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A kind of surface sulfur-containing silane modified silica microsphere and its synthesis method

A technology of silica and synthesis method, applied in the direction of dyeing organosilicon compound treatment, fibrous filler, etc., can solve the problems of affecting rubber properties, waste, leaving pores, etc., to reduce carbon emissions, rational synthesis method, and reduce pores. rate effect

Active Publication Date: 2015-10-28
江西晨光新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these silane coupling agents commonly used at present are very active at high temperatures, and it is easy to generate free radicals, causing a part of the rubber to vulcanize and polymerize in advance, resulting in waste
In addition, these silane coupling agents contain siloxyl groups, and when used, they will release small molecule alcohols with low boiling points, such as methanol and ethanol. performance, and small alcohol molecules directly discharged into the atmosphere are not conducive to environmental protection

Method used

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  • A kind of surface sulfur-containing silane modified silica microsphere and its synthesis method
  • A kind of surface sulfur-containing silane modified silica microsphere and its synthesis method
  • A kind of surface sulfur-containing silane modified silica microsphere and its synthesis method

Examples

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Effect test

Embodiment 1

[0032] 1. Preparation of silica microspheres with surface modified by mercaptopropylsilane

[0033] In a 2000mL three-neck flask equipped with mechanical stirring, reflux condenser and constant pressure dropping funnel, add 100g of 2 / g silica microspheres, add 1000g ethanol, add 1mL concentrated hydrochloric acid, adjust the pH value of the system to around 2, start mechanical stirring, dissolve 1g (4.2mmol) 3-mercaptopropyltriethoxysilane in 5mL In the water ethanol, slowly drop it through the constant pressure dropping funnel. After the dropwise addition, turn on the heating to reflux. After reacting for 5 hours, the gas chromatography detects that the 3-mercaptopropyltriethoxysilane has basically reacted, stop Heating, cooling to room temperature, filtering, washing the solid several times with absolute ethanol, checking the pH value of the washed ethanol, when the washed ethanol is neutral, collecting the solid product, and vacuum drying at 60°C for 6 hours to obta...

Embodiment 2

[0037] 1. Preparation of silica microspheres with surface modified by mercaptopropylsilane

[0038] In a 2000mL three-neck flask equipped with mechanical stirring, reflux condenser and constant pressure dropping funnel, add 300g of 2 / g of silica microspheres, add 1000g of methanol, add 3g of strong acidic cation exchange resin, start mechanical stirring, slowly drop 30g (0.153mol) of 3-mercaptopropyltrimethoxysilane through the constant pressure dropping funnel, After the dropwise addition, turn on and heat to reflux. After 5 hours of reaction, gas chromatography detects that the 3-mercaptopropyltriethoxysilane has basically reacted. Stop heating, cool down to room temperature, filter, and wash the solid with anhydrous methanol for 3 The second time, the solid was collected, and after vacuum drying at 60°C for 6 hours, the resin and silica microspheres were separated with a sieve with a pore size of about 0.3 mm to obtain 299.5 g of a white solid product of silica micr...

Embodiment 3

[0042] 1. Preparation of silica microspheres with surface modified by mercaptopropylsilane

[0043] In a 2000mL three-neck flask equipped with mechanical stirring, reflux condenser and constant pressure dropping funnel, add 200g of 2 / g of silica microspheres, add 1000g n-hexane, add 0.5mL sulfuric acid, the pH of the system is about 1, start mechanical stirring, dissolve 10g (42mmol) 3-mercaptopropyltriethoxysilane in 50mL n-hexane Slowly drop it through the constant pressure dropping funnel, after the drop is completed, turn on the heating to reflux, after reacting for 5 hours, take a sample of the n-hexane layer solution, and detect the 3-mercaptopropyltriethoxysilane in it by gas chromatography After the reaction was completed, the heating was stopped, the temperature was lowered to room temperature, filtered, the solid was washed several times with n-hexane, and the solid product was collected. After vacuum drying at 60° C. for 6 hours, 194.0 g of a white solid pro...

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Abstract

The invention discloses a silicon dioxide pellet with a sulfur silane modified surface and a synthesis method of the pellet, wherein a black ball in the structure represents a silicon dioxide pellet the surface of which is modified by sulfur silane of the structure. R is long-chain alkyl and comprises heptyl, amyl, nonyl and hendecyl, and the range of the ratio n / m of n to m is 0.01 to 1. The surface of the silicon dioxide pellet is mainly modified by the sulfur silane, so that the silicon dioxide pellet can be directly used as a rubber filler, and does not need an additional silane coupling agent, and meanwhile, the processed silicon dioxide pellet does not discharge volatile micromolecules again when being used as the rubber filler, so that the rubber performance can be improved, and the silicon dioxide pellet is more environmental friendly.

Description

technical field [0001] The invention relates to a silicon dioxide microsphere modified with sulfur-containing silane on the surface and a synthesis method thereof. Background technique [0002] Silica microspheres commonly used in industry are often used as reinforcing fillers for rubber and resin, commonly known as "white carbon black", which can greatly improve the mechanical properties of materials such as rubber and resin. When used for rubber reinforcement, since the bonding force between silica itself and rubber is not high, silane coupling agents are usually added to improve the bonding force between rubber and silica, and further improve the performance of rubber. In the field of rubber for automobile tires, with the introduction of the concept of "green tires", the amount of silica is also increasing year by year, and the application of silane coupling agents in the preparation of rubber for automobile tires has also attracted more and more attention. At presen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09C1/28C09C3/12
Inventor 丁建峰梁秋鸿葛利伟周煜华
Owner 江西晨光新材料股份有限公司
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