CN101906111B - Method for preparing methyl silicic acid and industrial hydrochloric acid by using hydrolysis of methyl trichlorosilane - Google Patents
Method for preparing methyl silicic acid and industrial hydrochloric acid by using hydrolysis of methyl trichlorosilane Download PDFInfo
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- CN101906111B CN101906111B CN2010102520229A CN201010252022A CN101906111B CN 101906111 B CN101906111 B CN 101906111B CN 2010102520229 A CN2010102520229 A CN 2010102520229A CN 201010252022 A CN201010252022 A CN 201010252022A CN 101906111 B CN101906111 B CN 101906111B
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- hydrochloric acid
- methyl
- acid
- hydrogen chloride
- trichloro silane
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Abstract
The invention discloses a method for preparing methyl silicic acid and industrial hydrochloric acid by using hydrolysis of methyl trichlorosilane, which comprises the following steps of: adding 10 to 13 parts of 14 to 16 percent diluted hydrochloric acid into a reaction kettle, stirring the diluted hydrochloric acid, dripping 1 part of methyl trichlorosilane into the kettle to obtain solid methyl silicic acid and hydrochloric acid liquid, and separating the solid methyl silicic acid and the hydrochloric acid liquid; and dripping the methyl trichlorosilane into the hydrochloric acid for two times by adopting the same method, and controlling the reaction temperature during dripping. The methyl silicic acid prepared by the method has small granules, and the cleaned granules are not easy to contain acid; and because the ratio of the pre-added diluted hydrochloric acid to the methyl trichlorosilane is high, the reaction temperature can be controlled to be low, the production efficiency is greatly improved, the hydrochloric acid byproduct is changed into the industrial hydrochloric acid with high concentration, the emission is greatly reduced, extremely low emission can fully meet the national related standards, the environment is improved, and the social benefit and the economic benefit are very high.
Description
Technical field
The present invention relates to a kind of method of utilizing the METHYL TRICHLORO SILANE hydrolysis to prepare methyl siliconic acid and technical hydrochloric acid.
Technical background
METHYL TRICHLORO SILANE is one of several kinds of principal monomers in monomer production, being produced of an organosilane monomer manufacturing enterprise, accounts for about 12% of monomer total amount in the production, and the ultimate production of current domestic METHYL TRICHLORO SILANE is about ten thousand tons of 8-10.Because the present domestic still a little very old product lines of rear portion product that can utilize the METHYL TRICHLORO SILANE preparation; Like silicone resin, silane coupling agent, methyl siliconic acid or the like; The market demand of these products is all little, wherein the more still methyl siliconic acid of usefulness at home.Various reasons causes METHYL TRICHLORO SILANE, and seriously drug on the market; Add that it belongs to very not easily-storied hazardous chemical again; Make methyl three silane with regard under the present domestic situation, it has become an organosilane monomer manufacturing enterprise to produce the sub product of a kind of special headache of dimethyldichlorosilane(DMCS).Its price 10000 yuan/ton during also from a high position fall to the processing costs of subsidizing 1000 yuan/ton of down-stream enterprises at present under one the tunnel.The simple and easy method of handling METHYL TRICHLORO SILANE in fact is exactly that hydrolysis prepares methyl siliconic acid; But domestic traditional technology is too simple at present; Because of a large amount of in treating processes, producing---METHYL TRICHLORO SILANE per ton produces the Hydrogen chloride of 3-4 ton concentration about 18%; Not only environment is made a big impact, and produced a difficult problem how to handle Hydrogen chloride again.
Summary of the invention
The object of the invention just provides a kind of good in economic efficiency, and the METHYL TRICHLORO SILANE hydrolysis that utilizes that can reduce environmental pollution prepares the method for methyl siliconic acid and technical hydrochloric acid.
The method of utilizing the METHYL TRICHLORO SILANE hydrolysis to prepare methyl siliconic acid and technical hydrochloric acid of the present invention may further comprise the steps:
1, in reaction kettle, adds the Hydrogen chloride of 10-13 part, concentration 14-16% earlier, start stirring, in still, drip 1 part METHYL TRICHLORO SILANE again; Because METHYL TRICHLORO SILANE and water reaction are violent; Control reaction temperature is below 50 ℃ during dropping, and reaction makes methyl siliconic acid and Hydrogen chloride, and the concentration of hydrochloric acid can reach about 21%; Use ordinary method with solid methyl siliconic acid and hydrochloric acid liquid separation, hydrochloric acid is subsequent use;
2, the Hydrogen chloride 10-13 part that above-mentioned steps is produced adds in another reaction kettle; Start stirring, in still, drip 1 part METHYL TRICHLORO SILANE, control reaction temperature is below 42 ℃ during dropping; Reaction makes methyl siliconic acid and Hydrogen chloride; It is about 26% that the concentration of hydrochloric acid can reach, and uses ordinary method with solid methyl siliconic acid and hydrochloric acid liquid separation, and hydrochloric acid is subsequent use;
3, the Hydrogen chloride 10-13 part that obtains in the step 2 is added in another reaction kettle; Start stirring; In still, drip 1 part METHYL TRICHLORO SILANE, control reaction temperature is below 38 ℃ during dropping, and reaction makes methyl siliconic acid and hydrochloric acid; It is about 31% that the concentration of hydrochloric acid can reach, and uses ordinary method with solid methyl siliconic acid and hydrochloric acid liquid separation.
This present invention's the reaction formula that utilizes the METHYL TRICHLORO SILANE hydrolysis to prepare methyl siliconic acid and technical hydrochloric acid is:
CH
3SiCl
3+3H
2O＝CH
3Si(OH)
3+3HCl
The method of utilizing the METHYL TRICHLORO SILANE hydrolysis to prepare methyl siliconic acid and technical hydrochloric acid of the present invention; Because adding earlier is Hydrogen chloride, so speed of response is just unhappy at the beginning the time, thereby it is also unhappy to heat up during reaction; The methyl siliconic acid particle that obtains is little, cleans in the particle and is not easy to contain acid; Owing to add Hydrogen chloride and the big 10-13 of METHYL TRICHLORO SILANE ratio in advance: 1; So can control temperature of reaction lowlyer, production efficiency is significantly improved, and by-product hydrochloric acid have become the high technical hydrochloric acid of concentration; Significantly reduced discharging; The minute quantity discharging also can meet relevant national standard fully, has improved environment, and social benefit and economic benefit are all very high.
Embodiment
A kind of method of utilizing the METHYL TRICHLORO SILANE hydrolysis to prepare methyl siliconic acid and technical hydrochloric acid may further comprise the steps:
1, the Hydrogen chloride of elder generation's 500 kilograms of addings, concentration 16% in reaction kettle is opened and is stirred, and in still, drips 40 kilograms METHYL TRICHLORO SILANE again; Control reaction temperature is below 50 ℃ during dropping; 22-25 minute dropping time, reaction makes 25.15 kilograms of methyl siliconic acids and 29.3 kilograms in Hydrogen chloride, and it is 20.8% that the concentration that detects hydrochloric acid reaches; Use ordinary method with solid methyl siliconic acid and hydrochloric acid liquid separation, hydrochloric acid is subsequent use;
2, above-mentioned Hydrogen chloride 12 weight parts are added in another reaction kettle, start stirring, in still, drip the METHYL TRICHLORO SILANE of 1 weight part; Control reaction temperature is below 42 ℃ during dropping; 28-30 minute dropping time, reaction makes methyl siliconic acid and Hydrogen chloride, the concentration of hydrochloric acid about 26%; Use ordinary method with solid methyl siliconic acid and hydrochloric acid liquid separation, hydrochloric acid is subsequent use;
3, the Hydrogen chloride that obtains in the step 2 10 weight parts are added in another reaction kettle; Start stirring, in still, drip the METHYL TRICHLORO SILANE of 1 weight part, control reaction temperature is below 38 ℃ during dropping; 32-35 minute dropping time; Reaction makes methyl siliconic acid and hydrochloric acid, and the concentration of hydrochloric acid is 31.3%, uses ordinary method with solid methyl siliconic acid and hydrochloric acid liquid separation.
Claims (1)
1. method of utilizing the METHYL TRICHLORO SILANE hydrolysis to prepare methyl siliconic acid and technical hydrochloric acid, it is characterized in that: it may further comprise the steps:
(1), the Hydrogen chloride that in reaction kettle, adds 10-13 part, concentration 14-16% earlier; Start stirring; In still, drip 1 part METHYL TRICHLORO SILANE again, control reaction temperature is below 50 ℃ during dropping, and reaction makes methyl siliconic acid and Hydrogen chloride; Use ordinary method with solid methyl siliconic acid and hydrochloric acid liquid separation, hydrochloric acid is subsequent use;
(2), the Hydrogen chloride 10-13 part that obtains in the above-mentioned steps (1) is added in another reaction kettle; Start stirring; In still, drip 1 part METHYL TRICHLORO SILANE, control reaction temperature is below 42 ℃ during dropping, and reaction makes methyl siliconic acid and Hydrogen chloride; Use ordinary method with solid methyl siliconic acid and hydrochloric acid liquid separation, hydrochloric acid is subsequent use;
(3), the Hydrogen chloride 10-13 part that obtains in the step (2) is added in another reaction kettle; Start stirring; In still, drip 1 part METHYL TRICHLORO SILANE, control reaction temperature is below 38 ℃ during dropping, and reaction makes methyl siliconic acid and hydrochloric acid; The concentration of hydrochloric acid reaches 31%, uses ordinary method with solid methyl siliconic acid and hydrochloric acid liquid separation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102520229A CN101906111B (en) | 2010-08-12 | 2010-08-12 | Method for preparing methyl silicic acid and industrial hydrochloric acid by using hydrolysis of methyl trichlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102520229A CN101906111B (en) | 2010-08-12 | 2010-08-12 | Method for preparing methyl silicic acid and industrial hydrochloric acid by using hydrolysis of methyl trichlorosilane |
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| Publication Number | Publication Date |
|---|---|
| CN101906111A CN101906111A (en) | 2010-12-08 |
| CN101906111B true CN101906111B (en) | 2012-11-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010102520229A Expired - Fee Related CN101906111B (en) | 2010-08-12 | 2010-08-12 | Method for preparing methyl silicic acid and industrial hydrochloric acid by using hydrolysis of methyl trichlorosilane |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104356159A (en) * | 2014-11-25 | 2015-02-18 | 廊坊师范学院 | Method for preparing silsesquioxane by virtue of hydrolysis of methyl trichlorosilane |
| CN109575221A (en) * | 2018-12-04 | 2019-04-05 | 镇江利德尔复合材料有限公司 | A kind of polyurethane shape memory material and preparation method thereof strengthened based on organosilicon polymer |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1218809A (en) * | 1998-11-03 | 1999-06-09 | 化学工业部星火化工厂 | Process for preparing sodium methyl-silicate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS638389A (en) * | 1986-06-27 | 1988-01-14 | Lion Corp | Production of silicon compound |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1218809A (en) * | 1998-11-03 | 1999-06-09 | 化学工业部星火化工厂 | Process for preparing sodium methyl-silicate |
Non-Patent Citations (4)
| Title |
|---|
| JP昭63-8389A 1988.01.14 |
| Takako Kudo et.al..Exploring the Mechanism for the Synthesis of Silsesquioxanes.3.The Effect of Substituents and Water.《J.Phys.Chem.A.》.2002,第106卷 * |
| 吴盛全.甲基三氯硅烷的综合利用.《有机硅材料》.2000,第14卷(第1期), * |
| 王大喜 等.甲基三氯硅烷水解反应机理的密度泛函研究.《分子科学学报》.2009,第25卷(第2期), * |
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