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Method for preparing mercaptosilane coupling agent by using phase transfer catalyst

The technology of a mercaptosilane coupling agent and a phase transfer catalyst is applied in the field of preparing a mercaptosilane coupling agent by using a phase transfer catalyst, which can solve the problems of cumbersome steps, high cost, low cost and the like, and achieves simple process, low manufacturing cost, and synthetic Responsive effect

Active Publication Date: 2019-11-22
湖南正量工程技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method steps are cumbersome. After the reaction is finished, triethylamine hydrochloride, a by-product of water treatment, is added to the reaction system. The total reaction time is more than 4 hours, and the reaction temperature is 80-150 ° C. The energy consumption is high and the cost is high.
[0007] At present, there is no method for preparing mercaptosilane coupling agent using phase transfer catalyst with high material utilization rate, high product yield, high product purity, high safety and low cost on the market.

Method used

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  • Method for preparing mercaptosilane coupling agent by using phase transfer catalyst
  • Method for preparing mercaptosilane coupling agent by using phase transfer catalyst

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Embodiment 1

[0023] The present embodiment comprises the following steps: add 126g water, 61.6g mass fraction to 70% sodium hydrosulfide (0.77mol) in the 1000ml three-neck flask that is equipped with heating, stirring, cooling reflux and temperature measuring device, start stirring, wait until all solids After dissolving, add 5.1g tetrabutylammonium bromide as a phase transfer catalyst, 336g toluene as a protective agent, 168.4g (0.7mol) chloropropyltriethoxysilane, heat and turn on the cooling reflux device, and heat up to 90~ 95°C, heat preservation reaction for 3 hours, stop stirring after the reaction, let stand for 2 minutes, the organic layer is sampled and detected by gas chromatography, the residual amount of chloropropyltriethoxysilane is 0.85%, the water phase is separated, and the organic layer is first normal Pressure evaporated toluene to remove the solvent, and then distilled under reduced pressure to collect 110~115°C (absolute pressure 4kPa) fractions to obtain 158g of produ...

Embodiment 2

[0026] The present embodiment comprises the following steps: add 126g water, 61.6g mass fraction to 70% sodium hydrosulfide (0.77mol) in the 1000ml three-necked flask that is equipped with heating, stirring, cooling reflux device and temperature measuring device, start stirring, wait for solid After all dissolved, add 4.5g tetrabutylammonium chloride, 280g toluene, 139.0g (0.7mol) chloropropyltrimethoxysilane in sequence, heat and turn on the cooling reflux device, raise the temperature to 88-92°C, and keep it warm for 4 hours After the reaction, stop stirring and leave it for 2 minutes. The organic layer is sampled and detected by gas chromatography. The residual amount of chloropropyltriethoxysilane is 0.68%. Distill under reduced pressure, collect fractions at 110-115°C (absolute pressure 4kPa), and obtain 129g of mercaptosilane coupling agent product.

[0027] According to gas chromatography detection in this example, the content of the prepared mercaptosilane coupling age...

Embodiment 3

[0029] The present embodiment comprises the following steps: add 130g water, 91.2g mass fraction to be 70% sodium hydrosulfide (0.84mol) in the 1000ml three-neck flask that is equipped with heating, stirring, cooling reflux and temperature measuring device, start stirring, wait until all solids After dissolving, add successively the composite catalyst that is made up of 2.5g benzyltriethylammonium chloride and 2.5g trioctylmethylammonium chloride tetrabutylammonium chloride, 380g sherwood oil, 127.8g (0.7mol) chloropropane Methyldimethoxysilane, heat up to 75-80°C, keep warm for 4 hours, stop stirring after the reaction, let stand for 2 minutes, organic layer sampling gas chromatography tracking detection, chloropropylmethyldimethoxysilane The residual amount is 0.45%, and the water phase is separated. The organic layer is first evaporated to remove the solvent toluene at normal pressure, and then distilled under reduced pressure to collect 95~98°C (absolute pressure 4kPa) frac...

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Abstract

The invention discloses a method for preparing a mercaptosilane coupling agent by using a phase transfer catalyst. Sodium hydrosulfide and halogenated alkyl alkoxy silane are used as raw materials, and a hydrocarbon organic solvent is adopted as a protective agent. The method comprises the following steps: carrying out synthetic reaction on the sodium hydrosulfide in a water phase and the halogenated organosilane dissolved in the hydrocarbon organic solvent by utilizing a phase transfer catalyst, separating a reaction product organic layer after the synthetic reaction is finished, performing distillation to remove the hydrocarbon organic solvent, and carrying out reduced pressure filtration and distillation to obtain the mercaptosilane coupling agent. The synthesis reaction is relatively complete, the product quality is relatively high, the yield of the prepared mercaptosilane coupling agent is greater than or equal to 93%, and the purity is greater than or equal to 99%; the process issimple, the synthesis reaction process is easy to control, tail gas can be recycled, and the safety of organic synthesis reaction is enhanced; the reaction requires a low temperature, and low requirements on equipment; the hydrocarbon organic solvent is recyclable; and the manufacturing cost is low.

Description

technical field [0001] The invention relates to a synthesis method of a mercaptosilane coupling agent, in particular to a method for preparing a mercaptosilane coupling agent using a phase transfer catalyst. Background technique [0002] Mercaptosilane coupling agent is a silicone coupling agent containing difunctional groups with different properties in the molecule. It is mainly used in the surface treatment of materials, and can improve the performance of glass fiber, clay, carbon black, silica, calcium carbonate, mica, etc. The compatibility between inorganic fillers and resins can improve the mechanical, electrical, water-resistant and weather-resistant properties of rubber and plastics, and is widely used in rubber and plastic products. [0003] At present, the synthesis of mercaptosilane coupling agent is usually carried out under anhydrous conditions, by reacting halogenated organosilane with ethylenediamine salt of hydrogen sulfide, or by reacting halogenated organo...

Claims

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Application Information

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IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/1892
Inventor 岳岩君唐友明华伟赵外荣龙丹丸子周德国胡清亮
Owner 湖南正量工程技术有限公司