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A kind of 4-vinyl epoxycyclohexane and preparation method thereof

A technology based on epoxycyclohexane and epoxy ring, which is applied in the field of 4-vinylepoxycyclohexane and its preparation, can solve the problems of product gel time prolongation, heavy metal ion residues, and affecting production efficiency. Achieve shortened gel time, low chlorine content, and improved production efficiency

Active Publication Date: 2019-12-13
JIANGSU TETRA NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Because prior art method adopts the method for traditional catalyzer to prepare 4-vinyl epoxycyclohexane, usually contains heavy metal ion (such as tungsten W) in this type of catalyzer, so reaction product also contains certain heavy metal ion residue correspondingly; Due to the influence of heavy metal ion catalysts, the final product also has heavy metal ions residues. This trace amount of heavy metal ions also affects the curing speed of the product (ie gel time); the cross-linking in the molecule is affected during curing, resulting in the gel time of the product extended, thus affecting production efficiency

Method used

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  • A kind of 4-vinyl epoxycyclohexane and preparation method thereof
  • A kind of 4-vinyl epoxycyclohexane and preparation method thereof
  • A kind of 4-vinyl epoxycyclohexane and preparation method thereof

Examples

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Effect test

Embodiment 1

[0028] A kind of preparation method of 4-vinyl epoxycyclohexane is characterized in that comprising the steps:

[0029] (1) Add 100g of 4-vinylcyclohexene, 300g of toluene, 110g of acetic anhydride and 8g of sodium acetate into a 1000ml three-necked flask, and cool to 5°C-15°C while stirring;

[0030] (2) Then start to drop 150g 35% hydrogen peroxide, control the rate of addition to keep the temperature of the reaction system no more than 25°C, complete the dropwise addition in about 2 hours, and react for 4 hours after the addition;

[0031] (3) Slowly add 60 g of commercially available 30% liquid caustic soda to the system to adjust the pH to 10-12, stir for 10 minutes and stand for phase separation, and separate the upper organic phase;

[0032] (4) Add 50g of 10% sodium sulfite aqueous solution to the organic phase, stir for 10 minutes and leave to separate the phases, separate the upper organic phase (pH=10-12, starch potassium iodide test paper shows no peroxide residue)...

Embodiment 2

[0035] A kind of preparation method of 4-vinyl epoxycyclohexane is characterized in that comprising the steps:

[0036] (1) Add 98g of 4-vinylcyclohexene, 280g of toluene, 108g of acetic anhydride and 8.5g of sodium acetate into a 1000ml three-necked flask, and cool to 5°C-15°C while stirring;

[0037] (2) Then start to drop 155g 35% hydrogen peroxide, control the rate of addition to keep the temperature of the reaction system no more than 25° C., drop it in about 2.5 hours, and react for 5 hours after the addition;

[0038] (3) Slowly add 65 g of commercially available 32% liquid caustic soda to the system to adjust the pH to 10-12, stir for 15 minutes to stand for phase separation, and separate the upper organic phase;

[0039] (4) Add 55g of 8% sodium sulfite aqueous solution again, stir for 15 minutes and let stand to separate the phases, separate the upper organic phase (pH=10-12, starch potassium iodide test paper shows no peroxide residue), and recover toluene through p...

Embodiment 3

[0042] A kind of preparation method of 4-vinyl epoxycyclohexane is characterized in that comprising the steps:

[0043] (1) Add 99g of 4-vinylcyclohexene, 290g of toluene, 112g of acetic anhydride and 8.4g of sodium acetate into a 1000ml three-necked flask, and cool to 5°C-15°C while stirring;

[0044] (2) Then start to drop 131g of 40% hydrogen peroxide, control the rate of addition to keep the temperature of the reaction system no more than 25°C, complete the dropwise addition in about 1.8 hours, and react for 6 hours after the addition;

[0045] (3) Slowly add 64 g of commercially available 35% liquid caustic soda to the system to adjust the pH to 10-12, stir for 12 minutes and stand for phase separation, and separate the upper organic phase;

[0046] (4) Add 35g of 15% sodium sulfite aqueous solution again, stir for 12 minutes and let stand to separate the phases, separate the upper organic phase (pH=10-12, starch potassium iodide test paper shows no peroxide residue), and...

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Abstract

The invention relates to 1,2-epoxy-4-vinylcyclohexane. 1,2-epoxy-4-vinylcyclohexane is prepared from the following raw materials in percentage by mass: 12%-14% of 4-vinyl-1-cyclohexene, 40%-45% of toluene, 17%-19% of acetic anhydride, 2%-4% of sodium acetate and 21%-23% of 35% hydrogen peroxide. The invention further relates to a preparation method of 1,2-epoxy-4-vinylcyclohexane. Prepared 1,2-epoxy-4-vinylcyclohexane has high yield and selectivity, and purity of a reaction product is improved; besides, 1,2-epoxy-4-vinylcyclohexane has low chlorine content and has no heavy metal residues, andgelation time of the product is short.

Description

technical field [0001] The invention relates to a preparation method of olefin, in particular to a 4-vinyl epoxycyclohexane and a preparation method thereof. Background technique [0002] 4-Vinyl epoxycyclohexane is an important fine chemical intermediate. It is a chemical product with a wide range of uses and good performance in the series of epoxy products. It can be widely used in the production of LED packaging materials, organic silicon modification Epoxy monomer synthesis, electronic chip packaging, coupling agents, adhesives, luminescent materials, reactive diluents and other industries and fields. The packaging of high-end electronic products is the basic manufacturing technology. The core parts of various industrial products (household appliances, computers, communications, medical care, aerospace, automobiles, etc.) are all composed of microelectronic components, optoelectronic components, radio frequency and wireless components, etc. Packaging, power supply and d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D301/16C07D301/12C07D303/04
CPCC07D301/12C07D301/16C07D303/04
Inventor 韩建伟常杨军贾泉吴宏亮
Owner JIANGSU TETRA NEW MATERIAL TECH
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