Preparation method of hydrogenated bisphenol A epoxy resin

A technology of epoxy resin preparation and hydrogenation of bisphenol, applied in the direction of organic chemistry, can solve the problems of difficult stirring, many by-products, long production cycle, etc., and achieve the goal of reducing raw material consumption, low material consumption and energy consumption, and high product yield Effect

Inactive Publication Date: 2012-11-07
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the difference in the structure and properties of hydrogenated bisphenol A and bisphenol A, following the general bisphenol A epoxy resin synthesis route will face many difficulties in actual production
For example, a small amount of water in the reaction raw materials causes Lewis acid hydrolysis, which affects the ring-opening effect; hydrogenated bisphenol A is insoluble in toluene, methyl isobutyl ketone (

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In a 2000ml reactor equipped with a stirrer, thermometer, water separator and condenser, 360g of hydrogenated bisphenol A and 400g of solvent toluene were added, stirring was turned on, and the temperature was raised to 113°C for reflux dehydration. After dehydration for 1h, the temperature was lowered to 100°C and 1.01g of the catalyst boron trifluoride ether was added. Through the peristaltic pump, 310g of epichlorohydrin was added dropwise at a constant speed to carry out the ring-opening addition etherification reaction. The dropping time of epichlorohydrin was 2.5h. After the addition, the temperature change and hydrogenation of the system were continuously observed. Dissolution of bisphenol A. As the ring-opening reaction exotherms, appropriate cooling measures should be taken during the dropping of epichlorohydrin to ensure that the reaction temperature is within 98-102°C. After the reaction, 207 g of toluene was recovered. Add 400 g of pure water to the reactio...

Embodiment 2

[0032] In a 2000ml reactor equipped with a stirrer, a thermometer, a water separator and a condenser, 360g of hydrogenated bisphenol A and 600g of solvent toluene were added, stirring was turned on, and the temperature was raised to 113°C for reflux dehydration. After dehydration for 1h, the temperature was lowered to 100°C and 1.01g of the catalyst boron trifluoride ether was added. 333g epichlorohydrin was added dropwise by a peristaltic pump at a constant speed to carry out the ring-opening addition etherification reaction. The dropping time of epichlorohydrin was 3h, and it was maintained for 1h after the addition. The temperature change and hydrogenated bisphenol of the system were continuously observed during the dripping process. A dissolution situation. As the ring-opening reaction exotherms, appropriate cooling measures should be taken during the dropping of epichlorohydrin to ensure that the reaction temperature is within 98-102°C. After the reaction, 450 g of toluen...

Embodiment 3

[0034] In a 2000ml reactor equipped with a stirrer, thermometer, water separator and condenser, 360g of hydrogenated bisphenol A and 420g of solvent toluene were added, stirring was turned on, and the temperature was raised to 110°C for reflux dehydration. After dehydration for 0.5h, the temperature is lowered to 100℃ and the catalyst AlCl is added. 4 1.01g. 333g epichlorohydrin was added dropwise by a peristaltic pump at a constant speed to carry out the ring-opening addition etherification reaction. The dropping time of epichlorohydrin was 3h, and it was maintained for 1h after the addition. The temperature change and hydrogenated bisphenol of the system were continuously observed during the dripping process. A dissolution situation. As the ring-opening reaction exotherms, appropriate cooling measures should be taken during the dropping of epichlorohydrin to ensure that the reaction temperature is within 98-102°C. After the reaction, 240 g of toluene was recovered. Add 400 ...

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PUM

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Abstract

The invention relates to a preparation method of hydrogenated bisphenol A epoxy resin. The preparation method comprises the steps of raw material pre-treatment, ring-opening addition and etherifying, ring-closing epoxidation, product post-treatment and the like. The specific steps are as follows: based on hydrogenated bisphenol A and epoxy chloropropane as raw materials, adding solvent; performing ring-opening etherifying by taking Lewis acid as a catalyst to produce chlorohydrin ether immediate; recovering part of the solvent, adding alkali solution and performing ring-closing dechlorinating reaction; carrying out post-treatment steps such as neutralizing, extracting, water washing, vacuum desolventizing to obtain hydrogenated bisphenol A epoxy resin, wherein the epoxide equivalent of the product is 210-240g/eq; the hydrolyzable chlorine content is not more than 1000ppm; the inorganic chloride content is not more than 10ppm; the viscosity is 2000-5000mPas at 25 DEG C; and the volatile component content is not more than 0.1%. The preparation method of hydrogenated bisphenol A epoxy resin has the advantages of stable process, low material and energy consumption, few by-products, simple water-washing and separating operation and high product yield, therefore, the preparation method can be applied in large-scale industrial production.

Description

Technical field [0001] The invention belongs to the technical field of organic polymer compounds, and specifically relates to a preparation method of hydrogenated bisphenol A epoxy resin. Background technique [0002] General-purpose bisphenol-A epoxy resin has disadvantages such as easy weathering, aging, and yellowing when used outdoors. In terms of molecular structure, the reason for the poor weather resistance of bisphenol A epoxy resin is due to the presence of a large number of unsaturated benzene ring structures in the molecular chain. Under the condition of long-term exposure to the atmosphere or ultraviolet rays, the molecular chain is easily broken, resulting in a significant decrease in the transparency, insulation, and strength of the cured bisphenol A epoxy resin. The development of epoxy resin products with strong weather resistance and suitable for outdoor use has become the expectation of epoxy resin production and application manufacturers in my country. [0003]...

Claims

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Application Information

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IPC IPC(8): C07D301/02C07D303/27C07D303/24
Inventor 任六波肖雄江铃傅江福汤文红
Owner CHINA PETROLEUM & CHEM CORP
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