CN105236413A - Silicon tetrachloride preparation method - Google Patents
Silicon tetrachloride preparation method Download PDFInfo
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- CN105236413A CN105236413A CN201510601692.XA CN201510601692A CN105236413A CN 105236413 A CN105236413 A CN 105236413A CN 201510601692 A CN201510601692 A CN 201510601692A CN 105236413 A CN105236413 A CN 105236413A
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- silicon tetrachloride
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Abstract
The invention relates to a silicon tetrachloride preparation method. The method comprises the following steps: 1, adding a metal catalyst into a reaction kettle provided with diatomite as a raw material, adding liquid chlorine, introducing nitrogen at a speed of 0.1-0.2m/s to remove air in the reaction kettle, and carrying out a chlorination reaction at 500-700DEG C for 3-5h; and 2, cooling after the reaction ends, filtering, transferring the obtained filtrate into a rectifying tower, heating and controlling the tower top temperature and the tower bottom temperature with inert gas as protection atmosphere, carrying out low temperature gas removal for 8-15h, carrying out total refluxing at a refluxing ratio of 10:1-18:1 for 4-6h, removing low boiling point substances from the tower top, collecting intermediate fraction, and filling to obtain silicon tetrachloride. The method has the advantages of easily available raw material, mild reaction conditions, easy purification of the above product, high yield and high purity of the product, simple operation and easy realization of industrialization.
Description
Technical field
The present invention relates to chemical field, particularly a kind of preparation method of silicon tetrachloride.
Background technology
Silicon tetrachloride is the most simple compounds that chlorine combines with silicon, molecular formula: SiCl
4, molecular weight: 169.90, proportion is 1.50, fusing point-70 DEG C, boiling point 57.6 DEG C, and the silicon tetrachloride of industrial one-level is colourless transparent liquid at normal temperatures.
The preparation method of silicon tetrachloride, comprise the most original silica sand chlorination process to rise, experienced by silicon carbide (silicon carbide) chlorination, ferrosilicon chlorination to elemental silicon chlorination several stage, these technological developments are all that searching is new, the silicon source that easier and chlorine reacts.Chlorination due to silicon is the process of high energy consumption, and many experts are endeavouring to explore new approach, to break away from the manufacturing process of high power consumption.The research that silicon tetrachloride manufactures novel process has industrial realistic meaning.Silicon tetrachloride belongs to important Chemicals, can manufacture gas-phase silica (high purity ultra-fine silicon dioxide), organosilane, silicon rubber, elemental silicon and semi-conductor pure silicon etc.These products permeate widely in each industrial circle.In general the production of senior silicon product, all has certain relation with silicon tetrachloride.And the value of these products is all very high, as gas-phase silica, tetraethyl silicate, elemental silicon etc., value per ton, all more than 10,000 yuan, belongs to meticulous Chemicals.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of silicon tetrachloride.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of preparation method of silicon tetrachloride, and step is:
(1) in reactor, with diatomite meeting raw material, add metal catalyst, add liquid chlorine, adopt simultaneously and pass into nitrogen and drive air in reactor away, carry out chlorination reaction, temperature of reaction is 500-700 DEG C, reaction times 3-5h, the speed that passes into of nitrogen is 0.1-0.2m/s, and described metal catalyst is copper;
(2) after reaction terminates; cooling; filter, filtrate is proceeded to rectifying tower, using rare gas element as protective atmosphere; heat up and control tower top temperature and bottom temperature; low temperature through 8-15h catches up with gas and 4-6h total reflux, chooses reflux ratio 10:1-18:1, and tower top gets rid of lower boiling; collect middle runnings, filling silicon tetrachloride.
In a preferred embodiment of the present invention, in step (1), diatomaceous particle diameter is 10-200 order.
In a preferred embodiment of the present invention, the temperature of reaction in step (1) is 550-650 DEG C, reaction times 3.5-4.5h, and the speed that passes into of nitrogen is 0.15-0.18m/s.
In a preferred embodiment of the present invention, described in step (1), the purity of liquified chlorine gas is 99.99%.
In a preferred embodiment of the present invention, the rectifying tower described in step (2) is the tray column of quartzy material.
In a preferred embodiment of the present invention, the tower top temperature described in step (2) is 50-60 DEG C.
In a preferred embodiment of the present invention, the bottom temperature described in step (2) is 70-80 DEG C.
In a preferred embodiment of the present invention, rapid reflux ratio described in (2) is 14:1-16:1.
Beneficial effect of the present invention is, owing to have employed technique scheme, method of the present invention not only raw material is easy to get, and reaction conditions is gentle, and product is easy to purifying, and product yield and purity higher, simple to operate, be easy to realize industrialization.
Embodiment
The specific embodiment of the present invention is described in detail as follows, but for illustrative purposes only instead of restriction the present invention.
Embodiment 1
(1) in reactor, can raw materials with 10 order diatomite, add copper powder, add liquid chlorine, adopt simultaneously and pass into nitrogen and drive air in reactor away, carry out chlorination reaction, temperature of reaction is 500 DEG C, reaction times 5h, and the speed that passes into of nitrogen is 0.1-0.2m/s;
(2) after reaction terminates; cooling; filter, filtrate is proceeded to rectifying tower, using rare gas element as protective atmosphere; heat up and control tower top temperature and bottom temperature; low temperature through 8h catches up with gas and 6h total reflux, chooses reflux ratio 10:1, and tower top gets rid of lower boiling; collect middle runnings, filling silicon tetrachloride.
Embodiment 2
(1) in reactor, can raw materials with 50 order diatomite, add copper powder, add liquid chlorine, adopt simultaneously and pass into nitrogen and drive air in reactor away, carry out chlorination reaction, temperature of reaction is 600 DEG C, reaction times 4h, and the speed that passes into of nitrogen is 0.1-0.2m/s;
(2) after reaction terminates; cooling; filter, filtrate is proceeded to rectifying tower, using rare gas element as protective atmosphere; heat up and control tower top temperature and bottom temperature; low temperature through 10h catches up with gas and 6h total reflux, chooses reflux ratio 12:1, and tower top gets rid of lower boiling; collect middle runnings, filling silicon tetrachloride.
Embodiment 3
(1) in reactor, can raw materials with 100 order diatomite, add copper powder, add liquid chlorine, adopt simultaneously and pass into nitrogen and drive air in reactor away, carry out chlorination reaction, temperature of reaction is 650 DEG C, reaction times 4h, and the speed that passes into of nitrogen is 0.1-0.2m/s;
(2) after reaction terminates; cooling; filter, filtrate is proceeded to rectifying tower, using rare gas element as protective atmosphere; heat up and control tower top temperature and bottom temperature; low temperature through 12h catches up with gas and 5h total reflux, chooses reflux ratio 14:1, and tower top gets rid of lower boiling; collect middle runnings, filling silicon tetrachloride.
Embodiment 4
(1) in reactor, can raw material with diatomite, add metal catalyst, add liquid chlorine, adopt simultaneously and pass into nitrogen and drive air in reactor away, carry out chlorination reaction, temperature of reaction is 700 DEG C, reaction times 3h, and the speed that passes into of nitrogen is 0.1-0.2m/s;
(2) after reaction terminates; cooling; filter, filtrate is proceeded to rectifying tower, using rare gas element as protective atmosphere; heat up and control tower top temperature and bottom temperature; low temperature through 14h catches up with gas and 4 total refluxs, chooses reflux ratio 16:1, and tower top gets rid of lower boiling; collect middle runnings, filling silicon tetrachloride.
Embodiment 5
(1) in reactor, can raw material with diatomite, add metal catalyst, add liquid chlorine, adopt simultaneously and pass into nitrogen and drive air in reactor away, carry out chlorination reaction, temperature of reaction is 700 DEG C, reaction times 3h, and the speed that passes into of nitrogen is 0.1-0.2m/s;
(2) after reaction terminates; cooling; filter, filtrate is proceeded to rectifying tower, using rare gas element as protective atmosphere; heat up and control tower top temperature and bottom temperature; low temperature through 15h catches up with gas and 4 total refluxs, chooses reflux ratio 18:1, and tower top gets rid of lower boiling; collect middle runnings, filling silicon tetrachloride.
Claims (8)
1. a preparation method for silicon tetrachloride, is characterized in that, step is:
(1) in reactor, with diatomite meeting raw material, add metal catalyst, add liquid chlorine, adopt simultaneously and pass into nitrogen and drive air in reactor away, carry out chlorination reaction, temperature of reaction is 500-700 DEG C, reaction times 3-5h, the speed that passes into of nitrogen is 0.1-0.2m/s, and described metal catalyst is copper;
(2) after reaction terminates; cooling; filter, filtrate is proceeded to rectifying tower, using rare gas element as protective atmosphere; heat up and control tower top temperature and bottom temperature; low temperature through 8-15h catches up with gas and 4-6h total reflux, chooses reflux ratio 10:1-18:1, and tower top gets rid of lower boiling; collect middle runnings, filling silicon tetrachloride.
2. the preparation method of silicon tetrachloride according to claim 1, is characterized in that, in step (1), diatomaceous particle diameter is 10-200 order.
3. the preparation method of silicon tetrachloride according to claim 1, is characterized in that, the temperature of reaction in step (1) is 550-650 DEG C, reaction times 3.5-4.5h, and the speed that passes into of nitrogen is 0.15-0.18m/s.
4. the preparation method of silicon tetrachloride according to claim 1, is characterized in that, described in step (1), the purity of liquified chlorine gas is 99.99%.
5. the preparation method of silicon tetrachloride according to claim 1, is characterized in that, the rectifying tower described in step (2) is the tray column of quartzy material.
6. the preparation method of silicon tetrachloride according to claim 1, is characterized in that, the tower top temperature described in step (2) is 50-60 DEG C.
7. the preparation method of silicon tetrachloride according to claim 1, is characterized in that, the bottom temperature described in step (2) is 70-80 DEG C.
8. the preparation method of silicon tetrachloride according to claim 1, is characterized in that, the reflux ratio described in step (2) is 14:1-16:1.
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| CN201510601692.XA CN105236413A (en) | 2015-09-21 | 2015-09-21 | Silicon tetrachloride preparation method |
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| CN201510601692.XA CN105236413A (en) | 2015-09-21 | 2015-09-21 | Silicon tetrachloride preparation method |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61274749A (en) * | 1985-05-31 | 1986-12-04 | Mitsui Toatsu Chem Inc | Preparation of disproportionation catalyst |
| CN87105671A (en) * | 1986-08-20 | 1988-06-01 | 陶氏康宁公司 | A kind of method for preparing halosilanes |
| JP3821922B2 (en) * | 1996-09-03 | 2006-09-13 | 株式会社トクヤマ | Method for producing silicon tetrachloride |
| CN101472839A (en) * | 2006-05-09 | 2009-07-01 | 诺尔斯海德公司 | Method for producing silicon tetrachloride |
| US20110250116A1 (en) * | 2008-12-03 | 2011-10-13 | Patrick James Harder | Process for Producing Trichlorosilane and Tetrachlorosilane |
| CN103420382A (en) * | 2013-08-19 | 2013-12-04 | 浙江富士特集团有限公司 | Synthetic method and manufacturing system for silicon tetrachloride |
| CN104276575A (en) * | 2013-07-09 | 2015-01-14 | 四川瑞能硅材料有限公司 | Chlorination reaction apparatus for silicon tetrachloride, preparation system for silicon tetrachloride, and preparation method |
-
2015
- 2015-09-21 CN CN201510601692.XA patent/CN105236413A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61274749A (en) * | 1985-05-31 | 1986-12-04 | Mitsui Toatsu Chem Inc | Preparation of disproportionation catalyst |
| CN87105671A (en) * | 1986-08-20 | 1988-06-01 | 陶氏康宁公司 | A kind of method for preparing halosilanes |
| JP3821922B2 (en) * | 1996-09-03 | 2006-09-13 | 株式会社トクヤマ | Method for producing silicon tetrachloride |
| CN101472839A (en) * | 2006-05-09 | 2009-07-01 | 诺尔斯海德公司 | Method for producing silicon tetrachloride |
| US20110250116A1 (en) * | 2008-12-03 | 2011-10-13 | Patrick James Harder | Process for Producing Trichlorosilane and Tetrachlorosilane |
| CN104276575A (en) * | 2013-07-09 | 2015-01-14 | 四川瑞能硅材料有限公司 | Chlorination reaction apparatus for silicon tetrachloride, preparation system for silicon tetrachloride, and preparation method |
| CN103420382A (en) * | 2013-08-19 | 2013-12-04 | 浙江富士特集团有限公司 | Synthetic method and manufacturing system for silicon tetrachloride |
Non-Patent Citations (2)
| Title |
|---|
| 张若愚: "用硅藻土制取四氯化硅", 《云南化工》 * |
| 张香兰等: "利用煤系富硅质资源生产四氯化硅的可行性研究", 《煤炭加工与综合利用》 * |
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