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A preparing method of hydantoin epoxy resin

A technology of hydantoin epoxy resin and epichlorohydrin, which is applied in the field of organic chemical raw material manufacturing, can solve the problems of not being able to filter out sodium chloride particles, losing the superiority of hydantoin epoxy resin, and difficulty in recycling epichlorohydrin, etc. , to achieve high epoxy value, reduce the amount of "three wastes" and avoid side reactions

Active Publication Date: 2016-08-10
NANTONG BAICHUAN NEW MATERIAL CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When epichlorohydrin is in contact with alcohols with active hydrogen for a long time under alkaline conditions, it may convert epichlorohydrin into alcohol ethers, which leads to the complexity of the reaction and makes the recovery of epichlorohydrin Propane becomes difficult, increasing unit consumption of production
In addition, in the case of precipitation to constant weight and high viscosity of the product, it is doubtful whether the by-produced, fine sodium chloride particles dispersed in the resin can be basically filtered out
And even if it is said in this method, light yellow solid or liquid is obtained after precipitation and filtration, it also shows that the molecular weight and viscosity of the obtained product are too large, and the superiority of hydantoin epoxy resin has been lost, so it is difficult to Downstream is well applied

Method used

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  • A preparing method of hydantoin epoxy resin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A preparation method of hydantoin epoxy resin, the steps comprising:

[0037] (1) Add 0.3 mol (38.4 g) of 5,5-dimethylhydantoin and 1.8 mol (166.5 g) Epichlorohydrin, so that the molar ratio of 5,5-dimethylhydantoin and epichlorohydrin is 1:6;

[0038] (2) Add 0.48% (1 g) tetramethylammonium bromide of 204.9 g of the sum of the mass of 5,5-dimethylhydantoin and epichlorohydrin in the flask as the ring-opening catalyst of epichlorohydrin. Place the reactor in an oil bath, start stirring, feed nitrogen gas at a flow rate of 20mL / min, gradually increase the temperature of the oil bath, and heat the reactant to 115°C in 3 hours to carry out the ring-opening reaction of epichlorohydrin;

[0039] (3) After 3 hours of reaction, stop the heating of the oil bath, maintain the stirring state, cool the reaction solution to 30°C, and then stop the nitrogen flow;

[0040] (4) Add 0.93 times (190.2 g) of acetone as a solvent to the sum of 204.9 g of 5,5-dimethylhydantoin and epichl...

Embodiment 2

[0051] A preparation method of hydantoin epoxy resin, the steps comprising:

[0052] (1) Add 0.3 mol (38.4 g) of 5,5-dimethylhydantoin and 1.5 mol (138.8 g) Epichlorohydrin, so that the molar ratio of 5,5-dimethylhydantoin and epichlorohydrin is 1:6;

[0053] (2) Add 0.28% (0.5g) tetramethylammonium chloride of 177.2g of the sum of 5,5-dimethylhydantoin and epichlorohydrin to the flask as the ring-opening catalyst of epichlorohydrin, Place the reactor in an oil bath, start stirring, feed nitrogen gas at a flow rate of 15mL / min, gradually increase the temperature of the oil bath, and heat the reactant to 116°C in 3.5 hours to carry out the ring-opening reaction of epichlorohydrin ;

[0054] (3) After reacting for 3.5 hours, stop the heating of the oil bath, maintain the stirring state, cool the reaction solution to 28°C, and then stop the nitrogen flow;

[0055] (4) Add 1.08 times (190.7g) tetrahydrofuran as a solvent to the sum of 177.2g of the mass of 5,5-dimethylhydantoin...

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Abstract

The invention relates to a preparing method of hydantoin epoxy resin. The method adopts 5,5-dimethylhydantoin and epichlorohydrin as raw materials, adopts a quaternary ammonium salt as a ring-opening catalyst, and includes heating and reacting under nitrogen protection, cooling, gradually adding a calculated amount of granular sodium hydroxide as a ring-closing catalyst in batches with a lower aliphatic ketone or tetrahydrofuran being adopted as a solvent, subjecting materials to suction filtration when the solvent exits to remove a part of sodium chloride granules, transferring filtrate to a distillation device, performing vacuum distillation, transferring a product out of an evaporator when the volume is reduced by about a half and a salt separates out, performing suction filtration to remove the salt, performing a plurality of times of vacuum distillation and suction filtration until no salt separates out through observation from the materials in vacuum distillation, and performing vacuum distillation until no solvent is evaporated in 1-5 min so as to obtain a product. The method is advantageous in that the method can effectively remove sodium chloride granules which are a by-product in a preparing process, thus reducing the content of inorganic chlorine in the product and improving product quality.

Description

technical field [0001] The invention relates to a method for preparing a low-polymerization epoxy resin product, in particular to a method for preparing a hydantoin epoxy resin, and belongs to the field of organic chemical raw material manufacturing. Background technique [0002] Hydantoin is a five-membered heterocyclic compound containing two nitrogen atoms, and it is a substance with a non-benzene ring nitrogen heterocyclic structure. Hydantoin epoxy resin formed from it and epichlorohydrin etc. is not flammable and has low smoke emission even when burned. Hydantoin epoxy resin has good solubility in water when it is not cured, and it also has excellent mechanical properties, thermal stability and good process performance. After it is cured with acids, aldehydes, amines, and imidazoles, the cured product has a small shrinkage rate and good crack resistance under the environment of temperature changes, so it has good heat resistance and weather resistance. The materials ...

Claims

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Application Information

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IPC IPC(8): C08G59/10
CPCC08G59/022C08G59/10
Inventor 薛建军张晓周国君潘洁姜伟伟马俊华
Owner NANTONG BAICHUAN NEW MATERIAL CO LTD
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