Preparation process of phenolic hydroxy epoxidation product

A technology of oxidation products and phenolic hydroxyl rings, applied in chemical/physical processes, organic compound/hydride/coordination complex catalysts, catalytic reactions, etc., can solve environmental pollution, reduce hydrolyzable chlorine content, low epoxy products and other problems, to achieve process stability, reduce the content of hydrolyzable chlorine and inorganic chlorine, and reduce the effect of environmental protection pressure

Inactive Publication Date: 2019-03-12
江苏和和新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The obtained product needs to be washed with water to remove salt, refined with alkali, and post-treatment steps such as water washing, neutralization, filtration, and solvent removal to reduce the hydrolyzable chlorine content. The lowest hydrolyzable chlorine content reaches 68.9ppm, but the above-mentioned post-treatment process Produce a large amount of waste water and VOC, causing great environmental pollution
[0007] Therefore, the currently disclosed phenolic hydroxyl epoxidation process still cannot directly obtain the epoxy product with low hydrolyzable chlorine content

Method used

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  • Preparation process of phenolic hydroxy epoxidation product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048]Heat 0.1 mol of benzyldiethylamine, 0.1 mol of γ-chloropropyltriethoxysilane, 100 mL of ethanol, and 0.02 mol of potassium iodide to 75°C under nitrogen protection, react for 1.5 hours, and obtain the quaternary ammonium salt mother liquor after filtering the product , Add 50mL of quaternary ammonium salt mother liquor dropwise to 100mL of distilled water / ethanol (20ml of water, 80ml of ethanol) to obtain a mixed solution, adjust the pH of the mixed solution to 5.0 with glacial acetic acid, and after standing for 2 hours, add 40 grams of halloysite nano The tube is put into it, fully soaked for 1-3 hours, and the water is removed by evaporation, and the obtained product is halloysite nanotube functionalized with quaternary ammonium salt.

[0049] Add bisphenol A and epichlorohydrin (molar ratio 1:2.1) under normal pressure, add the halloysite nanotube catalyst of the quaternary ammonium salt functionalization prepared in this embodiment (add catalyst according to benzyldi...

Embodiment 2

[0051] The raw materials and process parameters of the phenolic hydroxyl epoxidation process are exactly the same as in Example 1, except that the catalyst used is the halloysite nanotube catalyst that has been used 5 times and recovered in Example 1. The performance test results of the final product are listed in Table 1 below.

Embodiment 3

[0053] Heat 0.1 mol of benzyldiethylamine, 0.1 mol of γ-chloropropyltrimethoxysilane, 100 mL of methanol, and 0.02 mol of potassium iodide to 60°C under nitrogen protection, react for 1.5 hours, and filter the product to obtain a quaternary ammonium salt mother liquor. Add 50mL of quaternary ammonium salt mother liquor dropwise to 100mL of distilled water / methanol (20ml of water, 80ml of methanol), adjust the pH of this solution to 5.0 with glacial acetic acid, put 40g of halloysite nanotubes into it after standing for 2 hours, and fully After soaking for 3 hours, the water was removed by evaporation, and the obtained product was halloysite nanotubes functionalized with quaternary ammonium salts.

[0054] Add bisphenol F and epichlorohydrin (molar ratio 1:2) under normal pressure, add the halloysite nanotube catalyst of the quaternary ammonium salt functionalization prepared in this embodiment (add catalyst according to benzyldiethylamine raw material mol The amount is 0.005 o...

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Abstract

The invention discloses a preparation process of a phenolic hydroxy epoxidation product. A compound containing a phenolic hydroxyl group and epoxy chloropropane serve as raw materials; under the action of catalysts, chlorohydrin ether is prepared by etherification ring-opening reaction; a phenolic hydroxy epoxidation product is then prepared by ring-closure reaction; the catalysts are quaternary ammonium salt functionalized halloysite nanotubes. By the aid of the preparation process, the epoxidation product with a low hydrolysable chlorine content can be directly prepared, with no complicatedpost-treatment technologies required; the preparation process is stable, material consumption and energy consumption are low, byproducts are fewer, the catalysts can be recycled, and the preparation process can be used for large-scale industrial production.

Description

technical field [0001] The invention relates to an epoxy resin preparation process, in particular to a preparation process of a phenolic hydroxyl epoxidation product. Background technique [0002] Due to its excellent mechanical and electrical properties, epoxy resin has developed into a large class of thermosetting resins and is widely used in adhesives, structural composite materials, electronic semiconductor packaging and other fields. [0003] At present, the preparation process of epoxy resin is prepared by reacting phenolic hydroxyl compound with epichlorohydrin. The preparation process has a great influence on the effective utilization rate of epichlorohydrin, product yield, closed loop rate and waste water generation. With the increasingly stringent national environmental protection policies, the development of high-efficiency and green environmental protection processes has become extremely urgent. [0004] The traditional preparation process only uses alkali, such...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/26C07D301/28C07D303/24C07D303/27C07D303/23B01J31/02B01J31/26C08G59/06
CPCC07D301/26C07D301/28C07D303/23C07D303/24C07D303/27C08G59/022C08G59/063B01J31/0254B01J31/26B01J2231/4288Y02P20/584
Inventor 叶书怀张涛李诚马丹吉和信钟程苟明明袁凯王亮邵博文胡雪敬
Owner 江苏和和新材料股份有限公司
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