Silane coupling agent Si-75 synthetic method for improving 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: 2016-07-27
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 a

Method used

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  • Silane coupling agent Si-75 synthetic method for improving yield
  • Silane coupling agent Si-75 synthetic method for improving yield
  • Silane coupling agent Si-75 synthetic method for improving yield

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0032] Example 1 A synthesis method of silane coupling agent Si-75 with improved yield

[0033] It includes the following steps:

[0034] Step one, prepare 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;

[0037] (2) The first stage reaction

[0038] Start the rotary switch of the drying reactor to operate, turn on the water ring vacuum pump, and when the vacuum in the dryer reaches 0.082Mpa and is stable, steam is introduced into the drying reactor jacket, and the steam pressure is adjusted to 0.2-0.3Mpa. When the temperature in the drying reactor reaches 50℃, adjust the opening of the steam valve appropriately;

[0039] (3) Second stage reaction

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

[0041] (4) The third stage reaction

[0042] After 1 hour, perform vacuum sw...

Example Embodiment

[0065] Example 2 A method for synthesizing silane coupling agent Si-75 with improved yield

[0066] Step one, prepare 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 operate, turn on the water ring vacuum pump, and when the vacuum in the dryer reaches 0.082Mpa and is stable, steam is introduced into the drying reactor jacket, and the steam pressure is adjusted to 0.2-0.3Mpa. When the temperature in the drying reactor reaches 50℃, adjust the opening of the steam valve appropriately;

[0071] (3) Second stage reaction

[0072] Control the temperature in the drying reactor to 65-70°C, start timing when the temperature in the drying reactor reaches 65°C, and react for 1 hour;

[0073] (4) The third stage reaction

[0074] One hour later, the vacuum switch is performed, fir...

Example Embodiment

[0097] Example 3 A synthesis method of silane coupling agent Si-75 with improved yield

[0098] It includes the following steps:

[0099] Step one, prepare 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;

[0102] (2) The first stage reaction

[0103] Start the rotary switch of the drying reactor to operate, turn on the water ring vacuum pump, and when the vacuum in the dryer reaches 0.082Mpa and is stable, steam is introduced into the drying reactor jacket, and the steam pressure is adjusted to 0.2-0.3Mpa. When the temperature in the drying reactor reaches 50℃, adjust the opening of the steam valve appropriately;

[0104] (3) Second stage reaction

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

[0106] (4) The third stage reaction

[0107] One hour later, the vacuum swit...

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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 tires in recent years. It is widely used in vulcanized rubber products. The coupling of fillers or fibers to the rubber matrix to improve the performance of the product. Its application can improve the physical and mechanical properties of rubber, such as tensile strength, tear resistance, wear resistance, bending and cracking resistance, etc., can be significantly improved, and 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 suitable for natural rubber, isoprene rubber, styrene-butadiene rubber, butadi...

Claims

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Application Information

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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
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