CN1537858A - Method of producing triethyl methyl silicate using remnant of silane coupling agent - Google Patents
Method of producing triethyl methyl silicate using remnant of silane coupling agent Download PDFInfo
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- CN1537858A CN1537858A CNA2003101049356A CN200310104935A CN1537858A CN 1537858 A CN1537858 A CN 1537858A CN A2003101049356 A CNA2003101049356 A CN A2003101049356A CN 200310104935 A CN200310104935 A CN 200310104935A CN 1537858 A CN1537858 A CN 1537858A
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- ethanol
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- methyl silicate
- coupling agent
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Abstract
A process for preparing the triethyl methylsilicate from the leftover of silane coupling agent SCA602 includes such steps as adding alcohol, mixing for the reaction between alcohol and trichloromethyl silane in the leftover to obtain triethyl methylsilicate and hydrogen chloride, adding solvent, heating for removing chloropropene and hydrogen chloride, filtering and decoloring.
Description
Technical Field
The invention belongs to a production method of an acyclic compound, and particularly relates to a method for producing triethyl methyl silicate by using an addition front fraction produced in the production of a coupling agent of SCA602(LK959) and 3- (2-aminoethyl) aminopropyl methyl dimethoxy silane.
Background
At present, the addition front fraction generated in the production of the SCA602 silane coupling agent is dumped as an industrial waste. The component of the silane coupling agent is methyl trichlorosilane which is taken as the main component, and also contains methyl dichlorosilane, chloropropene and other silane substances. Belongs to a strong acid substance. Because the waste materials cannot be comprehensively utilized and poured, the environment is seriously polluted, and a plurality of available substances cannot be utilized to cause waste. At present, the same method as the method is not applied to production practice.
Disclosure of Invention
The invention aims to provide a method for producing triethyl methyl silicate by utilizing leftovers of a silane coupling agent, which can prevent environmental pollution and comprehensively utilize wastes to create economic benefits.
The purpose of the invention is realized by the following technical scheme. The process comprises four steps of mixing reaction, impurity removal, dehydrogenation and filtering decoloration.
First, mixed reaction
The addition front cut fraction generated by producing the SCA602 silane coupling agent is used as a raw material, and the production is directly carried out without any treatment. The mixing reaction is carried out in a mixing reactor and a reaction kettle.
Technical formula
Addition front fraction 1
0.5-0.8% of industrial ethanol
The raw materials are put into a reaction kettle through a mixing reactor according to a certain proportion, and the methyl trichlorosilane and the methyl dichlorosilane in the addition front fraction react with ethanol to generate triethyl methyl silicate and methyl diethoxy silane.
Secondly, removing impurities
The removal of impurities means the removal of chloropropene-based low-boiling substances and hydrogen chloride produced by the reaction from the addition front fraction. The solvent carrying heating removal method is adopted. The solvent can be ethanol, diethyl ether, cyclohexane, etc. Namely, the solvent is added firstly, and then the temperature is reduced and increased. And (4) evaporating the solvent, wherein the boiling point of the chloropropene impurities is low, the chloropropene impurities and the hydrogen chloride are evaporated along with the solvent, and after the evaporated solvent is cooled and recovered, the chloropropene impurities and the hydrogen chloride escape as gas and are absorbed by water or are discharged along with tail gas.
Thirdly, dehydrogenation treatment
Dehydrogenation is a process of dehydrogenating methyldiethoxysilane generated by the above-mentioned mixing reaction to form triethyl methylsilicate. Dehydrogenation is carried out in a dehydrogenation tank, and a catalyst is added for dehydrogenation treatment.
Fourthly, filtering and decoloring
And (3) filtering the colored material subjected to mixing reaction, impurity removal and dehydrogenation treatment, and removing the color to obtain the finished triethyl methyl silicate.
The invention has the advantages of simple process and easy implementation, and the addition front distillate is a strong acid substance which seriously pollutes the environment, and is dumped as waste to seriously pollute the environment and cause waste. The method makes use of waste, the produced triethyl methyl silicate is a chemical product with high price, and the byproduct hydrochloric acid is a product with large demand. Not only protects the environment, but also increases the economic benefit.
Drawings
The attached drawing is a process flow chart of the invention
1-addition front fraction tank 2-ethanol tank 3-ethanol recovery tank 4-mixing reactor 5-reaction kettle 6-filter tank
Detailed Description
First, mixed reaction
100 kg of the raw material of the addition front fraction is added into an addition front fraction tank (1), and recovered ethanol and ethanol are added into a recovered ethanol tank (3) and an ethanol tank (2). The total weight of ethanol in the two tanks is 60 kg, preferably 30 kg per tank. After the feeding is finished, the discharge valves of the three tanks are opened simultaneously, and the materials are introduced into the mixing reactor (4) by speed counting. And then enters the reaction kettle (5) through an overflow port. The reaction time is controlled to be 90 minutes, and the temperature is required to be between normal temperature and 80 ℃. To generate triethyl methyl silicate, methyl diethoxy silane and hydrogen chloride.
The reaction formula is as follows:
secondly, removing impurities
The impurity removal is carried out after all the distillate and the ethanol enter the reaction kettle for reaction. Removing chloropropene low-boiling-point impurities in the reacted material and hydrogen chloride generated in the reaction. Is a method for removing by heating carried by ethanol. The method comprises the steps of closing a feed valve, opening a vacuum pump, controlling the vacuum degree from a valve of a hydrogen chloride discharge pipe, introducing steam into an interlayer of the reaction kettle when the vacuum degree in the reaction kettle reaches below-0.08 Mpa, and controlling the temperature in the reaction kettle to rise to 80 ℃. When the temperature reaches 80 ℃, the steam valve and the vacuum pump are closed, and the reaction is recovered to normal pressure. At this time, 20 kg of ethanol was added to the reaction vessel through the mixing reactor via the feed pipe. Then, the pressure is reduced and the temperature is raised again, when the vacuum degree reaches below-0.08 Mpa and the temperature is raised to 80 ℃, a steam valve and a vacuum pump are closed, and the reaction is recovered to the normal pressure. Then adding 20 kg of ethanol into the feeding pipe, closing the feeding valve, reducing the pressure and raising the temperature again, and closing the steam valve and the vacuum pump when the vacuum degree reaches-0.08 Mpa again and the temperature is 80 ℃ so as to restore the reaction to normal pressure. The chloropropene low-boiling point impurities in the front fraction of the addition are carried away along with the distillation of the solvent. The hydrogen chloride content is reduced to below 0.05%. Removing impurities, or heating to 130 deg.C under normal pressure, and distilling off solvent to remove impurities.
Thirdly, dehydrogenation treatment
Dehydrogenation is to generate triethyl methyl silicate and methyl diethoxy silane after the mixing reaction, and dehydrogenation is to perform dehydrogenation treatment on the methyl diethoxy silane to generate the triethyl methyl silicate. The method comprises the steps of adding 10-20 kg of absolute ethyl alcohol into each 100 kg of materials after reaction, and then adding 100 g of catalyst. The catalyst can be zinc acetate or ethanolamine. Then placing the mixture in a dehydrogenation tank for standing for more than 24 hours, introducing the mixture into a distillation kettle after the hydrogen content is determined to be qualified, and distilling off the redundant ethanol. During the standing, hydrogen in a silicon-hydrogen bond in the methyldiethoxysilane is replaced by ethoxy in ethanol to generate triethyl methylsilicate and hydrogen, and the triethyl methylsilicate and the hydrogen escape from the opening of the tank.
The reaction formula is as follows:
fourthly, filtering and decoloring
And (3) filtering and decoloring the colored material subjected to mixing reaction, impurity removal and dehydrogenation treatment by an activated carbon layer (80-120 meshes). And removing the color of the material. Thus obtaining the finished product of triethyl methyl silicate.
The technical indexes of the triethyl methyl silicate produced by the method are as follows:
relative density: 0.95 to 1.00
SiO2The content is as follows: 30 to 34 percent
Acidity degree: less than or equal to 0.05 percent
Viscosity: less than or equal to 1.6
Low fraction: less than or equal to 2 percent
Claims (4)
1. The process of producing triethyl methyl silicate with leftover of silane coupling agent includes four steps of mixing reaction, eliminating impurity, dehydrogenation treatment and filtering decolorizing, and features that the distillate of SCA602 (or LK959) and 3- (2-aminoethyl) aminopropyl methyl dimethoxysilane as material is used directly in producing triethyl methyl silicate.
2. The method according to claim 1, wherein the mixing reaction is carried out in such a manner that the weight ratio of the ingredients is equal to 1: 0.5-0.8 of ethanol in the distillate ratio before addition.
3. The process of claim 1, wherein the removal of impurities is carried out by reacting the pre-addition fraction with ethanol at a weight ratio of 5: 1 in a solvent with a boiling point of less than 110 ℃, such as ethanol, diethyl ether, cyclohexane, etc., in a reaction vessel, and heating under reduced pressure to remove the solvent and impurities, wherein the vacuum degree is below-0.08 MPa and the temperature is 80 ℃, and the process can be repeated until the content of hydrogen chloride in the product is less than 0.05%, or heating at normal pressure to 130 ℃ to remove the solvent.
4. The method according to claim 1, wherein the weight ratio of the ethanol as the dehydrogenation feed to the catalyst is 1: 0.1 to 0.2: 0.001, and the treatment time is 20 to 70 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310104935 CN1274696C (en) | 2003-10-24 | 2003-10-24 | Method of producing triethyl methyl silicate using remnant of silane coupling agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310104935 CN1274696C (en) | 2003-10-24 | 2003-10-24 | Method of producing triethyl methyl silicate using remnant of silane coupling agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1537858A true CN1537858A (en) | 2004-10-20 |
| CN1274696C CN1274696C (en) | 2006-09-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310104935 Expired - Fee Related CN1274696C (en) | 2003-10-24 | 2003-10-24 | Method of producing triethyl methyl silicate using remnant of silane coupling agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079754A (en) * | 2010-12-27 | 2011-06-01 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation process of methyltriethoxysilane |
| CN102634028A (en) * | 2012-04-08 | 2012-08-15 | 荆州市江汉精细化工有限公司 | Method for preparing modified tetraethoxysilane by use of waste in production of 3-chloropropyltrichlorosilane |
-
2003
- 2003-10-24 CN CN 200310104935 patent/CN1274696C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079754A (en) * | 2010-12-27 | 2011-06-01 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation process of methyltriethoxysilane |
| CN102079754B (en) * | 2010-12-27 | 2012-10-17 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation process of methyltriethoxysilane |
| CN102634028A (en) * | 2012-04-08 | 2012-08-15 | 荆州市江汉精细化工有限公司 | Method for preparing modified tetraethoxysilane by use of waste in production of 3-chloropropyltrichlorosilane |
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| Publication number | Publication date |
|---|---|
| CN1274696C (en) | 2006-09-13 |
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Granted publication date: 20060913 Termination date: 20091124 |