A kind of preparation method of reactive epoxy resin diluent with low total chlorine content

A technology of total chlorine content and epoxy resin, applied in the direction of organic chemistry, etc., can solve the problem of high total chlorine, and achieve the effects of low hydrolyzed chlorine, reduced side reactions, and fewer by-products

Active Publication Date: 2018-06-22
辽阳鑫宇化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the shortcoming that the total chlorine of the reactive epoxy diluent prepared by the prior art is relatively high, the present invention provides a method for preparing a reactive epoxy resin diluent with low total chlorine content, the purpose is to adopt a high-efficiency composite catalyst in the etherification reaction stage, During the reaction process, reflux dehydration is carried out and special reagents are added to prevent side reactions from occurring. During post-treatment, the method of adding alkali and refining quaternary ammonium salts is used to reduce the hydrolyzed chlorine of the product to a lower level, the product is stable, and the epoxy resin is finally reduced. Chlorine content in diluent

Method used

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  • A kind of preparation method of reactive epoxy resin diluent with low total chlorine content
  • A kind of preparation method of reactive epoxy resin diluent with low total chlorine content

Examples

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Effect test

Embodiment 1

[0028] The preparation method of the active epoxy resin thinner of the low total chlorine content of the present embodiment is carried out according to the following steps:

[0029] (1) With C8 fatty alcohol and epichlorohydrin as raw materials, first the C8 fatty alcohol is pretreated, and 195g of C8 fatty alcohol is added in a 1000mL four-necked flask equipped with a stirrer, a thermometer and a condenser, and the purity of the C8 fatty alcohol is ≥ 99.0%, then heated the flask to 95°C under nitrogen protection, turned on the vacuum pump for dehydration for 60 minutes, then lowered the temperature to 90°C, added a composite catalyst to the flask: 1g of boron trifluoride ether, 2g of aluminum chloride and ferric chloride The mixture was stirred at 200rpm for 10min, kept at 100°C, and 416.3g of epichlorohydrin was added dropwise to the flask within 6h;

[0030] (2) After epichlorohydrin has been added dropwise, add 3.8g of 50% aqueous sodium hydroxide solution in the flask, st...

Embodiment 2

[0038] The preparation method of the reactive epoxy resin diluent of the low total chlorine content of this comparative example is carried out according to the following steps:

[0039] (1) With C8 fatty alcohol and epichlorohydrin as raw materials, first the C8 fatty alcohol is pretreated, and 130g of C8 fatty alcohol is added in a 1000mL four-necked flask equipped with a stirrer, thermometer and condenser. %, then heated the flask to 105°C under the protection of nitrogen, turned on the vacuum pump for dehydration for 60 minutes, then lowered the temperature to 90°C, added a composite catalyst to the flask: 0.65g boron trifluoride ether, added 1.3g aluminum chloride and chloride The iron mixture was stirred at 200rpm for 10min, kept at 100°C, and 369.6g of epichlorohydrin was added dropwise to the flask within 6h;

[0040] (2) After epichlorohydrin has been added dropwise, add 2.5g of 50% aqueous sodium hydroxide solution to the flask, stir for 10min, then add dropwise 100g ...

Embodiment 3

[0043] The preparation method of the active epoxy resin thinner of the low total chlorine content of the present embodiment is carried out according to the following steps:

[0044] (1) Take C10 fatty alcohol and epichlorohydrin as raw materials, first carry out pretreatment to C10 fatty alcohol, add 142gC10 fatty alcohol in a 1000mL four-necked flask equipped with stirrer, thermometer and condenser, C10 fatty alcohol purity ≥ 99.0%, then heated the flask to 105°C under nitrogen protection, turned on the vacuum pump for dehydration for 60 minutes, then lowered the temperature to 90°C, added a composite catalyst to the flask: 0.71g boron trifluoride ether, added 1.4g aluminum chloride and chlorine The mixture of ferric oxide was stirred at 200rpm for 10min, kept at 100°C, and 277.5g of epichlorohydrin was added dropwise to the flask within 6h;

[0045] (2) After epichlorohydrin has been added dropwise, add 4g of a 50% aqueous sodium hydroxide solution to the flask, stir for 10m...

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Abstract

The invention belongs to the technical field of epoxy resin preparation, and particularly relates to a preparation method of an active epoxy resin diluent with the low total chlorine content. The method comprises the steps that a compound catalyst is adopted in an etherification open loop reaction to improve the reaction efficiency, an alkaline solution and a mixture of a special reducing agent tris(2-carboxyethyl)phosphine and Zn powder are continuously added into a reaction system of an obtained chlorohydrin ether intermediate to inhibit a side reaction, and mixed liquid of alkali metal hydroxides and quaternary ammonium salt is lastly added for refining. According to the preparation method, the technology is stable, few by-products are generated, material consumption and energy consumption are low, and a large amount of epoxy chloropropane is not needed in the epoxy resin preparation process, so that the production cost is reduced; the product is stable, low in hydrolyzed chlorine content and low in chrominance; the epoxy resin diluent prepared through the method has the advantages that the total chlorine content is lower than 700 ppm, the hydrolyzable chlorine content is lower than 100 ppm, the viscosity is lower than 6 mPa / s, and the epoxide equivalent ranges from 245 g / eq to 275 g / eq.

Description

technical field [0001] The invention belongs to the technical field of epoxy resin preparation, and in particular relates to a preparation method of an active epoxy resin diluent with low total chlorine content. Background technique [0002] Alkyl glycidyl ether is a commonly used low-viscosity, colorless and odorless monofunctional diluent. It has the advantages of good flexibility and low volatility. Wetting property, excellent dye wetting ability. [0003] In recent years, related enterprises in my country are also developing epoxy resins with low total chlorine, which are mainly used in electronic materials, but lack of supporting low total chlorine active diluents, resulting in high content of halogen group elements in electronic formulations, especially It is the long-term use outdoors that leads to a decrease in the stability of electronic materials, and a decrease in insulation performance and corrosion resistance. Therefore, in the production process of epoxy resin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/18C08G59/20C07D303/22C07D301/26
CPCC07D301/26C07D303/22C08G59/18C08G59/20
Inventor 郭树志
Owner 辽阳鑫宇化工有限公司
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