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Method for preparing low content of organic chlorine epoxy resin

A technology of epoxy resin and solid epoxy resin, which is applied in the field of preparation of epoxy resin with low organic chlorine content, can solve the problems of increasing production cost, failing to meet the requirements of epoxy resin, reducing the yield of epoxy resin, etc., to achieve Increased productivity, low organic chlorine content, and reduced costs

Inactive Publication Date: 2008-09-17
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] It can be seen from the above that due to the limitation of process conditions when using conventional methods to produce epoxy resin, the organic chlorine content in the obtained product is relatively high, while the organic chlorine content in general electronic grade epoxy resin is required to be below 500ppm, high-purity electronic grade epoxy resin The organic chlorine content in the resin is required to be below 200ppm, and the epoxy resin produced by conventional methods cannot meet the requirements. Therefore, the epoxy resin produced by conventional methods must be refined to reduce the organic chlorine content, but a large amount of aging resin will be produced during refining , which greatly reduces the yield of epoxy resin and increases the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: novolak resin: 120g, epichlorohydrin: 660g, tetramethylammonium chloride: 2.4g, NaOH solution (42%): 135g.

[0025] Preparation steps: Add the raw materials novolac resin and epichlorohydrin into a 1000ml three-necked flask according to the ratio, start stirring to completely dissolve the novolak resin, then add tetramethylammonium chloride and stir evenly, and then raise the temperature to 65 ℃ for 3 hours, then, use a constant pressure dropping funnel to add 135g NaOH solution dropwise at a constant speed, and control the pressure in the three-necked flask to -0.06MPa~-0.085MPa, and the released epichlorohydrin is refluxed into the three-necked flask, and the water is left in the three-necked flask. In the liquid container, the dropping time is 2.5h. After the dropping is completed, keep the temperature and keep the pressure for 0.5h, and then filter the salt generated by the reaction with filter paper, and deepoxidize at 100~120℃, -0.06MPa~-0.09MPa Chlorop...

Embodiment 2

[0030] Example 2: bisphenol A: 129g, epichlorohydrin: 700g, tetramethylammonium chloride: 1.2g, NaOH solution (42%): 103.5g, toluene: 300g.

[0031] Preparation steps: Add the raw materials bisphenol A and epichlorohydrin into a 1000ml three-necked flask according to the ratio, start stirring to completely dissolve the bisphenol A, then add tetramethylammonium chloride and stir evenly, then raise the temperature to 85°C for reaction 3h, then, add 103.5g NaOH solution dropwise at a constant speed with a constant pressure dropping funnel, and control the pressure in the three-necked flask to -0.06MPa~-0.085MPa, and the released epichlorohydrin is refluxed into the three-necked flask, and the water is left in the liquid separation In the container, the dropping time is 3 hours. After the dropping is completed, keep the temperature and pressure for 1 hour, and remove the epichlorohydrin with salt at 100~120℃, -0.06MPa~-0.09MPa, then add 300g of toluene to dissolve the resin, and W...

Embodiment 4

[0044] Example 4: novolak resin: 120g, epichlorohydrin: 500g, NaOH solution (42%): 105.7g, toluene: 400g.

[0045] Preparation steps: Add the raw materials novolac resin and epichlorohydrin into a 1000ml three-neck flask according to the ratio, start stirring to completely dissolve the novolac resin, maintain the temperature at 70°C, and add 105.7g NaOH dropwise at a constant speed using a constant pressure dropping funnel Solution, and the pressure in the three-necked flask is controlled to -0.06MPa~-0.085MPa, the released epichlorohydrin is refluxed into the three-necked flask, and the water is left in the liquid separator. The dropping time is 7h. Hold the pressure for 2h. Remove epichlorohydrin with salt at 100~120°C, -0.06MPa~-0.09MPa, then add 400g of toluene to dissolve the resin, and wash off the salt in the resin, and finally at 100~140°C, -0.06MPa Toluene was removed at ~-0.09MPa to obtain 175g of epoxy resin.

[0046] Product performance:

[0047] Productive rate...

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Abstract

The invention relates to a method for preparing epoxy resin with low content of organic chlorine. The method is characterized in that: when in preparation, the used raw materials comprise: bisphenol A and the derivative thereof or linear phenol-formaldehyde resin or bisphenol S, quaternary ammonium salt, epichlorohydrin, sodium hydroxide and water; the preparation steps are as follows: the bisphenol A and the derivative thereof or the linear phenol-formaldehyde resin or the bisphenol S and the epichlorohydrin are dissolved and etherified; the temperature is controlled, the removed epichlorohydrin is returned to a three-neck flask, the water is remained in a liquid divider, the dripping time is 2 to 4h, the temperature and the pressure are kept for 0.5 to 1h after the completion of the dripping; a filter paper is used for filtering the salt which is generated by the reaction, and the epichlorohydrin is removed, thus obtaining the light yellow liquid or the solid epoxy resin. The preparation method which is provided by the invention can allow the synthetic epoxy resin to achieve the low content of the organic chlorine without being refined, thus greatly improving the yield of the epoxy resin, reducing the cost and having important practical significance on the development and the application.

Description

technical field [0001] The invention relates to a preparation method of epoxy resin with low organic chlorine content. Background technique [0002] Epoxy resins with low organic chlorine content have excellent physical and mechanical properties, electrical insulation properties, excellent bonding properties with various materials, and great flexibility in the use process, which are not available in other thermosetting resins. Therefore, it can be made into coatings, composite materials, casting materials, adhesives, molding materials and injection molding materials, and has been widely used in various fields of the national economy. [0003] The current preparation method of epoxy resin with low organic chlorine content is to produce epoxy resin by conventional method, and then refine the epoxy resin produced by conventional method to reduce the content of organic chlorine. [0004] There are three main processes for the production of epoxy resin in conventional methods: (...

Claims

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Application Information

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IPC IPC(8): C08G59/06C08G59/08
Inventor 陈立新景晨丽宋家乐
Owner NORTHWESTERN POLYTECHNICAL UNIV
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