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Method for preparing mercaptosilane coupling agent by channel reaction device

A technology of mercaptosilane coupling agent and channel reaction device, 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 long reaction cycle, poor stability, and unsafety , to achieve the effects of long conversion cycle, large output elasticity, and slow mass and heat transfer

Active Publication Date: 2019-04-23
南京曙光新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Technical problem: the purpose of the present invention is to provide a method for preparing mercaptosilane coupling agent by using channel reaction device for the large-scale industrial production of mercaptosilane coupling agent, and to prepare mercaptosilane coupling agent by using channel reaction device under solvent conditions, which solves the problem of Large-scale reaction equipment has problems such as long reaction cycle, unsafety, poor stability, impurities, polymers, etc., especially to reduce the odor problem caused by the production of large-scale reaction equipment

Method used

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  • Method for preparing mercaptosilane coupling agent by channel reaction device
  • Method for preparing mercaptosilane coupling agent by channel reaction device
  • Method for preparing mercaptosilane coupling agent by channel reaction device

Examples

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Effect test

Embodiment 1

[0062] Embodiment 1 prepares 3-mercaptopropyltriethoxysilane

[0063] The equation for the reaction of the two main raw materials is:

[0064] (C 2 h 5 O) 3 SiC 3 h 6 Cl + NaHS→(C 2 h 5 O) 3 SiC 3 h 6 SH + NaCl

[0065] Mass ratio of raw materials, 3-chloropropyltriethoxysilane (content 98%): sodium hydrosulfide hydrate (content 71%): solvent water: phase transfer catalyst tetrabutylammonium bromide: pH regulator sodium carbonate For 650:200:380:8:50.

[0066] Proceed as follows:

[0067] (1) Prepare sodium hydrosulfide aqueous solution: dissolve 200 parts of sodium hydrosulfide in 360 parts of water to prepare an aqueous solution.

[0068] (2) Preparation of aqueous solution of phase transfer catalyst: Dissolve 8 parts of phase transfer catalyst tetrabutylammonium bromide in 20 parts of water. (3) Mix the sodium hydrosulfide aqueous solution, the phase transfer catalyst aqueous solution, and the pH regulator sodium carbonate evenly, and heat the temperature to 6...

Embodiment 2

[0077] Example 2 Preparation of 3-octanoylthio-1-propyltriethoxysilane

[0078] The equation for the reaction of the two main raw materials is:

[0079] (C 2 h 5 O) 3 SiC 3 h 6 Cl + NaS(C=O)C 7 h 15 →(C 2 h 5 O) 3 SiC3 h 6 S(C=O)C 7 h 15 + NaCl

[0080] The mass ratio of raw materials, 3-chloropropyltriethoxysilane:sodium thiooctanoate aqueous solution (content 30%):phase transfer catalyst tetrabutylammonium bromide aqueous solution (content 25%) is 435:1060:24.

[0081] The steps are: add the aqueous solution of phase transfer catalyst tetrabutylammonium bromide to the aqueous solution of sodium thiooctanoate, mix well and heat to 75°C, the mixed solution, 3-chloropropyltriethoxy Silane is passed into the channel reaction device to react at the same time, and the reaction temperature is controlled at 90°C. The crude product is taken from the post-processing device connected to the channel reaction device, cooled and layered, and the upper organic phase is taken...

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Abstract

The invention provides a method for preparing a mercaptosilane coupling agent by using a channel reactor. In a solvent, a channel reactor is utilized to prepare the mercaptosilane coupling agent. The structural general formula of the mercaptosilane coupling agent is XmSiC3H6S(C=O)nY, wherein each X is independently alkyl group, alkoxy group, hydroxy group, R(OR')LO-, -ORO- or N(RO-)3, and at least one X is alkoxy group, hydroxy group or N(RO-)3; Y is hydrogen or alkyl group; R and R' are respectively independently straight-chain or branched-chain alkyl group; the average value of L is 1-30; m is 1, 2 or 3; and n is 0 or 1. The corrected diameter of the channel reactor channel is one micrometer to several centimeters; and the channel reactor is connected with an after-treatment device. The method solves the problems of long reaction period, poor stability, existence of impurity polymers and the like in the large-size reactor, and especially reduces the odor caused by the large-size reactor production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing a mercaptosilane coupling agent by using a channel reaction device. Background technique [0002] The mercaptosilane coupling agent and the modified mercaptosilane coupling agent (hereinafter referred to as mercaptosilane) that have appeared in recent years contain basic groups of SiC 3 h 6 S-) is an indispensable supporting raw material for green tires filled with white carbon black. Especially under the background of the introduction of relevant policies at home and abroad to promote the development of green tires, the research and development of mercaptosilane has also become an important part of the industry. Research hotspots. At present, the products that have been mass-produced include 3-mercaptopropyltrimethoxysilane (commonly known as: KH-590), 3-mercaptopropyltriethoxysilane (commonly known as: KH-580), 3-mercaptopropylm...

Claims

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Application Information

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Patent Type & Authority Patents(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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