Method for preparing tri(3-trimethoxysilylpropyl) isocyanurate

A technology of trimethoxysilylpropyl and trimethoxysilyl, which is applied in the field of preparation of triisocyanurate, can solve the problems of many side reactions, unsatisfactory, slow reaction speed, etc., so as to save reaction time , Improve production efficiency, improve the effect of reaction speed

Inactive Publication Date: 2010-08-18
ZHEJIANG HUTU PHARMCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the relatively complex reaction system of this kind of process, there are many side reactions and slow reaction speed, and all patents do not describe the subsequent separation process in detail, so it cannot ensure that the quality of the product can meet the needs of the market
[0005] Because 1,3,5-tris[3-(trimethoxysilyl)propyl]-1,3,5-triazine-2,4,6-trio

Method used

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  • Method for preparing tri(3-trimethoxysilylpropyl) isocyanurate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put 2050ml of dimethyl sulfoxide, 2052.8g (10mol) of 3-isocyanatopropyltrimethoxysilane (99.0% GC content) and 10.8g (0.2mol) of sodium methylate into the reactor, and pass through the reactor with nitrogen replacement In the air, the temperature was raised to 100°C, and the reaction was maintained for 6 hours, then the temperature was lowered to 20°C, and the insoluble matter was removed by filtration to obtain a filtrate. The filtrate is concentrated at a temperature of 150° C. under a vacuum of 15 Pa until there is no distillate under negative pressure to obtain a reddish-brown viscous liquid 1847g (i.e. crude product, content 85%), the selectivity of the product is 98.5%, and it is divided into 100g / min speed into 0.2m 2 In the molecular still, the temperature of the molecular still is controlled to be 200°C, the vacuum degree is 5Pa, and the light component obtained is 1,3,5-tris[3-(trimethoxysilyl) Propyl]-1,3,5-triazine-2,4,6-trione, weight 1535g, yield 74.78%,...

Embodiment 2

[0027] Put 3075ml of dimethyl sulfoxide, 2052.8g (10mol) of 3-isocyanatopropyltrimethoxysilane (99.0% GC content) and 16.2g (0.3mol) of sodium methoxide into the reactor, and pass through the reactor to replace it with nitrogen In the air, the temperature was raised to 130°C, and the reaction was kept for 4 hours, then the temperature was lowered to 20°C, and the insoluble matter was removed by filtration. The filtrate is concentrated at a temperature of 180° C. under a vacuum of 15 Pa until there is no distillate under negative pressure to obtain 1865 g of a reddish-brown viscous liquid (i.e. crude product, content 83.4%). The selectivity of the product is 97.6%, which is divided into 100 g / min speed into 0.2m 2 In the molecular still, the temperature of the molecular still is controlled to be 200°C, the vacuum degree is 2Pa, and the light component obtained is 1,3,5-tris[3-(trimethoxysilyl) Propyl]-1,3,5-triazine-2,4,6-trione, weight 1570g, yield 76.48%, content (ie purity...

Embodiment 3

[0029] Put 2052ml of N, N-dimethylformamide, 2052.8g (10mol) of 3-isocyanatopropyltrimethoxysilane (GC content 99.0%), 21.6g (0.4mol) of sodium methoxide into the reactor, and feed nitrogen The air in the reactor was replaced, the temperature was raised to 150° C., the temperature was kept for 3 hours, the temperature was lowered to 20° C., and the insoluble matter was removed by filtration. The filtrate is concentrated at a temperature of 150° C. under a vacuum of 15 Pa until no distillate is obtained, and 1901 g of a reddish-brown viscous liquid (i.e. crude product, content 86.1%) is obtained. The selectivity of the product is 99.1%. / min speed into 0.2m 2 In the molecular still, the temperature of the molecular still is controlled to be 230°C, the vacuum degree is 10Pa, and the light component obtained is 1,3,5-tris[3-(trimethoxysilyl) Propyl]-1,3,5-triazine-2,4,6-trione, weight 1601g, yield 77.99%, content (ie purity) 98.05%.

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Abstract

The invention discloses a method for preparing tri(3-trimethoxysilylpropyl) isocyanurate, which comprises the following steps: performing polycondensation reaction on 3-isocyanate group propyl trimethoxy silane serving as a monomer in the presence of a catalyst and a solvent, and concentrating the filtrate obtained by filtering the reaction product to obtain a crude product of 1,3,5-tri[3-(trimethoxysilicyl)propyl]-1,3,5-triazine-2,4,6-triketone. The method has the advantages of low cost, high conversion rate, high purity of the product, good selectivity of the product, simple operation and suitability for industrial production.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of tris(3-trimethoxysilylpropyl)isocyanurate. Background technique [0002] 1,3,5-tris[3-(trimethoxysilyl)propyl]-1,3,5-triazine-2,4,6-trione (Tris(3-trimethoxysilylpropyl)isocyanurate) also known as Tris(3-trimethoxysilylpropyl)isocyanurate, molecular formula: C 21 h 45 N 3 o 12 Si 3 , CAS: 26115-70-8, boiling point 543.9°C (760mmHg), stable at room temperature, soluble in acetonitrile, acetone, N,N-dimethylformamide (DMF), etc., methanol is hydrolyzed when it meets water, and its structural formula is as follows Show:. [0003] Wherein, Me is a methyl group. [0004] 1,3,5-tris[3-(trimethoxysilyl)propyl]-1,3,5-triazine-2,4,6-trione is an excellent adhesion promoter and As a bonding agent, it can effectively improve the adhesion of polyvinyl chloride (PVC) and other materials to the substrate, and is widely used in various chemical building materi...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 吴建平胡文江唐欣陈思先
Owner ZHEJIANG HUTU PHARMCHEM
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