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ChemicalBook CAS DataBase List 1,3,5-Triglycidyl isocyanurate

1,3,5-Triglycidyl isocyanurate synthesis

6synthesis methods
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Yield:2451-62-9 84%

Reaction Conditions:

Stage #1:cyanuric acid with sodium hydroxide; pH=7.5 at 60;
Stage #2:epichlorohydrin with benzyltrimethylammonium chloride at 115 - 120; for 7.5 h;Catalytic behavior;Temperature;

Steps:

1
10 g of isocyanuric acid was added to a four-necked flask while slowly adding 50% sodium hydroxide solution, the reaction temperatureMaintained at 60 ° C. In the course of the reaction,The pH of the reaction system was maintained at 7.5.After the mechanical stirring for 0.5 hour, the water was distilled off under reduced pressure, and the remaining liquid was filtered to obtain a white solid which was dried in an oven for 12 hours and then allowed to pass the infrared detection and liquid phase detection,It was proved that isocyanuric acid had reacted completely with sodium hydroxide and the yield of the reaction was 95%.The dried trisodium isocyanurate (moisture content ≤ 0.5%) and excess epichlorohydrin (mass ratio18: 1) was added to the flask at the same time, and the phase transfer catalyst benzyltrimethylammonium chloride was added.The reaction is carried out under anhydrous reflux conditions and the reaction temperature is between 115 and 120 ° C. The reaction time was 7.5 hours.After completion of the reaction, excess epichlorohydrin was distilled off by distillation under reduced pressure.In the vacuum distillation, the system of vacuum control in the 10mmHg below the system temperature maintained at 35 ~ 40 ,Continuous distillation under reduced pressure for 6 hours, continue to heat up to 80 ~ 85 , continuous distillation under reduced pressure 2 hours,Excessive epichlorohydrin is distilled off.After the reaction product is distilled off under reduced pressure epichlorohydrin, methanol is added, crystallized and then filtered,A white solid TGIC (triglycidyl isocyanurate) was obtained in a yield of 84%.After testing, the epoxy equivalent of 102.4g / mol; chlorine content of 0.12%;Melting point between 97-99 ; epichlorohydrin residue of 12ppm; are in line with national standards.

References:

Mt. Huang Huahui Technology Co., Ltd.;Fang Xianghong;Yang Zhiping;Tang Zengrong;He Ling;Cao Zhen CN104892586, 2017, B Location in patent:Paragraph 0013-0016

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