
Advantage of the present invention is:
1. after catalyst once adds, in its life-span validity period, needn't add.So in the normal productive process just the silica flour that falls of postreaction get final product, so the catalyst consumption is few.
2. catalyst activity is good, and the condition that hydrogenation requires is lower, and reaction pressure is generally 15kg/cm
2, temperature is generally at 500 ℃.
3.SiCl
4A transformation efficiency height can reach 15～30%.
4. have only individual layer gas to divide Fabric plate in the reactor, thus simple in structure, easy handling.
Embodiment:
Reactor: diameter Dg 70mm, high 2m, bed depth 0.8m.
Processing condition: gas space velocity 0.072m/S, 500 ℃ of temperature of reaction, pressure 15kg/cm
2
Result: SiCl
4A transformation efficiency 26.74%.
Claims (3)
1, a kind of with gas SiCl
4After hydrogen mixes, carry out hydrogenation by the silicon powder layer that contains the certain proportion catalyst and generate SiHCl
3Method, it is characterized in that selected catalyst is Powdered nickel accelerant, this catalyst once adds in the reactor, activated processing, hydrogenation can carry out continuously, temperature of reaction is 400～500 ℃, pressure 10～20kg/cm
2
2, catalyst according to claim 1 is characterized in that at first and will carry out 4 hours activation treatment in 430 ℃ nitrogen atmosphere by being that 2～4% amount is mixed with the ratio of silica flour.
3, according to the described production of claim 1 SiHCl
3Method, it is characterized in that H
2With SiCl
4Mole ratio be 1～4: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85107465 CN85107465A (en) | 1985-10-12 | 1985-10-12 | New process for hydrogenation of silicon tetrachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85107465 CN85107465A (en) | 1985-10-12 | 1985-10-12 | New process for hydrogenation of silicon tetrachloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN85107465A true CN85107465A (en) | 1987-04-15 |
Family
ID=4795639
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 85107465 Pending CN85107465A (en) | 1985-10-12 | 1985-10-12 | New process for hydrogenation of silicon tetrachloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN85107465A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102639440A (en) * | 2009-08-04 | 2012-08-15 | 施米德硅晶片科技有限责任公司 | Process and system for producing trichlorosilane |
-
1985
- 1985-10-12 CN CN 85107465 patent/CN85107465A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102639440A (en) * | 2009-08-04 | 2012-08-15 | 施米德硅晶片科技有限责任公司 | Process and system for producing trichlorosilane |
| CN102639440B (en) * | 2009-08-04 | 2017-05-31 | 施米德硅晶片科技有限责任公司 | The method and apparatus for preparing silicochloroform |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |