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Method for preparing polysulfide silane coupling agent by passage reaction device

A technology of channel reaction device and silane coupling agent, which is applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., and can solve problems such as unsafety, long reaction cycle, and blockage

Active Publication Date: 2016-06-22
南京曙光新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004]Technical problem: the purpose of this invention is to provide a kind of utilization channel reaction device to prepare polysulfide silane coupling agent for industrial large-scale production polysulfide silane coupling agent The method uses sodium polysulfide and 3-chloropropyltriethoxysilane to prepare polysulfide silane coupling agent by using a channel reaction device under solvent conditions, which solves the problem of long reaction cycle, unsafety, and poor stability of large-scale reaction equipment. problem, addressing possible clogging with channel reaction devices

Method used

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  • Method for preparing polysulfide silane coupling agent by passage reaction device
  • Method for preparing polysulfide silane coupling agent by passage reaction device
  • Method for preparing polysulfide silane coupling agent by passage reaction device

Examples

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Embodiment 1

[0050] Example 1 Preparation of Si17.

[0051] The mass ratio of raw material caustic soda (solid sodium hydroxide), sulfur powder, solvent water, phase transfer catalyst tetrabutylammonium bromide, and 3-chloropropyltriethoxysilane is 120:150:330:4:480 .

[0052] Dissolve tetrabutylammonium bromide in water to form a catalyst solution, the mass ratio of the two is 1:6, and the temperature is controlled at 10°C-50°C; the caustic soda, sulfur powder and the remaining water are mixed at 50°C-80°C Prepare sodium polysulfide aqueous solution under reaction; Mix sodium polysulfide aqueous solution and catalyst solution and keep the temperature at 50°C-70°C, enter the channel reaction device from a feed port of the channel reaction device, and simultaneously 3-chloropropyltri The ethoxysilane is fed into the channel reaction device to mix and react with the sodium polysulfide aqueous solution, and the reaction temperature is controlled at 84-86°C. Sampling is taken from the coll...

Embodiment 2

[0053] Example 2 Prepare a polysulfide silane coupling agent with an average value of n of 2.20~2.50, corresponding to the product Si75 in GB / T30309-2013.

[0054] The mass ratio of raw material sodium sulfide pentahydrate, sulfur powder, solvent water, phase transfer catalyst tetrabutylammonium bromide, pH regulator sodium bicarbonate, 3-chloropropyltriethoxysilane is 175:45:280: 4:60:478.

[0055] Dissolve tetrabutylammonium bromide in water to form a catalyst solution, the mass ratio of the two is 1:6, and the temperature is controlled at 10°C-50°C; sodium sulfide pentahydrate, sulfur powder, sodium bicarbonate and the remaining water are mixed in Prepare sodium polysulfide aqueous solution by reacting at 50°C-80°C; mix sodium polysulfide aqueous solution and catalyst solution and keep the temperature at 50°C-70°C, enter the channel reaction device from a feed port of the channel reaction device, and simultaneously put 3-Chloropropyltriethoxysilane is passed into the cha...

Embodiment 3

[0056] Example 3 Prepare a polysulfide silane coupling agent with an average value of n of 2.05~2.25, corresponding to the product Si85 in GB / T30309-2013.

[0057] The mass ratio of raw materials sodium sulfide pentahydrate, sulfur powder, solvent water, phase transfer catalyst tetrabutylammonium bromide, pH regulator sodium carbonate, and 3-chloropropyltriethoxysilane is 175:37:280:4 :50:478.

[0058] Dissolve tetrabutylammonium bromide in water to form a catalyst solution, the mass ratio of the two is 1:6, and the temperature is controlled at 10°C-50°C; sodium sulfide pentahydrate, sulfur powder, sodium carbonate and the remaining water are mixed at 50 Under the condition of ℃-80 ℃, react to prepare sodium polysulfide aqueous solution; mix sodium polysulfide aqueous solution and catalyst solution and keep the temperature at 50 ℃-70 ℃, enter the channel reaction device from a feed port of the channel reaction device, and simultaneously put 3 -Chloropropyltriethoxysilane is...

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Abstract

The invention aims at providing a method for preparing a polysulfide silane coupling agent by a passage reaction device for industrial polysulfide silane coupling agent production. Under the solvent condition, sodium polysulfide and 3-chloropropyl triethoxysilane take a reaction in the passage reaction device for preparing the polysulfide silane coupling agent, wherein (1) the structure general formula (a) of the polysulfide silane coupling agent is (C2H5O)3-Si-C3H6-Sn-C3H6-Si-(OC2H5)3. . . (a); in the formula, n=1 to 10, and the average value of the n is 2.0 to 4.0; (2) the passage reaction device is connected with a posttreatment device. The method solves the problems of long reaction period, unsafety, poor stability and the like of large-sized reaction equipment, and solves the problem that the blockage can be caused by using the passage reaction device.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing a polysulfide silane coupling agent by utilizing a channel reaction device. Background technique [0002] The method of preparing polysulfide silane coupling agent by using sodium polysulfide and 3-chloropropyltriethoxysilane is known, including non-solvent process and solvent process. The non-solvent process refers to the preparation of sodium polysulfide from sulfur and anhydrous sodium sulfide under high temperature and anaerobic conditions, and then reacts with 3-chloropropyltriethoxysilane; the solvent process is divided into organic solvent process, aqueous solution phase transfer catalyst process, salt solution phase transfer catalyst process, aqueous buffer system phase transfer catalyst process, water-organic solvent phase transfer catalyst process, etc. Non-solvent technology, because sulfur and sodium polysulfide are eas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/1892
Inventor 陶再山李春华
Owner 南京曙光新材料有限公司
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