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Preparing method for epoxy resin active diluent of low organic chlorine content

An epoxy resin reactive diluent and organochlorine technology, applied in the field of reactive diluent preparation, can solve the problems of insignificant effect, multiple production process waste water, increase production cost, etc. The effect of low production costs

Active Publication Date: 2007-04-11
NANTONG XINGCHEN SYNTHETIC MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation method of the active diluent in the prior art: firstly, under the action of a catalyst, monohydric or polyhydric alcohols, phenols, acid anhydrides or carboxylic acids undergo a ring-opening reaction with equal or slightly excess epichlorohydrin, and then use an alkali metal Hydroxide undergoes a ring-closing reaction, and then extracts, washes, and removes the solvent to obtain a reactive diluent. The content of organic chlorine is high (>0.02, eq / 100), and it is difficult to meet the increasingly sophisticated application requirements of epoxy resins.
Usually, the method to reduce the organic chlorine content of active diluent is to increase the amount of alkali metal hydroxide, and reduce the organic chlorine content by using a method with a large amount of hydroxyl substances in alcohol or phenol. The effect of this method is not obvious. Moreover, more production process wastewater will be generated, which will increase the consumption of alkali metal hydroxides and increase production costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A preparation method of epoxy resin reactive diluent with low organic chlorine content, comprising:

[0021] The first step is to mix one of alcohol or phenol, benzene solvent and catalyst. The mass of benzene solvent is 0.5-1.0 times of the mass of alcohol or phenol. For example, it can be selected as 0.7, 0.82, 0.9, 0.95. 1-10‰ of alcohol or phenol mass, for example, 1‰, 2.5‰, 3‰, 3.4‰, 5‰, 6.5‰, 8‰, 9‰;

[0022] The alcohol is one of monohydric or dihydric or polyhydric alcohols, the phenol is monohydric phenol or dihydric phenol, the number of carbon atoms in alcohol is 2-14, the number of carbon atoms in phenol is 6-10, and the benzene solvent is benzene or One of toluene, the catalyst is BF 3 -Ether or SnCl 4 Or a kind of in the quaternary ammonium salt, in the present embodiment, alcohol can be butanol, octanol, lauryl alcohol, allyl alcohol, benzyl alcohol, ethylene glycol, polyethylene glycol, propylene glycol, butanediol, hexane One of diol, glycerol, and t...

Embodiment 2

[0031] Synthesis of benzyl glycidyl ether: Dissolve 216g benzyl alcohol in 150ml benzene, add 3ml BF 3 -Ethyl ether, add 85g of epichlorohydrin dropwise at 30~35°C, drop it in about 4 hours, keep it at 35~40°C for 2 hours, add a certain amount of benzyltriethylammonium chloride 0.2g, at 30±2 Add 347g of sodium hydroxide 30% solution dropwise at ℃ for 2 hours. After dropping, raise the temperature to 45-50℃ and keep it for 2 hours. Then add about 500g of benzene, wash with water until neutral, debenzene to 100℃ under normal pressure, and then add The pressure was -0.09Mpa and debenzene was reduced to 100°C to obtain 328g of benzyl glycidyl ether with an epoxy value of 0.432eq / 100g and an organic chlorine content of 0.0116eq / 100g.

[0032] Without adding benzyltriethylammonium chloride, the benzyl glycidyl ether obtained under the same conditions has an epoxy value of 0.408eq / 100g and an organic chlorine content of 0.0352eq / 100g.

Embodiment 3

[0034] Synthesis of trimethylolpropane glycidyl ether: add 400ml benzene to 335g trimethylolpropane, add BF 3-Ethyl ether 7.5ml, add 694g of epichlorohydrin dropwise at 35~40°C, drop it in about 6 hours, adjust the temperature to 40~45°C for 3 hours, add 0.96g of benzyltriethylammonium chloride, Add 660g of sodium hydroxide 40% solution dropwise at 2°C for 2 hours. After dropping, the temperature is raised to 45-50°C and maintained for 2 hours. The head pressure was -0.092Mpa and debenzene was decompressed to 140°C to obtain 743g of trimethylolpropane glycidyl ether with an epoxy value of 0.717eq / 100g and an organic chlorine content of 0.0031eq / 100g.

[0035] Without adding benzyltriethylammonium chloride, the trimethylolpropane glycidyl ether obtained under the same conditions has an epoxy value of 0.701eq / 100g and an organic chlorine content of 0.0195eq / 100g.

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PUM

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Abstract

The process of preparing active epoxy resin diluent with low organochlorine content includes the following steps: mixing alcohol or phenol, benzene solvent and catalyst, dropping chloroepoxy propane into the mixture at 10-55 deg.c for 4-12 hr, and stilling at 20-60 deg.c for 2-4 hr; adding quaternary ammonium salt as the phase transfer catalyst, dropping water solution of sodium hydroxide of 30-50 wt% concentration at 20-55 deg.c for 2-4 hr, raising the temperature by 5-15 deg.c, and maintaining for 1-5 hr; and extracting, neutralizing or water washing to eliminate sodium chloride, and eliminating benzene solvent to obtain active epoxy resin diluent with low organochlorine content. During the ring-closing reaction, phase transfer catalyst, rather than alkali metal hydroxide, is added to result in even high organochlorine eliminating effect.

Description

technical field [0001] The invention relates to a preparation method of a reactive diluent, in particular to a preparation method of an epoxy resin reactive diluent with low organic chlorine content. Background technique [0002] Reactive diluents generally refer to low-molecular compounds with one or more than two epoxy groups, which can directly participate in the curing reaction of epoxy resin and become part of the cross-linked network structure of cured epoxy resin. Almost no effect, the main function of the reactive diluent is to reduce the viscosity of the epoxy resin curing system, and sometimes it can also play the role of toughening, strengthening or flame retardancy. [0003] The preparation method of the active diluent in the prior art: firstly, under the action of a catalyst, monohydric or polyhydric alcohols, phenols, acid anhydrides or carboxylic acids undergo a ring-opening reaction with equal or slightly excess epichlorohydrin, and then use an alkali metal ...

Claims

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Application Information

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IPC IPC(8): C08G59/40C07D303/08C08K5/15
Inventor 江秀明陈明朱胜仙
Owner NANTONG XINGCHEN SYNTHETIC MATERIAL
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