CN1056881A - The preparation technology of r-chloropropyl trichloro-silane - Google Patents
The preparation technology of r-chloropropyl trichloro-silane Download PDFInfo
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- CN1056881A CN1056881A CN 90105667 CN90105667A CN1056881A CN 1056881 A CN1056881 A CN 1056881A CN 90105667 CN90105667 CN 90105667 CN 90105667 A CN90105667 A CN 90105667A CN 1056881 A CN1056881 A CN 1056881A
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- silane
- reaction
- rhodium
- chloropropyl trichloro
- preparation technology
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Abstract
The present invention is the preparation technology of silicone couplet and silicone couplet intermediate r-chloropropyl trichloro-silane.This technology is to be raw material with trichlorosilane and propenyl chloride, with compounds such as platinum, rhodium, palladium or complex compound as catalyzer, with thiodiphenylamine, pentanoic, phenylenediamine etc. as promotor, one-step synthesis r-chloropropyl trichloro-silane.Compared with prior art, the present invention can reduce byproduct of reaction, and reaction yield is reached more than 70%.Simultaneously, the present invention can make the platinum, rhodium, palladium compound or the complex compound catalyst that use in the reaction be reduced to the 1/2-1/10 of usage quantity in the prior art.
Description
The r-chloropropyl trichloro-silane has following array structure (I):
Compound is a silicone couplet, external trade(brand)name A-143, and can be widely used in rubber, plastics, synthetic resins or the like the macromolecular material by (I) further synthetic a series of silicone couplet.
Compound (I) is a raw material by trichlorosilane (II) and propenyl chloride (III), under catalyst action, prepares through addition reaction.Catalyzer generally uses metallic compound or metal complexs such as platinum, palladium, rhodium, and other adds small amount of amine compounds such as thiodiphenylamine, diphenylamine, phenylenediamine etc. as promotor.United States Patent (USP) (U, S 3925434), Japanese Patent (JaPan 7524927), Deutsches Wirtschafts Patent (Ger East 117021), Czech patents (Czech CS 196917) adopt platinum, palladium compound or complex compound to make catalyzer respectively, Deutsches Wirtschafts Patent (Ger East 103903) is made catalyzer with rhodium complex, all with thiodiphenylamine, diphenylamine, phenylenediamine etc. as promotor, with (II) and (III) is raw material, preparation r-chloropropyl trichloro-silane.Though the catalyzer structure difference that above patent is used is precious metal chemical complexs such as platinum, rhodium, palladium, addition is about 1/100000～1/10 of reactant gross weight, and catalyzer has accounted for bigger ratio in production cost.React more owing to paying in the reaction in addition, make productive rate on the low side, be generally 60～65% of theoretical amount.
The present invention seeks to compound (II) and (III) is raw material, becomes complex compound to make catalyzer with compounds such as platinum, rhodium, palladiums, makes promotor with thiodiphenylamine, pentanoic, phenylenediamine etc., synthetic preparation r-chloropropyl trichloro-silane.Adopt recovery set with catalyzer, promotor method in the reaction, make that catalyst levels reduces in the entire reaction course, productive rate is higher simultaneously.
Purpose of the present invention can reach by following measure: the recovery set vinasse of compounds such as containing platinum, rhodium, palladium or complex compound catalyst, make catalyst consumption reduce, the cover consumption of vinasse is 1/10 of a vinasse total amount～all, apply mechanically number of times and do not limit.
Purpose of the present invention can also reach by following measure: because main by product is SiCl in the reaction
4(IV) and CH
3CH
2CH
2SiCl
3(V) therefore, adds an amount of distillation foreshot (mainly being made up of compound III, IV, V) in reaction mass, can suppress to pay reaction during reaction, reduces by product, improves yield.The cover consumption of distillation foreshot is 1/10 of a collecting amount～all, apply mechanically number of times and do not limit.
The present invention compared with prior art has following advantage:
Adopt the present invention to produce the r-chloropropyl trichloro-silane, need not to change or increase equipment, can make the addition of catalyzer only be 1/2～1/10 of prior art, simultaneously reaction yield is reached more than 70%, reduced production cost.
Example one
In the reactor that agitator, thermometer, frozen water refrigerative reflux condensing tube and dropping funnel are housed, add 332g(4.35mol) propenyl chloride, 3ml 1%(weight/volume) Platinic chloride-ethylene glycol dimethyl ether solution, be heated to 42 ℃.Add 571g(content 95% in the dropping funnel, 4mol) trichlorosilane is added dropwise to 30g in the reactor earlier, 42 ℃ of reactions 10 minutes, adds the 100mg thiodiphenylamine, and after 2 minutes, a thermopositive reaction begins to take place.The control reacting liquid temperature continues to drip trichlorosilane at 45～45 ℃, dropwises in about 1 hour.Reaction solution is warming up to 60 ℃, stirring reaction 20 minutes.
180～186 ℃ of fractions are collected in distillation, get colorless liquid product 534g, yield: 63%.
Example two
With example together in the reactor of sampling device, add example one gained vinasse 5g, distillation foreshot 200g, the 1%(weight/volume) Platinic chloride monoethylene glycol dme solution 0.4ml, 332g(4.35mol) propenyl chloride, the 30g trichlorosilane, reacting by heating liquid to 42 ℃ reacts after 10 minutes, add the 100mg thiodiphenylamine, after 2 minutes, a thermopositive reaction begins to take place, and the control reaction solution is at 40～45 ℃, in 1 hour, be added dropwise to trichlorosilane 541g(again and add 95% trichlorosilane 571g altogether, 4mol), reaction solution is warming up to 60 ℃, continued stirring reaction 20 minutes.
180～186 ℃ of fractions are collected in distillation, get colorless liquid product 594g, yield: 70%.
Claims (3)
1, a kind of is raw material with trichlorosilane and propenyl chloride, with platinum, rhodium, palladium compound or complex compound as catalyzer, with thiodiphenylamine, pentanoic, phenylenediamine as promotor, the preparation technology of one-step synthesis r-chloropropyl trichloro-silane, it is characterized in that the recovery set reaction distillation raffinate of the catalyzer that contains platinum, rhodium, palladium compound or complex compound, it is the reaction distillation foreshot of silicon tetrachloride, propyltrichlorosilan that recovery set has been used major ingredient.
2, the preparation technology of r-chloropropyl trichloro-silane according to claim 1 is characterized in that recovery set with the reaction distillation raffinate of catalyzer that contains platinum, rhodium, palladium compound or complex compound, and the cover consumption is 1/10 of a raffinate～all, apply mechanically number of times and do not limit.
3, the preparation technology of r-chloropropyl trichloro-silane according to claim 1, it is characterized in that the recovery set major ingredient is the reaction distillation front-end volatiles of silicon tetrachloride, propyltrichlorosilan, the cover consumption is applied mechanically number of times and is not limit for 1/10～all of the distillation foreshot.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90105667 CN1056881A (en) | 1990-05-28 | 1990-05-28 | The preparation technology of r-chloropropyl trichloro-silane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90105667 CN1056881A (en) | 1990-05-28 | 1990-05-28 | The preparation technology of r-chloropropyl trichloro-silane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1056881A true CN1056881A (en) | 1991-12-11 |
Family
ID=4879475
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90105667 Pending CN1056881A (en) | 1990-05-28 | 1990-05-28 | The preparation technology of r-chloropropyl trichloro-silane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1056881A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040538C (en) * | 1994-11-21 | 1998-11-04 | 中国科学院化学研究所 | Method for preparation of 3-chloropropyl trichloro-silane |
| CN103408579A (en) * | 2013-09-03 | 2013-11-27 | 浙江华亿工程设计有限公司 | Synthesis method of gamma-chloropropyltrichlorosilane |
-
1990
- 1990-05-28 CN CN 90105667 patent/CN1056881A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040538C (en) * | 1994-11-21 | 1998-11-04 | 中国科学院化学研究所 | Method for preparation of 3-chloropropyl trichloro-silane |
| CN103408579A (en) * | 2013-09-03 | 2013-11-27 | 浙江华亿工程设计有限公司 | Synthesis method of gamma-chloropropyltrichlorosilane |
| CN103408579B (en) * | 2013-09-03 | 2016-06-08 | 浙江华亿工程设计有限公司 | The synthetic method of a kind of ��-chloropropyl trichloro-silane |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |