Preparation method of sulfur-containing silane coupling agent

A technology of sulfur silane coupling agent and chloropropyl triethoxysilane, which is applied in the field of preparation of sulfur-containing silane coupling agent, can solve the problem of high heating loss of Si69 or Si75, increased color of Si69 or Si75, tri-n-butylene High toxicity of amines and other problems, to achieve the effect of reducing the activation energy of the reaction, the reaction rate is fast, and the corrosiveness

Inactive Publication Date: 2021-10-01
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above synthesis process, tri-n-butylamine will be introduced into Si69 or Si75. Tri-n-butylamine has high toxicity, and there are certain safety hazards in the use process; in addition, it will cause the heating loss of Si69 or Si75 to be too high; The color of Si69 or Si75 is aggravated, affecting the appearance of the product

Method used

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Examples

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preparation example Construction

[0034] The application provides a preparation method of sulfur-containing silane coupling agent Si69, comprising the following steps in sequence:

[0035] 1.1) preparing disodium tetrasulfide solution;

[0036] 1.2) The disodium tetrasulfide solution prepared in step 1.1), the crown ether phase transfer catalyst and γ-chloropropyltriethoxysilane undergo a chemical reaction, and an intermediate liquid A is obtained after the reaction is completed;

[0037] 1.3) The intermediate liquid A prepared in step 1.2) is sequentially subjected to liquid separation, activated carbon decolorization, and distillation to obtain the sulfur-containing silane coupling agent Si69.

[0038] In one embodiment of the present application, step 1.1) is specifically: a chemical reaction occurs after the aqueous solution of sodium hydroxide is mixed with sulfur powder to form a disodium tetrasulfide solution.

[0039] In one embodiment of the present application, the reaction temperature for the chemi...

Embodiment 1

[0056] A preparation method of sulfur-containing silane coupling agent Si69, comprising the following steps carried out in sequence:

[0057] 1.1) Add a total of 70g of aqueous solution containing 32.62g of sodium hydroxide to a 500mL flask, add 44.3g of sulfur powder, control the reaction temperature to 90°C, and the reaction time to 1h;

[0058] 1.2) Then add 1.5g of 18-crown-6, and then add 137.5g of intermediate γ-chloropropyltriethoxysilane (γ2), control the reaction temperature at 70°C, and react for 1.5h under stirring. After the reaction is completed, intermediate Liquid A;

[0059] 1.3) The intermediate liquid A obtained in the step 1.2) was subjected to liquid separation, activated carbon decolorization, and distillation in sequence to obtain 149.5 g of light yellow Si69 transparent liquid after completion.

[0060] In Example 1, the calculated yield with γ2 is 98.68%, the total sulfur content in the sulfur-containing silane coupling agent Si69 is 22.78wt%, and the ...

Embodiment 2

[0062] A preparation method of sulfur-containing silane coupling agent Si69, comprising the following steps carried out in sequence:

[0063] 1.1) In a 500mL flask, add 60g of aqueous solution containing 28.54g of sodium hydroxide in total, add 38.8g of sulfur powder, control the reaction temperature to 90°C, and the reaction time to 1h;

[0064] 1.2) Then add 1.5g of 15-crown-5, then add 120.3g of intermediate γ-chloropropyltriethoxysilane (γ2), control the reaction temperature at 70°C, and react for 1.5h under stirring. After the reaction is completed, intermediate Liquid A;

[0065] 1.3) The intermediate liquid A prepared in the step 1.2) is sequentially subjected to liquid separation, activated carbon decolorization, and distillation to obtain 133 g of light yellow Si69 transparent liquid after completion.

[0066] In Example 2, the calculated yield with γ2 is 98.81%, the total sulfur content in the sulfur-containing silane coupling agent Si69 is 22.75wt%, and the chlorin...

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Abstract

The invention provides a preparation method of a sulfur-containing silane coupling agent, and particularly relates to a preparation method of sulfur-containing silane coupling agents Si69 and Si75. The method comprises the following steps: carrying out chemical reaction on a sodium polysulfide solution, a crown ether phase transfer catalyst and gamma-chloropropyltriethoxysilane to generate the sulfur-containing silane coupling agent; wherein the crown ether type phase transfer catalyst is 18-crown-6 or 15-crown-5. The crown ether phase transfer catalyst is adopted, so that the reaction rate is increased, and the reaction temperature is reduced; the product does not contain tri-n-butylamine, so that potential safety hazards in the use process are avoided; the problem that the heating decrement of the product is too high is solved; the problem that the color of the product is gradually increased along with the prolonging of the storage time of the product is solved; generated wastewater does not contain ammonia nitrogen, so that the pollution to the environment is small; the product yield is greater than or equal to 98%, the impurity content is less than or equal to 2.0 wt%, the heating loss is less than or equal to 1.0%, and the chromaticity is still 6 after the product is stored for 6 months.

Description

technical field [0001] The invention relates to the technical field of preparation of silane coupling agents, in particular to a preparation method of sulfur-containing silane coupling agents. Background technique [0002] Silica is used as a reinforcing filler. The rubber compound reinforced with silica has higher strength and tear performance, better wet skid resistance, and lower rolling resistance. Silica is an indispensable reinforcement for green tires. filler. Due to the presence of a large amount of silicon hydroxyl groups on the surface of silica, silica is easy to agglomerate in non-polar rubber (such as NR, styrene-butadiene rubber and butadiene rubber), resulting in increased viscosity of the rubber compound, poor processing performance, and white A large number of silanol groups on the surface of carbon black are acidic and hygroscopic, which affect the vulcanization rate and crosslinking density of the compound. In order to improve the dispersion of silica in...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07F7/18C07F7/20C01B17/20C01B17/34B01J31/02
CPCC07F7/1804C07F7/1892C07F7/20C01B17/20C01B17/34B01J31/0204
Inventor马德龙王文博潘琳琳王庆振吴彩英陈云刚刘建元张新
OwnerSHANDONG YANGGU HUATAI CHEM