CN104804031A - Method for preparing chloromethyl chlorosilane through light chlorination process - Google Patents
Method for preparing chloromethyl chlorosilane through light chlorination process Download PDFInfo
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- CN104804031A CN104804031A CN201510160422.XA CN201510160422A CN104804031A CN 104804031 A CN104804031 A CN 104804031A CN 201510160422 A CN201510160422 A CN 201510160422A CN 104804031 A CN104804031 A CN 104804031A
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- chlorosilane
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Abstract
The invention relates to a method for preparing chloromethyl chlorosilane through light chlorination process. In the method, the chloromethyl chlorosilane is produced through the reaction of chlorine and methyl chlorosilane under the reaction condition of illumination. The method has good economic property, and the reaction condition is easy to control.
Description
Technical field
The present invention relates to a kind of production method of heavy chemicals, especially a kind of light chlorination process prepares the method for chloromethyl chlorosilane.
Background technology
In the production of polysilicon, containing impurity such as part monomethyl dichlorosilane, dimethyldichlorosilane(DMCS)s in raw material trichlorosilane, these impurity enter in reduction furnace, can be reduced by hydrogen, form with carbon-containing impurities on polycrystalline silicon rod deposits, thus have impact on the quality product of polysilicon.In order to ensure the quality of polysilicon product in reduction furnace in prior art, this kind of impurity in raw material must be removed, generally adopt rectification and purification method to the removal of this impurity in existing production technique, after being proposed by the impurity of methyl chlorosilane class, because this kind of material of methyl chlorosilane range of application is little, purity is wayward, general is all that this type of impurity is carried out drip washing process, need to use liquid caustic soda, considerably increase production cost, also can cause certain pollution to environment.After being extracted by methyl chlorosilane, generally processing obtains chloromethyl chlorosilane again, sells, add value-added content of product as the derived product in production of polysilicon.Methyl chlorosilane is made chloromethyl chlorosilane and generally have thermal chlorination and sulfuryl chloride chlorination process.Thermal chlorination mainly adopts gas phase chlorination, select chlorine as chlorizating agent, methyl chlorosilane is passed in reactor, be heated to 300-400 DEG C, pass into certain proportion chlorine to react, reaction products therefrom is chloromethyl chlorosilane and unreacted methyl chlorosilane, obtains target substance chloromethyl chlorosilane after carrying out purification rectifying.This kind of method by-products content is low, but transformation efficiency only can reach about 70%, and complex process equipment, processing condition are wayward, are not suitable for widely applying and producing.Sulfuryl chloride chlorination process adopts during low temperature has the Diisopropyl azodicarboxylate of larger capacity of decomposition, as radical initiator, methyl chlorosilane at the boiling point with Cl
2there is substitution reaction in SO, thus produces chloromethyl chlorosilane, and the reaction of this method is simple, workable, but compare employing chlorine as reagent, high cost.
Summary of the invention
The object of the invention is to solve in prior art prepare exist in chloromethyl chlorosilane method high cost, complex process equipment, not easily mass-produced problem, provide a kind of good economy performance, method that light chlorination process that reaction conditions is easy to control prepares chloromethyl chlorosilane.
For realizing above object, technical solution of the present invention is: a kind of light chlorination process prepares the method for chloromethyl chlorosilane, comprises the following steps:
1) passed into by chlorine in the container being loaded with methyl chlorosilane liquid, chlorine and methyl chlorosilane are reacted, and the weight ratio of chlorine and methyl chlorosilane is between 3:12500 to 8:12500;
2) step 1 chlorine pass into react with methyl chlorosilane in container time, set up at container the illumination that light source carries out 1.5-3 hour outward;
3) close light source, purification & isolation is carried out to the product obtained in container, obtains chloromethyl chlorosilane.
The material of the container in described step 1) is corresponding with employing light source, and the energy transmissive that light source is produced enters in container.
Described step 2) in the ultra-violet lamp of light source to be wavelength be 365nm, 0.44kw irradiate.
Compared with prior art, beneficial effect of the present invention is:
The chlorination that employing light chlorination process carries out methyl chlorosilane is very effective, chlorination transformation efficiency can reach more than 50%-98%, and the condition that reaction is carried out is easy to control, and can not introduce new impurity, effectively plant-scale production can be carried out in comparatively economic mode.
Embodiment
The present invention is further detailed explanation below:
Light chlorination process prepares a method for chloromethyl chlorosilane, comprises the following steps:
1) passed into by chlorine in the container being loaded with methyl chlorosilane liquid, chlorine and methyl chlorosilane are reacted, and the weight ratio of chlorine and methyl chlorosilane is between 3:12500 to 8:12500;
2) step 1 chlorine pass into react with methyl chlorosilane in container time, set up at container the illumination that light source carries out 1.5-3 hour outward;
3) close light source, purification & isolation is carried out to the product obtained in container, obtains chloromethyl chlorosilane.
The material of the container in described step 1) is corresponding with employing light source, and the energy transmissive that light source is produced enters in container.
Described step 2) in the ultra-violet lamp of light source to be wavelength be 365nm, 0.44kw irradiate.
Below in conjunction with embodiment, the present invention is described in detail.
Case study on implementation 1:
Thick methyl chlorosilane raw material (main content 95%) 200KG is pressed in reaction vessel, chlorine 20L is passed in reaction vessel, due under mark condition, the density of chlorine is 3.17g/L, now the weight ratio of chlorine and methyl chlorosilane is 4:12500, illumination 2 hours under ultra-violet lamp, optimal wavelength is that the ultra-violet lamp of 365nm, 0.44kw irradiates, and the material of container adopts this UV-light transmissive to enter.Close light source, stop illumination.Carry out proximate analysis to product extraction, the main content of chloromethyl chlorosilane is 85%, and after entering next step purification & isolation, the main content of chloromethyl chlorosilane can reach more than 98%, meets need of production completely.
Case study on implementation 2:
Thick methyl chlorosilane raw material (main content 95%) 200 kilograms is pressed in reaction vessel, chlorine 30L is passed in reaction vessel, due under mark condition, the density of chlorine is 3.17g/L, now the weight ratio of chlorine and methyl chlorosilane is 6:12500, illumination 2 hours 30 points under ultra-violet lamp, optimal wavelength is that the ultra-violet lamp of 365nm, 0.44kw irradiates, and the material of container adopts this UV-light transmissive to enter.Close light source, stop illumination.Carry out proximate analysis to product extraction, the main content of chloromethyl chlorosilane is 90%, and after entering next step purification & isolation, the main content of chloromethyl chlorosilane can reach more than 98%, meets need of production completely.
The chlorination that employing light chlorination process carries out methyl chlorosilane is very effective, chlorination transformation efficiency can reach more than 50%-98%, and the condition that reaction is carried out is easy to control, and can not introduce new impurity, effectively plant-scale production can be carried out in comparatively economic mode.Good economy performance of the present invention, reaction conditions are easy to control.
Claims (3)
1. light chlorination process prepares a method for chloromethyl chlorosilane, comprises the following steps:
1) passed into by chlorine in the container being loaded with methyl chlorosilane liquid, chlorine and methyl chlorosilane are reacted, and the weight ratio of chlorine and methyl chlorosilane is between 3:12500 to 8:12500;
2) step 1 chlorine pass into react with methyl chlorosilane in container time, set up at container the illumination that light source carries out 1.5-3 hour outward;
3) close light source, purification & isolation is carried out to the product obtained in container, obtains chloromethyl chlorosilane.
2. a kind of light chlorination process according to claim 1 prepares the method for chloromethyl chlorosilane, it is characterized in that: the material of the container in described step 1) is corresponding with employing light source, and the energy transmissive that light source is produced enters in container.
3. a kind of light chlorination process according to claim 1 prepares the method for chloromethyl chlorosilane, it is characterized in that: described step 2) in the ultra-violet lamp of light source to be wavelength be 365nm, 0.44kw irradiate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510160422.XA CN104804031A (en) | 2015-04-08 | 2015-04-08 | Method for preparing chloromethyl chlorosilane through light chlorination process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510160422.XA CN104804031A (en) | 2015-04-08 | 2015-04-08 | Method for preparing chloromethyl chlorosilane through light chlorination process |
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| CN104804031A true CN104804031A (en) | 2015-07-29 |
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| CN201510160422.XA Pending CN104804031A (en) | 2015-04-08 | 2015-04-08 | Method for preparing chloromethyl chlorosilane through light chlorination process |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4101397A (en) * | 1976-04-02 | 1978-07-18 | Dynamit Nobel Aktiengesellschaft | Process for the preparation of alpha-chloromethylsilanes |
| CN1317488A (en) * | 2001-03-16 | 2001-10-17 | 中国科学院上海有机化学研究所 | Process and equipment for preparing chloromethyl chlorosilane by gas-phase chlorination |
| CN1962669A (en) * | 2006-11-21 | 2007-05-16 | 上海试四赫维化工有限公司 | Process for preparing chloromethylmethyldichlorsilane |
-
2015
- 2015-04-08 CN CN201510160422.XA patent/CN104804031A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4101397A (en) * | 1976-04-02 | 1978-07-18 | Dynamit Nobel Aktiengesellschaft | Process for the preparation of alpha-chloromethylsilanes |
| CN1317488A (en) * | 2001-03-16 | 2001-10-17 | 中国科学院上海有机化学研究所 | Process and equipment for preparing chloromethyl chlorosilane by gas-phase chlorination |
| CN1962669A (en) * | 2006-11-21 | 2007-05-16 | 上海试四赫维化工有限公司 | Process for preparing chloromethylmethyldichlorsilane |
Non-Patent Citations (2)
| Title |
|---|
| 王明成等，: "光氯化法合成ClCH2SiCl3的研究", 《化工科技》 * |
| 袁法祥等，: "甲基三氯硅烷的氯化方法", 《化工科技》 * |
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Application publication date: 20150729 |