Preparation method of high-ortho-position electronic grade phenolic resin with high hydroxyl content

A technology of phenolic resin and high hydroxyl group, which is applied in the field of preparation of electronic-grade phenolic resin with high ortho position and high hydroxyl content, which can solve the problems of inability to be used as a curing agent, high content of phenolic resin impurities and free phenol, poor adhesion and mechanical properties, etc. problem, to achieve the effect of increasing the reaction crosslinking point, less impurity content, and fast curing speed

Inactive Publication Date: 2018-08-03
SUZHOU XINGYE MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The phenolic resin produced by this method has high content of impurities and free phenol, poor electrical insulation, adhesion and mechanical properties, and obviously cannot be used as a curing agent for epoxy molding compounds used in electronic packaging materials

Method used

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  • Preparation method of high-ortho-position electronic grade phenolic resin with high hydroxyl content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Add 85 kg of phenol, 15 kg of o-cresol, and 1.6 kg of zinc acetate in the reactor, stir and heat up to 90°C;

[0035] (2) Start timing when the temperature reaches 90°C, add 120 kg of 37% formaldehyde solution dropwise continuously within 2 hours, and keep warm for 2 hours after adding;

[0036] (3) After the heat preservation is completed, vacuum dehydration is carried out, and the electronic grade deionized water vapor system is turned on at the same time, and the water vapor is passed into the bottom of the reaction kettle. The temperature of the inner material is controlled at 50-100°C, and the temperature is raised slowly. When the temperature reaches 120°C, the dehydration is stopped;

[0037] (4) Immediately after dehydration, add deionized water at a temperature of 95°C to the reaction kettle, stir for 60 minutes and then stand still, separate the upper layer of water after standing still for 60 minutes, wash with water for 5 times in the same way, and finis...

Embodiment 2

[0041] (1) Add 75 kilograms of phenol, 20 kilograms of m-cresol, 5 kilograms of cardanol and 1.8 kilograms of zinc acetate in the reactor, stir and be warming up to 85 ℃;

[0042] (2) Start timing when the temperature reaches 90°C, add 140 kg of 37% formaldehyde solution dropwise continuously within 2.5 hours, and keep warm for 3 hours after adding;

[0043] (3) After the heat preservation is completed, vacuum dehydration is carried out, and the electronic grade deionized water vapor system is turned on at the same time, and the water vapor is passed into the bottom of the reactor. The pressure of the steam is controlled at 0.60Mpa, and the pressure in the reactor is controlled at -0.07Mpa. The temperature of the inner material is controlled at 50-100°C, and the temperature is raised slowly. When the temperature reaches 130°C, the dehydration is stopped;

[0044] (4) Immediately after the dehydration is completed, add deionized water at a temperature of 90°C to the reactor, st...

Embodiment 3

[0048] (1) Add 60 kg of phenol, 25 kg of nonylphenol, 15 kg of cardanol and 2.3 kg of zinc acetate in the reactor, stir and heat up to 95°C;

[0049] (2) Start timing when the temperature reaches 95°C, add 125 kg of 37% formaldehyde solution continuously dropwise within 1.5 hours, and keep warm for 4 hours after adding;

[0050] (3) After the heat preservation is completed, vacuum dehydration is carried out, and the electronic grade deionized water vapor system is turned on at the same time, and the water vapor is passed into the bottom of the reaction kettle. The temperature of the inner material is controlled at 50-100°C, and the temperature is raised slowly. When the temperature reaches 120°C, the dehydration is stopped;

[0051](4) Immediately after the dehydration is completed, add deionized water at a temperature of 90°C to the reactor, stir for 40 minutes, then stand still, separate the upper layer of water after standing still for 60 minutes, wash with water 5 times in...

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PUM

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Abstract

The invention relates to a preparation method of high-ortho-position special phenolic resin with high hydroxyl content. The preparation method is characterized in that zinc salt is adopted to performcatalysis, alkylphenol is adopted to replace phenol, the molar ratio of phenolic reaction is greater than 1, and after the reaction is finished, special deionized water washing and steam purging processes are adopted to effectively reduce the contents of impurity ions, volatile components and free phenols in the resin. The resin prepared by the preparation method provided by the invention has thecharacteristics of high electric insulativity, high cohesiveness, high thermal stability, high mechanical properties, low viscosity, low curing temperature, low dielectric constant, low thermal expansion coefficient, low hygroscopicity, low stress and the like, and can be widely applied to high and new technology fields of electronics, foundry industry, aerospace and the like.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and in particular relates to a preparation method of electronic-grade phenolic resin with high ortho position and high hydroxyl content. Background technique [0002] Electronic-grade special phenolic resins belong to the linear phenol formaldehyde series and are mainly used in the fields of epoxy molding compounds and copper clad laminates. Among them, the special phenolic resins used in the production of epoxy molding compounds not only require extremely low content of impurity ions and free phenols, but also take into account It has excellent electrical insulation and material processability. At present, it mainly depends on foreign imports, and only a few domestic enterprises produce, but there is still a big gap in quality compared with foreign imports. [0003] The domestic conventional production method is: formaldehyde and phenol are added to the reactor after being measured in...

Claims

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Application Information

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IPC IPC(8): C08G8/24
CPCC08G8/24
Inventor 王进兴戴旭吉祖明朱文英王文浩史制强沈杨彬
Owner SUZHOU XINGYE MATERIALS TECH
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