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A kind of synthetic method of silane coupling agent si-75 that improves yield

A technology of silane coupling agent and synthesis method, which is applied in the field of silane coupling agent, can solve the problems of short storage time of finished products, low product purity, low conversion rate of raw materials and low yield of products, etc., so as to improve the conversion rate of raw materials and improve the quality of products. Purity, the effect of improving product yield

Active Publication Date: 2018-08-14
威海市和谐硅业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The conversion rate of raw materials and product yield are low, and the product purity is lower than 97%;
[0006] (2) The quality of the product is poor: high chlorine content and impurity content; low total sulfur content;
[0007] (3) The stability of the finished product is poor, and the storage time of the finished product is short;
[0008] (4) Long response time

Method used

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  • A kind of synthetic method of silane coupling agent si-75 that improves yield
  • A kind of synthetic method of silane coupling agent si-75 that improves yield
  • A kind of synthetic method of silane coupling agent si-75 that improves yield

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Effect test

Embodiment 1

[0032] Embodiment 1 A kind of synthetic method of silane coupling agent Si-75 improving yield

[0033] Include the following steps:

[0034] Step 1. Preparation of Sodium Disulfide

[0035] (1) Add raw materials

[0036] Add 100Kg of low-iron sodium sulfide and 20.8Kg of elemental sulfur to the double-cone drying reactor after metering;

[0037] (2) The first stage reaction

[0038] Start the rotary switch of the drying reactor to make it run, turn on the water ring vacuum pump, when the vacuum degree in the dryer reaches 0.082Mpa and is stable, inject steam into the jacket of the drying reactor to adjust the steam pressure to 0.2-0.3Mpa. When the temperature in the drying reactor reaches 50 °C, the opening of the steam valve is properly adjusted;

[0039] (3) The second stage reaction

[0040] Control the temperature in the drying reactor to be 60-65 °C, start timing when the temperature in the drying reactor reaches 60 °C, and react for 1 hour;

[0041] (4) The third s...

Embodiment 2

[0065] Embodiment 2 A kind of synthetic method of silane coupling agent Si-75 improving yield

[0066] Step 1. Preparation of Sodium Disulfide

[0067] (1) Add raw materials

[0068] Add 101.5Kg of low-iron sodium sulfide and 21.2Kg of elemental sulfur to the double-cone drying reactor after metering;

[0069] (2) The first stage reaction

[0070] Start the rotary switch of the drying reactor to make it run, turn on the water ring vacuum pump, when the vacuum degree in the dryer reaches 0.082Mpa and is stable, inject steam into the jacket of the drying reactor to adjust the steam pressure to 0.2-0.3Mpa. When the temperature in the drying reactor reaches 50 °C, the opening of the steam valve is properly adjusted;

[0071] (3) The second stage reaction

[0072] The temperature in the drying reactor is controlled to be 65-70 °C, and the time is started when the temperature in the drying reactor reaches 65 °C, and the reaction is performed for 1 hour;

[0073] (4) The third s...

Embodiment 3

[0097] Embodiment 3 A kind of synthetic method of silane coupling agent Si-75 improving yield

[0098] Include the following steps:

[0099] Step 1. Preparation of Sodium Disulfide

[0100] (1) Add raw materials

[0101] Add 108.8Kg of low-iron sodium sulfide and 22Kg of elemental sulfur to the double-cone drying reactor after metering;

[0102] (2) The first stage reaction

[0103] Start the rotary switch of the drying reactor to make it run, turn on the water ring vacuum pump, when the vacuum degree in the dryer reaches 0.082Mpa and is stable, inject steam into the jacket of the drying reactor to adjust the steam pressure to 0.2-0.3Mpa. When the temperature in the drying reactor reaches 50 °C, the opening of the steam valve is properly adjusted;

[0104] (3) The second stage reaction

[0105] Control the temperature in the drying reactor to be 60-65 °C, start timing when the temperature in the drying reactor reaches 60 °C, and react for 1 hour;

[0106] (4) The third s...

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Abstract

The invention provides a silane coupling agent Si-75 synthetic method for improving the yield.The method comprises the steps of preparation of sodium disulfide and preparation of a silane coupling agent Si-75.In the process of preparation of the silane coupling agent Si-75, gamma-chloropropyltriethoxysilane and sodium sulfide containing low iron with the weight ratio being 100:(31.25-37.5) are added.According to the prepared product, the yield is 97.11-97.73%, the raw material conversion rate is 98.62-98.94%, and the product purity is 99.23-99.36%.The prepared product is good in quality, and is the faint yellow transparent liquid from the appearance; the density (20 DEG C) is 1.032-1.043 g / cm<3>, the flash point is larger than or equal to 105-106.5 DEG C, the chlorine content is smaller than or equal to 0.12-0.29%, the impurity content is smaller than or equal to 0.19-0.42%, and the total sulphur content reaches 14.5-15.2%.

Description

technical field [0001] The invention relates to a method for synthesizing a silane coupling agent Si-75 with improved yield, and belongs to the technical field of silane coupling agents. Background technique [0002] Bis-[propyltriethoxysilane]-disulfide (Si-75 for short) is an important additive for the rapid development of green tire production in recent years. It is widely used in vulcanized rubber system products. Coupling of fillers or fibers with rubber matrix to improve product performance. Its application improves the physical and mechanical properties of rubber, the tensile strength, tear strength, wear resistance, and resistance to bending and cracking can be significantly improved, and the permanent deformation can be reduced. Because it is easier to disperse uniformly in rubber and plastic, it can also reduce the viscosity of the rubber compound and improve the processing performance. It is suitable for natural rubber, isoprene rubber, styrene-butadiene rubber, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C08K5/548
CPCC07F7/1804C08K5/548
Inventor 郭祥荣郭学阳王璀庄青杨荣华张秀玲
Owner 威海市和谐硅业有限公司