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 me

Method used

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

Examples

Experimental program
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Example Embodiment

[0033] Example 1

[0034] (1) Add 85 kilograms of phenol, 15 kilograms of o-cresol, and 1.6 kilograms of zinc acetate into the reactor, stir and raise the temperature to 90°C;

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

[0036] (3) After the heat preservation is completed, perform vacuum dehydration, and at the same time turn on the electronic grade deionized water vapor system, and pass the water vapor into the bottom of the reactor. The pressure of the water vapor is controlled at 0.80Mpa, and the pressure in the reactor is controlled at -0.09Mpa. The temperature of the internal materials is controlled at 50~100℃, and the temperature rises slowly. When the temperature reaches 120℃, the dehydration is stopped;

[0037] (4) Immediately after dehydration, add deionized water at a temperature of 95°C into the reactor, stir for 60 minute...

Example Embodiment

[0040] Example 2

[0041] (1) Add 75 kilograms of phenol, 20 kilograms of m-cresol, 5 kilograms of cardanol and 1.8 kilograms of zinc acetate into the reactor, stir and raise the temperature to 85°C;

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

[0043] (3) After the heat preservation is completed, perform vacuum dehydration, and at the same time turn on the electronic grade deionized water vapor system, and pass the water vapor into the bottom of the reactor. The pressure of the water vapor is controlled at 0.60Mpa, and the pressure in the reactor is controlled at -0.07Mpa. The temperature of the internal material is controlled at 50~100℃, and the temperature rises slowly. When the temperature reaches 130℃, the dehydration is stopped;

[0044] (4) Immediately after dehydration, add deionized water at a temperature of 90°C into the reactor, s...

Example Embodiment

[0047] Example 3

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

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

[0050] (3) After the heat preservation is completed, perform vacuum dehydration, and at the same time turn on the electronic grade deionized water vapor system, and pass the water vapor into the bottom of the reactor. The pressure of the water vapor is controlled at 0.60Mpa, and the pressure in the reactor is controlled at -0.08Mpa. The temperature of the internal materials is controlled at 50~100℃, and the temperature rises slowly. When the temperature reaches 120℃, the dehydration is stopped;

[0051] (4) Immediately after dehydration, add deionized water at a temperature of 90°C into the reactor, stir for 40 m...

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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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