CN102311453A - Method for preparing phenyltrichlorosilane from polysilicon by-product trichlorosilane - Google Patents
Method for preparing phenyltrichlorosilane from polysilicon by-product trichlorosilane Download PDFInfo
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- CN102311453A CN102311453A CN201110320772A CN201110320772A CN102311453A CN 102311453 A CN102311453 A CN 102311453A CN 201110320772 A CN201110320772 A CN 201110320772A CN 201110320772 A CN201110320772 A CN 201110320772A CN 102311453 A CN102311453 A CN 102311453A
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- trichlorosilane
- chlorobenzene
- silicane
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Abstract
The invention provides a method for preparing phenyltrichlorosilane from polysilicon by-product trichlorosilane. The method comprises the following steps that trichlorosilane and chlorobenzene are preheated respectively and undergo a thermal condensation reaction; and the products obtained by the previous step are subjected to condensation, fractionation and recondensation to form phenyltrichlorosilane. The method can prepare phenyltrichlorosilane from polysilicon by-product trichlorosilane. The method can realize reasonable utilization of low-purity trichlorosilane, save energy and resources, realize low consumption and high output, reduce production cost, and improve production efficiency and social benefits.
Description
Technical field
The present invention relates to a kind of method for preparing phenyl-trichloro-silicane by polysilicon by product trichlorosilane.
Background technology
Phenyl-trichloro-silicane Chinese full name one phenyl-trichloro-silicane is commonly called as phenyl chlorosilane, benzene for trichlorosilane, English name: Phenyltrichlorosilane, and molecular formula is C
6H
5SiCl
3
Publication number is that disclosing a kind of in the patent of invention " preparation method of phenyl-trichloro-silicane and device " of CN101875663A is the method for feedstock production phenyl-trichloro-silicane with the certified products trichlorosilane; Its raw material adopts the certified products trichlorosilane; Trichlorosilane is claimed trichlorosilane, trichlorosilane again, and molecular formula is SiHCl
3The complex manufacturing of certified products trichlorosilane, price is higher, and the production cost of this invention is high.The production process of certified products trichlorosilane is: silica flour joins trichlorosilane synthetic furnace after super-dry, with the down reaction of hydrogenchloride high temperature, generates the bullion trichlorosilane, thick trichlorosilane gas through cyclonic separation, dust removal and filtration after, condensing surface.Non-condensable gas will send tail gas washing tower through fluid-tight, and the phlegma distillation tower separate to be purified, adopt two towers to purify continuously after, go out the trichlorosilane product from cat head.The trichlorosilane that obtains also will take off the production that boron, dephosphorization just can be used for polysilicon, and the silicon tetrachloride that produces is difficult to handle.
It is that trichlorosilane more than 99% is a raw material that the polysilicon industry needs purity, further refiningly improves purity of trichlorosilane and restores the production polysilicon product.In recent years, domestic polysilicon industry is fast-developing, and the coming five years polysilicon output will increase fast, and simultaneously, by product low-purity trichlorosilane output also will increase fast, if can not effectively utilize, will cause the wasting of resources and environmental stress.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method that is prepared phenyl-trichloro-silicane by polysilicon by product trichlorosilane.
For solving the problems of the technologies described above, the invention provides and a kind ofly prepare the method for phenyl-trichloro-silicane by polysilicon by product trichlorosilane, comprise following process step:
A, trichlorosilane and chlorobenzene are pressed in the preheater separately with nitrogen respectively, the weight percent concentration of trichlorosilane is 50% ~ 90%, and the weight ratio of trichlorosilane and chlorobenzene is 1: (0.5～1.5);
B, trichlorosilane and chlorobenzene are heated to 201～600 ℃ respectively in preheater separately after, get in the steel tubular reactor drum more together;
C, in the steel tubular reactor drum; Trichlorosilane and chlorobenzene are heated to 500～700 ℃ together; And trichlorosilane and chlorobenzene be-0.1 at pressure～-0.09MPa, duration of contact carry out the thermal condensation reaction under 3～40 seconds, the condition of continuous feeding and discharging, generate the mixed gas that contains phenyl-trichloro-silicane;
The mixed gas of d, outflow steel tubular reactor drum gets into first condensing surface and is condensed into below 50 ℃, obtains containing first phlegma of phenyl-trichloro-silicane, silicon tetrachloride, benzene, chlorobenzene;
E, let first phlegma get in the separation column to be heated; By the boiling point of component order, at the following gas of cat head elder generation's aftercut intercepting: when temperature is 56～59 ℃ the intercepting silicon tetrachloride, when temperature is 78～82 ℃ intercepting benzene, when temperature is 128～133 ℃ the intercepting chlorobenzene, when temperature is 198～203 ℃ the intercepting phenyl-trichloro-silicane.
Method provided by the invention utilizes polysilicon by product trichlorosilane to prepare phenyl-trichloro-silicane, the low-purity trichlorosilane has been carried out reasonable utilization, save energy, resource; Realize low consumption; High production has reduced production cost, has improved productivity effect and social benefit.
As optimization of the present invention; Following gas with said e step: silicon tetrachloride, benzene, chlorobenzene, phenyl-trichloro-silicane get into second condensing surface successively and are condensed into below 50 ℃, obtain the corresponding phlegma of silicon tetrachloride, benzene, chlorobenzene, phenyl-trichloro-silicane respectively.Be beneficial to preserve, transport.
The uncooled tail gas that obtains when in first condensing surface gas being carried out condensation, its staple is HCl, gets into the tail gas recycle treatment system and can be made into hydrochloric acid and sell.
Embodiment
Further specify the present invention through embodiment below.
Embodiment 1
Prepare the method for phenyl-trichloro-silicane by polysilicon by product trichlorosilane, comprise following process step:
A, 1000kg trichlorosilane and 500kg chlorobenzene are pressed in the preheater separately with nitrogen respectively, the weight percent concentration of trichlorosilane is 50%;
B, trichlorosilane and chlorobenzene are heated to 600 ℃ respectively in preheater separately after, get in the steel tubular reactor drum more together;
C, in the steel tubular reactor drum; Trichlorosilane and chlorobenzene are heated to 700 ℃ together; And trichlorosilane and chlorobenzene be-0.1 at pressure～-0.09MPa, duration of contact carry out the thermal condensation reaction under 3～40 seconds, the condition of continuous feeding and discharging, generate the mixed gas that contains phenyl-trichloro-silicane;
The mixed gas of d, outflow steel tubular reactor drum gets into first condensing surface and is condensed into below 50 ℃, obtains containing first phlegma of phenyl-trichloro-silicane, silicon tetrachloride, benzene, chlorobenzene;
E, let first phlegma intermittently get in the tower still of separation column to be heated; By the boiling point of component order, at the following gas of cat head elder generation's aftercut intercepting: when temperature is 56～59 ℃ the intercepting silicon tetrachloride, when temperature is 78～82 ℃ intercepting benzene, when temperature is 128～133 ℃ the intercepting chlorobenzene, when temperature is 198～203 ℃ the intercepting phenyl-trichloro-silicane.
F, the gas that the e step is obtained: silicon tetrachloride, benzene, chlorobenzene, phenyl-trichloro-silicane get into second condensing surface successively and are condensed into below 50 ℃, obtain the corresponding phlegma of silicon tetrachloride, benzene, chlorobenzene, phenyl-trichloro-silicane respectively.
Wherein, Polysilicon by product trichlorosilane can silicon industry development in science and technology ltd be buied from Jiangsu; The phone of the said firm is: 0516-85868888; The address of the said firm is: Xuzhou City, Jiangsu Province economic and technological development zone, and the quality index of polysilicon by product trichlorosilane is: weight percent concentration: 50%; Outward appearance: colourless transparent liquid has micro-mechanical impurity; Boron (B)≤350ppb, phosphorus (P)≤250ppb.
Tail gas in the production process is processed hydrochloric acid through recovery and processing system.
Embodiment 2
Prepare the method for phenyl-trichloro-silicane by polysilicon by product trichlorosilane, comprise following process step:
A, 1000kg trichlorosilane and 1000kg chlorobenzene are pressed in the preheater separately with nitrogen respectively, the weight percent concentration of trichlorosilane is 75%;
B, trichlorosilane and chlorobenzene are heated to 400 ℃ respectively in preheater separately after, get in the steel tubular reactor drum more together;
C, in the steel tubular reactor drum; Trichlorosilane and chlorobenzene are heated to 650 ℃ together; And trichlorosilane and chlorobenzene be-0.1 at pressure～-0.09MPa, duration of contact carry out the thermal condensation reaction under 3～40 seconds, the condition of continuous feeding and discharging, generate the mixed gas that contains phenyl-trichloro-silicane;
The mixed gas of d, outflow steel tubular reactor drum gets into first condensing surface and is condensed into below 50 ℃, obtains containing first phlegma of phenyl-trichloro-silicane, silicon tetrachloride, benzene, chlorobenzene;
E, let first phlegma intermittently get in the tower still of separation column to be heated; By the boiling point of component order, at the following gas of cat head elder generation's aftercut intercepting: when temperature is 56～59 ℃ the intercepting silicon tetrachloride, when temperature is 78～82 ℃ intercepting benzene, when temperature is 128～133 ℃ the intercepting chlorobenzene, when temperature is 198～203 ℃ the intercepting phenyl-trichloro-silicane.
F, the gas that the e step is obtained: silicon tetrachloride, benzene, chlorobenzene, phenyl-trichloro-silicane get into second condensing surface successively and are condensed into below 50 ℃, obtain the corresponding phlegma of silicon tetrachloride, benzene, chlorobenzene, phenyl-trichloro-silicane respectively.
Wherein, Polysilicon by product trichlorosilane can silicon industry development in science and technology ltd be buied from Jiangsu; The phone of the said firm is: 0516-85868888; The address of the said firm is: Xuzhou City, Jiangsu Province economic and technological development zone, and the quality index of polysilicon by product trichlorosilane is: weight percent concentration: 75%; Outward appearance: colourless transparent liquid has micro-mechanical impurity; Boron (B)≤350ppb, phosphorus (P)≤250ppb.
Tail gas in the production process is processed hydrochloric acid through recovery and processing system.
Embodiment 3
Prepare the method for phenyl-trichloro-silicane by polysilicon by product trichlorosilane, comprise following process step:
A, 1000kg trichlorosilane and 1500kg chlorobenzene are pressed in the preheater separately with nitrogen respectively, the weight percent concentration of trichlorosilane is 90%;
B, trichlorosilane and chlorobenzene are heated to 201 ℃ respectively in preheater separately after, get in the steel tubular reactor drum more together;
C, in the steel tubular reactor drum; Trichlorosilane and chlorobenzene are heated to 500 ℃ together; And trichlorosilane and chlorobenzene be-0.1 at pressure～-0.09MPa, duration of contact carry out the thermal condensation reaction under 3～40 seconds, the condition of continuous feeding and discharging, generate the mixed gas that contains phenyl-trichloro-silicane;
The mixed gas of d, outflow steel tubular reactor drum gets into first condensing surface and is condensed into below 50 ℃, obtains containing first phlegma of phenyl-trichloro-silicane, silicon tetrachloride, benzene, chlorobenzene;
E, let first phlegma intermittently get in the tower still of separation column to be heated; By the boiling point of component order, at the following gas of cat head elder generation's aftercut intercepting: when temperature is 56～59 ℃ the intercepting silicon tetrachloride, when temperature is 78～82 ℃ intercepting benzene, when temperature is 128～133 ℃ the intercepting chlorobenzene, when temperature is 198～203 ℃ the intercepting phenyl-trichloro-silicane.
F, the gas that the e step is obtained: silicon tetrachloride, benzene, chlorobenzene, phenyl-trichloro-silicane get into second condensing surface successively and are condensed into below 50 ℃, obtain the corresponding phlegma of silicon tetrachloride, benzene, chlorobenzene, phenyl-trichloro-silicane respectively.
Wherein, Polysilicon by product trichlorosilane can silicon industry development in science and technology ltd be buied from Jiangsu; The phone of the said firm is: 0516-85868888; The address of the said firm is: Xuzhou City, Jiangsu Province economic and technological development zone, and the quality index of polysilicon by product trichlorosilane is: weight percent concentration: 90%; Outward appearance: colourless transparent liquid has micro-mechanical impurity; Boron (B)≤350ppb, phosphorus (P)≤250ppb.
Tail gas in the production process is processed hydrochloric acid through recovery and processing system.
Claims (2)
1. prepare the method for phenyl-trichloro-silicane by polysilicon by product trichlorosilane, comprise following process step:
A, trichlorosilane and chlorobenzene are pressed in the preheater separately with nitrogen respectively, the weight percent concentration of trichlorosilane is 50% ~ 90%, and the weight ratio of trichlorosilane and chlorobenzene is 1: (0.5～1.5);
B, trichlorosilane and chlorobenzene are heated to 201～600 ℃ respectively in preheater separately after, get in the steel tubular reactor drum more together;
C, in the steel tubular reactor drum; Trichlorosilane and chlorobenzene are heated to 500～700 ℃ together; And trichlorosilane and chlorobenzene be-0.1 at pressure～-0.09MPa, duration of contact carry out the thermal condensation reaction under 3～40 seconds, the condition of continuous feeding and discharging, generate the mixed gas that contains phenyl-trichloro-silicane;
The mixed gas of d, outflow steel tubular reactor drum gets into first condensing surface and is condensed into below 50 ℃, obtains containing first phlegma of phenyl-trichloro-silicane, silicon tetrachloride, benzene, chlorobenzene;
E, let first phlegma get in the separation column to be heated; By the boiling point of component order, at the following gas of cat head elder generation's aftercut intercepting: when temperature is 56～59 ℃ the intercepting silicon tetrachloride, when temperature is 78～82 ℃ intercepting benzene, when temperature is 128～133 ℃ the intercepting chlorobenzene, when temperature is 198～203 ℃ the intercepting phenyl-trichloro-silicane.
2. the method for preparing phenyl-trichloro-silicane by polysilicon by product trichlorosilane according to claim 1; It is characterized in that: let the following gas of e step: silicon tetrachloride, benzene, chlorobenzene, phenyl-trichloro-silicane get into second condensing surface successively and are condensed into below 50 ℃, obtain the corresponding phlegma of silicon tetrachloride, benzene, chlorobenzene, phenyl-trichloro-silicane respectively.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110320772A CN102311453A (en) | 2011-10-20 | 2011-10-20 | Method for preparing phenyltrichlorosilane from polysilicon by-product trichlorosilane |
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| CN201110320772A CN102311453A (en) | 2011-10-20 | 2011-10-20 | Method for preparing phenyltrichlorosilane from polysilicon by-product trichlorosilane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114588845A (en) * | 2022-03-16 | 2022-06-07 | 陕西德信祥能源科技有限公司 | Synthesis system of phenyl chlorosilane |
Citations (5)
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|---|---|---|---|---|
| GB695761A (en) * | 1950-08-10 | 1953-08-19 | British Thomson Houston Co Ltd | Improvements in and relating to aryl-substituted halogenosilanes |
| GB1088720A (en) * | 1964-10-14 | 1967-10-25 | Ceskoslovenska Akademie Ved | Process for the manufacture of phenylchlorosilanes |
| CN1807238A (en) * | 2005-10-26 | 2006-07-26 | 杭州师范学院 | Special type organochlorosilane preparation method |
| CN101693720A (en) * | 2009-09-15 | 2010-04-14 | 杭州师范大学 | Method for utilizing silicon chloride to prepare phenyl-trichloro-silicane and diphenyl dichlorosilane through Gerber method |
| CN101875663A (en) * | 2010-04-30 | 2010-11-03 | 蚌埠合众硅氟新材料有限公司 | Preparation method and device of phenyl trichlorosilane |
-
2011
- 2011-10-20 CN CN201110320772A patent/CN102311453A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB695761A (en) * | 1950-08-10 | 1953-08-19 | British Thomson Houston Co Ltd | Improvements in and relating to aryl-substituted halogenosilanes |
| GB1088720A (en) * | 1964-10-14 | 1967-10-25 | Ceskoslovenska Akademie Ved | Process for the manufacture of phenylchlorosilanes |
| CN1807238A (en) * | 2005-10-26 | 2006-07-26 | 杭州师范学院 | Special type organochlorosilane preparation method |
| CN101693720A (en) * | 2009-09-15 | 2010-04-14 | 杭州师范大学 | Method for utilizing silicon chloride to prepare phenyl-trichloro-silicane and diphenyl dichlorosilane through Gerber method |
| CN101875663A (en) * | 2010-04-30 | 2010-11-03 | 蚌埠合众硅氟新材料有限公司 | Preparation method and device of phenyl trichlorosilane |
Non-Patent Citations (1)
| Title |
|---|
| 陈建强: "苯基氯硅烷的研究及其应用", 《浙江化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114588845A (en) * | 2022-03-16 | 2022-06-07 | 陕西德信祥能源科技有限公司 | Synthesis system of phenyl chlorosilane |
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Application publication date: 20120111 |