Amino/mercapto silane modified silica and preparation method thereof

A technology of mercaptosilane and silica, which is applied in the field of silica materials for the rubber industry, can solve the problems of reducing the surface reactivity of coupling agents and white carbon black powders, affecting the processing performance of rubber materials, etc., and achieving the reduction of hydrophilicity Sex, inhibition of agglomeration and secondary agglomeration, post-treatment pollution effect

Active Publication Date: 2013-03-13
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of this treatment method will reduce the reactivity of the coupling agent and the surface of the silica powder, and there will be unreacted silane coupling agent on the surface of the silica. Agglomeration will occur on the surface of silica and affect the processing performance of the rubber compound

Method used

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  • Amino/mercapto silane modified silica and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A. Weigh 21.3g Na 2 SiO 3 9H 2 O, dissolved in 50mL deionized water to prepare an aqueous solution with a concentration of 1.5M, heated to dissolve; 7.5g of concentrated sulfuric acid was slowly added to water, and diluted to a concentration of 5M sulfuric acid solution 15mL;

[0027] B. When the temperature of the sodium silicate solution reaches 25°C, start to add the sulfuric acid solution dropwise while stirring, and the sulfuric acid solution dropping rate is 0.1mL / min;

[0028] C. when the pH value of reaction solution was about 2, stop dripping sulfuric acid solution;

[0029] D. adjust the pH value to 7 with a concentration of ammonia solution of 7.5M;

[0030] E. After filtering and cleaning the material liquid obtained in step D, disperse the silica with ethanol, quickly add 0.75g γ-aminopropyltriethoxysilane, and then add 1.5g γ-mercaptopropyltriethoxy Silane;

[0031] F. After stirring and reacting for 1 hour at room temperature, remove ethanol by filtr...

Embodiment 2

[0033] A. Weigh 22.7g Na 2 SiO 3 9H 2 O, dissolved in 100mL deionized water to prepare an aqueous solution with a concentration of 0.8M, heated to dissolve; take 8g of concentrated sulfuric acid and slowly add it to water, and dilute to 80mL of a 1M sulfuric acid solution;

[0034] B. When the temperature of the sodium silicate solution reaches 30°C, start to drop the sulfuric acid solution while stirring, and the sulfuric acid solution dropping rate is 1.5mL / min;

[0035] C. when the pH value of reaction solution was about 2, stop dripping sulfuric acid solution;

[0036] D. adjust the pH value to 7 with a concentration of 5M ammonia solution;

[0037] E. After filtering and cleaning the material liquid obtained in step D, disperse silicon dioxide with ethanol, quickly add 0.4g N-β(aminoethyl)-γ-aminopropyltriethoxysilane, and then add 2.0 g2-mercaptoethyltriethoxysilane;

[0038] F. After stirring and reacting for 1 hour at room temperature, remove ethanol by filtration...

Embodiment 3

[0040] A. Weigh 28.4g Na 2 SiO 3 9H 2 O, dissolved in 100mL deionized water to prepare an aqueous solution with a concentration of 1.0M, heated to dissolve; take 10g of concentrated sulfuric acid and slowly add it to water, and dilute to 100mL of a sulfuric acid solution with a concentration of 0.5M;

[0041] B. When the temperature of the sodium silicate solution reaches 40°C, start to add the sulfuric acid solution dropwise while stirring, and the sulfuric acid solution dropping rate is 2.0mL / min;

[0042] C. when the pH value of reaction solution was about 2, stop dripping sulfuric acid solution;

[0043] D. adjust the pH value to 8 with a concentration of 10M ammonia solution;

[0044] E. After filtering and cleaning the material liquid obtained in step D, disperse the silica with deionized water, quickly add 1.5g γ-aminopropyltrimethoxysilane, and then add 0.6g γ-mercaptopropyltrimethoxy base silane;

[0045] F. After stirring and reacting for 1 hour at room temperatur...

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Abstract

The invention belongs to the field of silica materials for the rubber industry, and particularly relates to an amino / mercapto silane modified silica and a preparation method thereof. According to the invention, an in-situ synthesis method is adopted, so that aminosilane and mercapto silane coordinately modify the surface of silica; and in the process of modification, by using the autocatalysis action of aminosilane, the hydroxyl radical reaction of mercapto silane and the surface of silica is accelerated, so that the aminosilane and the mercapto silane are effectively wrapped on the surface of the silica, thereby improving the dispersion of the silica in rubber materials; and meanwhile, the reaction between silane coupling agents can be inhibited, thereby improving the processing performance of rubber materials.

Description

technical field [0001] The invention belongs to the field of silica materials for rubber industry, and in particular relates to an amino / mercaptosilane modified silica material and a preparation method thereof. Background technique [0002] In 1992, the French Michelin company used a large amount of white carbon black in the tread rubber of car tires to manufacture the first generation of energy-saving and environmentally friendly tires, which became "green tires". The rolling resistance of green tires is about 20% lower than that of ordinary tires, and it has the characteristics of low heat generation, good tear resistance and wet skid resistance. Since then, the application of silica as a rubber reinforcing material in high-performance tires has continuously achieved progress. However, due to the small particle size of silica, it is easy to fly and aggregate, and it is not easy to disperse in rubber, so the application of silica is limited. [0003] The dispersibility an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/28C09C3/12C08K9/10C08K9/06C08K3/36C08L7/00
Inventor 赵丽丽董栋蒋小强
Owner BEIJING RED AVENUE INNOVA
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