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Novel method for preparing triglycidyl isocyanurate

A technology of glycidyl ester and isocyanuric acid tri, which is applied in the direction of organic chemistry and coating, can solve the problems of affecting the electrical performance of TGIC, low yield, and high recycling cost, so as to solve the problem of sewage treatment, reduce production cost, Guaranteed productivity effect

Active Publication Date: 2015-09-09
HUANGSHAN HUAHUI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This synthetic route has the following disadvantages: in the first step reaction, the feed ratio of raw material isocyanuric acid and epichlorohydrin is about 1:15, and the amount of epichlorohydrin is far excessive, and the recovery cost is high; the second step ring-closing reaction The yield is low, and the product contains chlorine, which seriously affects the electrical properties of TGIC

Method used

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  • Novel method for preparing triglycidyl isocyanurate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 10 g of isocyanuric acid was added into the four-necked flask, and at the same time, 50% sodium hydroxide solution was slowly added dropwise, and the reaction temperature was maintained at 60°C. During the reaction, the pH value of the reaction system was maintained at 7.5. After mechanical stirring for 0.5 hours, 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 used for later use. Through infrared detection and liquid phase detection, it was proved that isocyanuric acid has been combined with hydrogen The sodium oxide reacted completely, and the yield of the reaction was 95%.

[0016] Add the dried trisodium isocyanurate (moisture content≤0.5%) and excess epichlorohydrin (mass ratio: 18:1) into the flask at the same time, and add the phase transfer catalyst benzyl trimethyl chloride ammonium chloride. The reaction is carried out under the condition of an...

Embodiment 2

[0019] 10 g of isocyanuric acid was added into the four-necked flask, and at the same time, 50% sodium hydroxide solution was slowly added dropwise, and the reaction temperature was maintained at 55°C. During the reaction, the pH value of the reaction system was maintained at 7.5. After mechanical stirring for 1 hour, the water was distilled off by vacuum distillation, and the remaining liquid was filtered to obtain a white solid, which was dried in an oven for 12 hours and then used for later use. Through infrared detection and liquid phase detection, it was proved that isocyanuric acid had been combined with hydrogen The sodium oxide reacts completely, and the yield of the reaction is above 98%.

[0020] Add the dried trisodium isocyanurate (moisture content ≤ 1.0%) and excess epichlorohydrin (mass ratio: 15:1) into the flask at the same time, and add the phase transfer catalyst benzyl triethyl chloride ammonium chloride. The reaction is carried out under the condition of ...

Embodiment 3

[0023] 10 g of isocyanuric acid was added into the four-necked flask, and at the same time, 50% sodium hydroxide solution was slowly added dropwise, and the reaction temperature was maintained at 50°C. During the reaction, the pH value of the reaction system was maintained at 8.2. After 2 hours of mechanical stirring, 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 used for later use. Through infrared detection and liquid phase detection, it was proved that isocyanuric acid had been combined with hydrogen The sodium oxide reacts completely, and the yield of the reaction is above 98%.

[0024] Add the dried trisodium isocyanurate (moisture content ≤ 2.0%) and excess epichlorohydrin (mass ratio: 16:1) into the flask at the same time, and add the phase transfer catalyst benzyl triethyl chloride ammonium chloride. The reaction is carried out under the condition of ...

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Abstract

The invention discloses a method for preparing triglycidyl isocyanurate, which comprises the following steps: (1) reacting isocyanuric acid and a sodium hydroxide solution under low temperature conditions, keeping the pH value of the reaction system at 4-6, and carrying out vacuum distillation to continuously distil water out of the reaction system to obtain trisodium isocyanurate; (2) sufficiently drying the trisodium isocyanurate, and reacting with excessive epoxy chloropropane in the presence of a phase-transfer catalyst to obtain a triglycidyl isocyanurate crude product; and (3) carrying out vacuum distillation on the excessive epoxy chloropropane, adding a methanol solvent, and cooling to crystallize, thereby obtaining the triglycidyl isocyanurate pure product. The method efficiently solves the problem of sewage treatment caused by chlorine-containing wastewater, ensures the product yield, and lowers the production cost. The product can satisfy the national standard. The method has the advantages of simple technique and low equipment investment, and is suitable for wide popularization and application.

Description

technical field [0001] The invention belongs to the field of chemical production and relates to a green preparation method of a common powder coating curing agent, in particular to a new method for preparing triglycidyl isocyanurate. Background technique [0002] Triglycidyl isocyanurate (TGIC) is a heterocyclic compound, mainly used as a cross-linking curing agent for carboxyl-containing polyester resin (PES) and polyacrylate (PA). Due to the stable triazine ring structure in the TGIC molecule, the TGIC powder coating has good heat resistance and weather resistance; at the same time, the triazine ring has an amide group, which makes it easy to crystallize into crystals, suitable for large-scale industrial production . In addition, TGIC can undergo curing reaction with epoxy curing agents such as carboxylic acid, acid anhydride, amine, phenolic resin, etc. to form a cross-linked infusible insoluble substance, which has excellent mechanical, heat resistance, arc resistance a...

Claims

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Application Information

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IPC IPC(8): C07D405/14C09D7/12
CPCC07D405/14C09D7/63
Inventor 方向宏杨志萍汤增荣何领曹镇
Owner HUANGSHAN HUAHUI TECH
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