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A kind of method of liquid phase catalytic synthesis cyanuric acid

A cyanuric acid, liquid-phase catalysis technology, applied in the direction of organic chemistry, can solve the problems of low reaction temperature, long reaction time, increased energy consumption, etc., and achieve the effects of increasing reaction temperature, good product quality, and reducing solvent costs

Active Publication Date: 2011-12-21
王铁招
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The liquid phase method (USP3297697, CN 101624380A) using a relatively low boiling point solvent can obtain a product with an equivalent whiteness to the refined product of the solid phase method, the reaction temperature is low, the reaction time is long, the amide by-products are high, and the reaction at the boiling point Increased energy consumption of the reaction

Method used

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  • A kind of method of liquid phase catalytic synthesis cyanuric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Heat 100 grams of urea in a reaction kettle to 80°C, dehydrate at a constant temperature for 15 minutes under stirring, add 100 grams of N,N-dimethylformamide, 0.4 grams of catalyst sodium dihydrogen phosphate, and 5 grams of cyanuric acid, and stir The temperature was raised to reflux under the conditions, and the urea was condensed for 5 hours at the reflux temperature of 165° C. to obtain a hot slurry composed of cyanuric acid and N,N-dimethylformamide. Cool to room temperature under stirring conditions to fully crystallize cyanuric acid, filter with a vacuum filter, wash the cyanuric acid filter cake with clear water after the suction filtration is completed until there is no organic solvent residue, and obtain the cyanuric acid filter cake. Dry in a drying oven at 110°C for 3 hours to obtain 58.3 grams of white cyanuric acid. In this example, by weighing before and after the reaction of the reflux condenser, it is determined that the urea sublimation number is 3 gr...

Embodiment 2

[0021] Heat 100 grams of urea in a reaction kettle to 80°C, and heat for 15 minutes under stirring conditions, add 200 grams of N,N-dimethylformamide, 0.2 grams of catalyst sodium dihydrogen phosphate, and 10 grams of cyanuric acid, and stir. Lower the temperature to reflux, urea was subjected to condensation reaction at 160° C. of reflux temperature for 6 hours, and the following operations were the same as example 1 to obtain 51.2 grams of white cyanuric acid, 3 grams of urea sublimation number, and the solvent contained 14.4 grams of cyanuric acid after the reaction, producing 80% rate.

Embodiment 3

[0023] Heat 100 grams of urea in a reaction kettle to 80°C, heat for 15 minutes under stirring conditions, add 200 grams of N,N-dimethylacetamide, 0.2 grams of catalyst sodium dihydrogen phosphate, and 6 grams of cyanuric acid, and stir. Lower the temperature to reflux, and the urea under the reflux temperature of 176° C. was subjected to condensation reaction for 4 hours. The following operations were the same as example 1 to obtain 63.3 grams of white cyanuric acid, 4 grams of urea sublimation number, and the solvent contained 6 grams of cyanuric acid after the reaction. Rate 92%

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Abstract

The invention discloses a CA (Cyanuric Acid) liquid phase catalytic synthesis method which comprises the following steps of: (1) heating and dehydrating urea; (2) adding an organic solvent, a catalyst and the CA, heating to make the urea have a condensation reaction at backflow temperature, obtaining heat slurry consisting of the CA and the organic solvent, wherein the organic solvent is N,N-dimethylformamide or N,N-dimethylacetylamide, the catalyst is sodium dihydrogen phosphate or disodium hydrogen phosphate, and the CA finished product is a common industrial product; and (3) cooling down the heat slurry obtained from the step (2), carrying out solid-liquid separation to obtain a CA filter cake containing the organic solvent, washing the filter cake in clear water till no organic solvent is residual, and drying to obtain white CA crystals. According to the CA liquid phase catalytic synthesis method disclosed by the invention, the CA finished product can be directly obtained without refining, and the solvent can be recycled after recovery treatment, thus the production cost is low, the production yield is high, the quality is good, no three wastes pollute the environment, and the production is safe; and the CA liquid phase catalytic synthesis method is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for liquid-phase catalytic synthesis of cyanuric acid, which belongs to the technical field of organic synthesis in the chemical industry. Background technique [0002] Cyanuric acid or cyanuric acid (abbreviated as CA) is an important chemical intermediate, hundreds of important derivatives can be synthesized from it, and new compounds are still increasing, involving medicine, pesticides, dyes, coatings and auxiliaries and other fields. The series of chemical products developed downstream mainly include: disinfectant series, including chlorinated isocyanuric acid compounds trichloroisocyanuric acid and sodium dichloroisocyanurate; halogen-free nitrogen-containing flame retardant cyanuric acid-melamine ( MCA); Polyester powder coating curing agent TGIC (TGIC), isocyanurate compounds trihydroxyethyl isocyanurate, triacryl isocyanurate, triglycidyl isocyanurate, etc. organic compounds. [0003] The production methods ...

Claims

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Application Information

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IPC IPC(8): C07D251/32
Inventor 王铁招
Owner 王铁招