CN101318971B - Method for reducing ethyl alcohol in sulphur-containing silicone hydride - Google Patents
Method for reducing ethyl alcohol in sulphur-containing silicone hydride Download PDFInfo
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- CN101318971B CN101318971B CN2008100198106A CN200810019810A CN101318971B CN 101318971 B CN101318971 B CN 101318971B CN 2008100198106 A CN2008100198106 A CN 2008100198106A CN 200810019810 A CN200810019810 A CN 200810019810A CN 101318971 B CN101318971 B CN 101318971B
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- ethanol
- alcohol
- sulfuric silane
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- sulphur
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Abstract
The invention relates to a method for reducing ethanol in sulphur-containing silane. The method comprises the following steps that: (1) the sulphur-containing silane and C5-C8 alcohol are thrown into a reactor according to a proportion of 1 to between 6 and 7.2; simultaneously, a titanium ester as a catalyst is added into the reactor; (2) materials in the reactor are heated till ethanol flows outand kept between 90 and 120 DEG C for 1 to 10 hours; when the effluent quantity of the ethanol reaches over 80 percent of the theoretical quantity, the reaction is finished; (3) under vacuum with a pressure of more than 0.09MPa below zero, residual ethanol and unreacted C5-C8 alcohol in reactants are evaporated out at a temperature of between 100 and 120 DEG C till no distillate flows out; and (4) the reactants are cooled to a temperature of between 20 DEG C below zero and 30 DEG C and filtered. The method has simple process, easy implementation, safety and environmental protection.
Description
Technical field
The present invention relates to a kind of minimizing sulfuric silane alcoholic acid method, thereby can in rubber mixing process, reduce the ethanol volatile matter.
Background technology
Sulfuric silane is one of requisite auxiliary agent of production environmental protection tire, is widely used in the sulfur vulcanized rubber goods.But owing in the sulfuric silane molecule 6 ethanol groups are arranged usually; in rubber mixing process, the filler in the sulfuric silane molecule in ethanol group and the rubber (as: white carbon black) reacts, and forms silicon-oxygen-silicon bound; ethanol is released, and brings harm for safety, labour hygiene and environment protection.
Summary of the invention
The technical problem to be solved in the present invention is exactly existing sulfuric silane existing alcoholic acid volatilization problem in rubber mixing process, and alcoholic acid method in a kind of minimizing sulfuric silane is provided.
For technical problem is stated in solution, the present invention adopts following technical scheme:
In the presence of catalyzer, pass through oxyethyl group in the sulfuric silane and C
5-C
8Transesterify takes place in alcohol, is contained the sulfuric silane compound of ethanol group hardly, specifically comprises the steps:
1) with sulfuric silane and C
5-C
8Alcohol is in 1: the ratio of 6-7.2 drops in the reactor, adds titanate catalyst simultaneously;
2) with in the reactor material be warming up to after ethanol flows out, 90 ℃-120 ℃ insulations 1-10 hour down, reach 80% when above of theoretical amount, reaction end when ethanol flows out;
3) with reactant under-vacuum more than the 0.09MPa, 100 ℃-120 ℃ steam residual ethanol and unreacted C
5-C
8Alcohol is not till have cut to flow out;
4) reactant being cooled to-20 ℃-30 ℃ filters down.
Titanate catalyst in the step 1) is positive titanium isopropylate or positive metatitanic acid four esters, and its weight consumption is sulfuric silane and C
5-C
8The 100-10000ppm of the total amount of alcohol.
C in the step 1)
5-C
8The preferred 2-Ethyl Hexanol of alcohol, amylalcohol or hexanol.
Chemical equation involved in the present invention is as follows:
(EtO)
3Si-Alk-S
x-Alk-Si (EtO)
3(sulfuric silane)+6HO-C
8H
17(C
5-C
8Alcohol)+catalyzer → reaction generation monomer or polymer organic silane compound, wherein:
The Et-ethyl;
Alk-is the divalence hydrocarbon of 3 carbon atoms;
The present invention is except that the ethanol of removing final residual and unreacted raw material need to carry out under-vacuum more than the 0.09MPa, and the remaining reaction process is carried out under normal pressure.
The present invention has following advantage
1, technology letter of the present invention is easy to implement;
2, the product by the present invention preparation has higher flash-point, and the content of ethanol group is less than 10% after measured for product, and rudimentary alcohol radical reduction reaches more than 90% in the product, in use discharges ethanol hardly;
3, help health of operators and environment protection;
4, improved the security of rubber mixing-milling technique.
Embodiment
Embodiment 1
In the there-necked flask of being furnished with agitator, thermometer and distiller condenser, add 538 gram (1 mole) two (triethoxy propyl group) tetrasulfides, add 858 gram (6.6 moles) 2-Ethyl Hexanols, under agitation add the positive titanium isopropylate of 5 grams, heat up, when reaching 90 ℃, temperature of reaction have ethanol to flow out, slowly be warming up to 90 ℃-120 ℃ and be incubated 3 hours down, under-0.1MPa vacuum, distill, when temperature of charge when not having material to flow out for 120 ℃, stop distillation, cold filtration, product are yellow liquid, yield 95.6%.
Embodiment 2
In the there-necked flask of being furnished with agitator, thermometer and distiller condenser, add 474 gram (1 mole) two (triethoxy propyl group) disulphide, add 858 gram (6.6 moles) 2-Ethyl Hexanols, under agitation add 5 gram tetrabutyl titanates, heat up, when reaching 90 ℃, temperature of reaction have ethanol to flow out, slowly be warming up to 115 ℃-120 ℃ and be incubated 5 hours down, under-0.1MPa vacuum, distill, when temperature of charge when not having material to flow out for 120 ℃, stop distillation, cold filtration, product are yellow liquid, yield 96.3%.
Embodiment 3
In the there-necked flask of being furnished with agitator, thermometer and distiller condenser, add 538 gram (1 mole) two (triethoxy propyl group) tetrasulfides, add 528 gram (6 moles) amylalcohols, under agitation add 5 gram tetrabutyl titanates, heat up, when reaching 90 ℃, temperature of reaction have ethanol to flow out, slowly be warming up to 115 ℃-120 ℃ and be incubated 5 hours down, under-0.1MPa vacuum, distill, when temperature of charge when not having material to flow out for 120 ℃, stop distillation, cold filtration, product is a yellow liquid, yield 94.5%.
Embodiment 4
In the there-necked flask of being furnished with agitator, thermometer and distiller condenser, add 474 gram (1 mole) two (triethoxy propyl group) disulphide, add 712 gram (7.2 moles) hexanols, under agitation add the positive titanium isopropylate of 5 grams, heat up, when reaching 90 ℃, temperature of reaction have ethanol to flow out, slowly be warming up to 115 ℃-120 ℃ and be incubated 10 hours down, under-0.1MPa vacuum, distill, when temperature of charge when not having material to flow out for 120 ℃, stop distillation, cold filtration, product are yellow liquid, yield 97.5%.
Claims (4)
1. one kind is reduced alcoholic acid method in the sulfuric silane, it is characterized in that comprising the steps:
1) with sulfuric silane and C
5-C
8Alcohol is in 1: the ratio of 6-7.2 drops in the reactor, adds titanate catalyst simultaneously;
2) material in the reactor has been warming up to after ethanol flows out, 90 ℃-120 ℃ following insulation reaction 1-10 hour, reach 80% when above of theoretical amount, reaction end when ethanol flows out;
3) with reactant under-vacuum more than the 0.09MPa, 100 ℃-120 ℃ steam residual ethanol and unreacted C
5-C
8Alcohol is not till have cut to flow out;
4) reactant being cooled to-20 ℃-30 ℃ filters down.
2. reduce alcoholic acid method in the sulfuric silane according to claim 1, it is characterized in that the titanate catalyst in the step 1) is positive titanium isopropylate, its weight consumption is sulfuric silane and C
5-C
8The 100-10000ppm of the total amount of alcohol.
3. reduce alcoholic acid method in the sulfuric silane according to claim 1, it is characterized in that the by product ethanol in the reaction process is steamed at any time.
4. reduce alcoholic acid method in the sulfuric silane according to claim 1, it is characterized in that C
5-C
8Alcohol is selected from 2-Ethylhexyl Alcohol, amylalcohol or hexanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100198106A CN101318971B (en) | 2008-03-17 | 2008-03-17 | Method for reducing ethyl alcohol in sulphur-containing silicone hydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100198106A CN101318971B (en) | 2008-03-17 | 2008-03-17 | Method for reducing ethyl alcohol in sulphur-containing silicone hydride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101318971A CN101318971A (en) | 2008-12-10 |
| CN101318971B true CN101318971B (en) | 2010-12-15 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100198106A Active CN101318971B (en) | 2008-03-17 | 2008-03-17 | Method for reducing ethyl alcohol in sulphur-containing silicone hydride |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108997409A (en) * | 2018-08-28 | 2018-12-14 | 山东省宁津县浩润科技有限公司 | A method of reducing ethyl alcohol in polysulfide silanes coupling agent |
| CN109762014B (en) * | 2019-03-05 | 2021-03-26 | 湖北江瀚新材料股份有限公司 | Preparation method of solid sulfur-containing silane |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273975A (en) * | 1998-06-10 | 2000-11-22 | 德古萨－于尔斯股份公司 | Novel low plymer organosilylane polysulphideane and its use in rubber and moulded products |
-
2008
- 2008-03-17 CN CN2008100198106A patent/CN101318971B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273975A (en) * | 1998-06-10 | 2000-11-22 | 德古萨－于尔斯股份公司 | Novel low plymer organosilylane polysulphideane and its use in rubber and moulded products |
Non-Patent Citations (1)
| Title |
|---|
| J.W. ten Brinke,et al.Mechanistic aspects of the role of coupling agents in silica-rubber composites.《Composites Science and Technology》.2003,第63卷1165-1174. * |
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| Publication number | Publication date |
|---|---|
| CN101318971A (en) | 2008-12-10 |
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