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Solvent method synthetic process of Si-75

A technology of propyltriethoxysilane and disulfide disulfide, which is applied in the field of solvent-based synthesis technology, can solve the problems of short product storage period, easy failure, reduced yield, serious pollution, etc., and achieves long storage period, easy operation, good color effect

Inactive Publication Date: 2015-07-29
NANCHANG GANYU ORGANOSILICONE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the generation of irritating gases such as sulfur hydrogen and sulfur oxides during the heating process, the pollution is serious, the operation is difficult, and the energy consumption is high.
Later, a phase-transfer catalytic aqueous phase method was used. This method is simpler to operate than the above method, but because the amount of sulfur powder in the reaction system decreases and the alkalinity increases, the raw material γ-chloropropyltriethoxysilane and the product are easily hydrolyzed, and the yield decreases. The product has a short storage period and is prone to failure, and because of the use of more expensive catalysts, a large amount of sewage containing catalysts needs to be treated, which is not conducive to environmental protection

Method used

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  • Solvent method synthetic process of Si-75

Examples

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Effect test

Embodiment 1

[0021] A kind of solvent method synthetic technique of bis-(Y-propyl triethoxysilane) disulfide, this technique comprises following process steps:

[0022] A. Put sodium sulfide containing 9 crystalline waters and sulfur powder in an equimolar ratio with it into a pond porcelain reactor equipped with a stirrer, reflux condenser, water separator and thermometer; (because sulfur meets iron to form black iron sulfide instead of iron reactors)

[0023] B. Add toluene with a weight ratio of 1.8 times that of sodium sulfide containing 9 crystal water, stir and heat to 80°C to start dehydration, and remove all the water to 110°C to clear the toluene;

[0024] C. Cool to below 50°C, add Y-chloropropyltriethoxysilane with a molar ratio of 2.03 times of sodium sulfide and anhydrous ethanol with an equal weight ratio of toluene, and then add ethylene glycol diethyl ether with 0.4 times the weight of toluene , heated to control the reaction temperature at 95-100°C, and reacted for four h...

Embodiment 2

[0030] 1. A solvent method synthesis process of bis-(γ-propyltriethoxysilane) disulfide, which comprises the following process steps:

[0031] A. Put sodium sulfide containing 9 crystalline waters and sulfur powder in an equimolar ratio with it into a pond porcelain reactor equipped with a stirrer, reflux condenser, water separator and thermometer; (because sulfur meets iron to form black iron sulfide and cannot use iron reactors).

[0032] B. Add toluene with a weight ratio of 1.6 times that of sodium sulfide containing 9 crystal water, stir and heat to 90°C to start reflux dehydration, and remove all the water to 110°C to clear the toluene;

[0033] C. Cool down to below 50°C, add γ-chloropropyltriethoxysilane with a molar ratio of 2.00 times that of sodium sulfide and absolute ethanol with an equal weight ratio to toluene, and then add ethylene glycol diethylene glycol with a weight ratio of 0.3 times that of toluene. Diethyl ether, heating and controlling the reaction te...

Embodiment 3

[0036] 1. A solvent method synthesis process of bis-(γ-propyltriethoxysilane) disulfide, which comprises the following process steps:

[0037] A. Put sodium sulfide containing 9 crystalline waters and sulfur powder in an equimolar ratio with it into a pond porcelain reactor equipped with a stirrer, reflux condenser, water separator and thermometer; (because sulfur meets iron to form black iron sulfide instead of iron reactors)

[0038] B. Add toluene whose weight ratio is 2 times that of sodium sulfide containing 9 crystalline waters, stir and heat to 110°C to start reflux dehydration, and to 110°C to remove all the toluene for clarification;

[0039]C. Cool down to below 50°C, add γ-chloropropyltriethoxysilane with a molar ratio of 2.06 times that of sodium sulfide and absolute ethanol with an equal weight ratio to toluene, and then add ethylene glycol diethylene glycol with a weight ratio of 0.6 times that of toluene. Diethyl ether, heated to control the reaction temperatu...

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Abstract

The invention relates to a solvent method synthetic process of Si-75. Si-75 can be used for radial tyres and other rubber products and belongs to the technical field of coupling agents. The solvent method synthetic process comprises the following steps: adding sodium sulfide containing nine crystal water and powdered sulfur into methylbenzene, heating, dewatering, cooling, adding gamma-chloropropyl triethoxysilane and absolute ethyl alcohol, then adding ethylene glycol diethyl ether, heating, after the reaction, cooling to the room temperature, filtering inorganic salt and impurities for industrial salt application, transferring filtrate to a distiller, distilling solvent and foreshot under reduced pressure for recycling, and performing distillation to obtain the Si-75 when the vacuum degree is greater than or equal to 0.090 Mpa and the temperature is greater than or equal to 150 DEG C, wherein the molar ratio of the sodium sulfide to the powdered sulfur is 1:1, the weight ratio of the methylbenzene to the sodium sulfide is 1.6-2, the weight ratio of the gamma-chloropropyl triethoxysilane to the sodium sulfide is 2.00-2.06, the weight ratio of the absolute ethyl alcohol to the absolute ethyl alcohol is 1:1, and the weight ratio of the ethylene glycol diethyl ether to the methylbenzene is 0.3-0.6.

Description

technical field [0001] The invention relates to a solvent method synthesis process of bis-(γ-propyltriethoxysilane) disulfide, which can be used in radial tires and other rubber products , belongs to the field of coupling agent technology. Background technique [0002] Bis-(γ-propyltriethoxysilane) disulfide business name: Silicon-75 (Si-75) is a multifunctional silane coupling agent successfully used in the rubber industry, its application makes the physical and The mechanical properties are improved, the tensile strength, tear strength, wear resistance, bending and cracking resistance can be significantly improved, and the permanent deformation can be reduced. Because it is easier to disperse evenly in rubber and plastics, it can also reduce the viscosity of the rubber and improve the processing performance. It is especially suitable for vulcanized rubber systems that use silicon compounds as reinforcing agents. Suitable fillers include carbon black, white carbon black, ...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 刘泓刘兵
Owner NANCHANG GANYU ORGANOSILICONE
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