Epoxy resin dechlorinating agent as well as preparation method and application thereof

A technology of epoxy resin and chlorine removal agent, which is applied in the field of chlorine removal agent to achieve the effects of large application value, reduction of chlorine content and cost of use

Active Publication Date: 2022-04-15
智仑超纯环氧树脂(西安)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the epoxy resin prepared by this method still has a relatively high chlorine content, and the chlorine removal agent used in this chlorine removal method can only be used once

Method used

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  • Epoxy resin dechlorinating agent as well as preparation method and application thereof
  • Epoxy resin dechlorinating agent as well as preparation method and application thereof
  • Epoxy resin dechlorinating agent as well as preparation method and application thereof

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preparation example Construction

[0044] The preparation principle of the epoxy resin dechlorination agent of the present invention is: the epoxy resin dechlorination agent uses 1,5-hexadiyne and benzene azide as raw materials, copper sulfate pentahydrate and sodium ascorbate as catalysts, through azide and The click reaction of the alkyne can obtain the intermediate I, and then the addition reaction of the alkyne and the amino group can obtain the intermediate II, and finally, the epoxy resin dechlorination agent can be obtained through the polymerization reaction of the terminal double bond.

[0045] The epoxy resin dechlorination agent of the present invention has a ring structure, and there are 4 polarized C-H bonds on the 1,2,3-triazole ring and the benzene ring, which can realize - Captured, and the structure is stable. It captures Cl - The mechanism is as follows:

[0046]

[0047] The present embodiment provides a kind of preparation method of epoxy resin chlorine removal agent, comprises the foll...

Embodiment 1

[0062] Add 44.35g of the first organic solvent (the mass ratio of water and tert-butanol is 1:1) in the there-necked flask equipped with stirrer, then add 7.88g catalyst (wherein the mol ratio of copper sulfate pentahydrate and sodium ascorbate is 1: 2), the temperature was raised to 60°C. Subsequently, 7.8g (0.1mol) of 1,5-hexadiyne and 11.9g (0.1mol) of benzene azide were dissolved in 20g of the first organic solvent, and slowly added dropwise to the three-necked flask, and the dropping time was kept at 4h. 12h, full argon protection. After completion of the reaction, cool to room temperature, extract with dichloromethane, separate the organic phase, dry with anhydrous sodium sulfate, filter and spin evaporate to remove the dichloromethane to obtain intermediate I.

[0063] 19.7g (0.1mol) of intermediate I and 7.1g (0.1mol) of acrylamide were dissolved in 40.2g of acetone and placed in a reactor, 0.67g of sodium hydroxide was added as a catalyst, and the pressure of the rea...

Embodiment 2

[0066] Add 107.8g of the first organic solvent (the mass ratio of water and tert-butanol is 1:1) in the there-necked flask equipped with stirrer, then add 10.65g catalyst (wherein the mol ratio of copper sulfate pentahydrate and sodium ascorbate is 1: 2), the temperature was raised to 60°C. Subsequently, 9.4g (0.12mol) of 1,5-hexadiyne and 11.9g (0.1mol) of benzene azide were dissolved in 20g of the first organic solvent, and slowly added dropwise to the three-necked flask, and the dropping time was maintained at 5h, and the reaction 14h, full argon protection. After completion of the reaction, cool to room temperature, extract with dichloromethane, separate the organic phase, dry with anhydrous sodium sulfate, filter and spin evaporate to remove the dichloromethane to obtain intermediate I.

[0067] 19.7g (0.1mol) of intermediate I and 8.5g (0.12mol) of acrylamide were dissolved in 65.8g of acetone and placed in the reactor, 0.94g of sodium hydroxide was added as a catalyst,...

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Abstract

The invention provides an epoxy resin dechlorinating agent as well as a preparation method and application thereof. According to the epoxy resin dechlorinating agent, 1, 5-hexadiyne and azidobenzene serve as raw materials, copper sulfate pentahydrate and sodium ascorbate serve as catalysts, an intermediate I is obtained through the click reaction of azide and alkyne, then an intermediate II is obtained through the addition reaction of alkyne and amino, and finally the epoxy resin dechlorinating agent is obtained through the polymerization reaction of end-group double bonds. The epoxy resin dechlorinating agent has a cyclic structure and has high affinity and selectivity to chloride ions, four polarized C-H bonds exist on a 1, 2, 3-triazole ring and a benzene ring, the chloride ions in epoxy resin can be stably captured, and the epoxy resin dechlorinating agent can be recycled while the chlorine content of the epoxy resin is reduced.

Description

technical field [0001] The present application relates to the technical field of chlorine removal agents, in particular to an epoxy resin chlorine removal agent and its preparation method and application. Background technique [0002] With the continuous development of information technology, electronic components, integrated circuits, chips and other related industries have stricter requirements on the chlorine content of epoxy resin. Epoxy resin is commonly used as an encapsulant and adhesive in the electronics industry. If the chlorine content is too high, the hydrolyzable chlorine in the epoxy resin will be hydrolyzed under high temperature and pressure to produce hydrochloric acid during the bonding process of semiconductor packaging and electronic components. , so as to corrode components and circuit boards, so this requires the epoxy resin used in the electronics industry to have a lower chlorine content. [0003] At present, the commonly used chlorine removal method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/60C08G59/02
CPCY02W30/62
Inventor 杜彪
Owner 智仑超纯环氧树脂(西安)有限公司
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