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Synthetic method of thiocyanatopropyltriethoxysilane

A technology of thiocyanopropyltriethoxysilane and chloropropyltriethoxysilane, which is applied in the field of chemical preparation, can solve the problem of difficult product quality to meet new demands, unsatisfactory physical and chemical properties, troublesome process steps, etc. problems, to achieve the effect of low cost, short reaction time and high product yield

Inactive Publication Date: 2012-10-17
QINGDAO UNIV OF SCI & TECH
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AI Technical Summary

Problems solved by technology

However, the existing thiocyanopropyl triethoxysilane preparation process generally has troublesome process steps, high preparation cost, difficult product quality to meet new demands, unsatisfactory physical and chemical properties, and unfriendly environment.

Method used

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Examples

Experimental program
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Effect test

Embodiment

[0008] Example: Put 0.2mol of KSCN in 50ml of deionized water, and add NaOH at the same time to adjust the pH value of the reaction solution to 9-10, stir and heat the mixed solution in the reaction device to 65-70°C until the solids are all After dissolving, add 23ml of toluene, dissolve 0.006mol of triethylbenzyl ammonium bromide in 10ml of water, add it to the reaction device, heat up to 80-85°C, and keep the temperature to add 0.19mol of chloropropane Triethoxysilane was dripped into the reaction device of the mixed solvent at a flow rate. After the dripping was completed, the reaction was kept for 30 minutes. The whole process was kept in a state of stirring and reflux. After the reaction, stop heating and stirring, and separate the liquid. The lower layer is the water phase; the organic phase is washed with saturated NaCl solution, adsorbed by activated carbon, filtered and distilled under reduced pressure to obtain transparent liquid thiocyanopropyltriethoxysilane.

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Abstract

The invention relates to a synthetic method of thiocyanatopropyltriethoxysilane and belongs to the technical field of chemical preparation. The synthetic method comprises the following steps of: preparing potassium thiocyanate into a solution of 4 mol / L, stirring, adding NaOH, adjusting pH value, pouring into a reaction device, heating the mixed liquor until solids are dissolved, adding toluene, dissolving BTEAC into water to prepare a solution, adding the solution into the reaction device, heating, keeping warm, dropping chloropropyl triethoxysilane at flow velocity into the reaction device filled with the mixed solvent, carrying out thermostatic reaction, stopping heating and stirring, carrying out liquid separation to obtain an upper layer being an organic phase and a lower layer being a water phase, washing the organic phase by the use of a saturated NaCl solution, absorbing with active carbon and water-absorbing resin, filtering, followed by vacuum distillation so as to obtain thiocyanatopropyltriethoxysilane. The synthetic method has advantages of simple technological process, safe and reliable operation, short reaction time, high product yield, low cost and wide application range, and is especially suitable for large-scale industrial production.

Description

Technical field: [0001] The invention relates to a synthesis method of thiocyanopropyl triethoxysilane, which belongs to the technical field of chemical preparation. Background technique: [0002] Silane coupling agent is a general term for compounds containing organic functional groups and hydrolyzable silane active groups in the molecule. The purpose of using a coupling agent is to combine organic matter with incompatible fillers and rubber matrix to improve the adhesiveness of the compound. Adding a coupling agent to the compound can improve the dispersibility of the filler and improve the material properties and molding properties of the compound. Materials that utilize these properties include rubber resins, coatings, adhesives, glass, and metal surface treatment agents. Sulfur-containing silane coupling agent has always been an indispensable auxiliary agent in rubber processing, mainly used to improve the dispersion of inorganic fillers in rubber and improve the combi...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 孙立水葛国杰瞿永涛
Owner QINGDAO UNIV OF SCI & TECH
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