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Production method for electronic-grade phenolic resin

A technology of phenolic resin and production method, applied in the direction of circuits, electrical components, electrical solid devices, etc., can solve the problems of high free phenol content, high impurity content of phenolic resin, poor electrical performance, etc., and achieve low free phenol content and impurity content less, good electrical performance

Inactive Publication Date: 2011-09-14
LIANYUNGANG ZHONGHE SCI & TECH +1
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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 many impurities, high free phenol content, high volatile content, and poor electrical properties, so it cannot be used as a curing agent for "epoxy molding compounds for packaging semiconductor devices and integrated circuits".

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 46g (37%) formaldehyde into a 1000ml reactor, then add 9g oxalic acid, add 550g phenol after stirring for 5 minutes, then start stirring and heat up, when the temperature reaches: 80°C, then continue dropwise within 1 hour 213g formaldehyde, heat preservation reaction after addition: 4 hours, then continuously add the remaining 46g formaldehyde dropwise within 30 minutes, heat preservation reaction for 30 minutes after addition, and the reaction ends. Then add 300g deionized water into the reactor, wash with water, vacuum dehydrate after washing 5 times, when the vacuum degree reaches: -0.09Mpa, when the temperature reaches: 100°C, steam distillation starts, and after 12 hours of distillation, the secondary dehydration, when Vacuum degree reaches: -0.1Mpa, temperature reaches: 120°C, then the reactants are continuously added to the thin-film evaporator, the internal pressure of the evaporator: -0.1Mpa, temperature: 160°C. After the material was added, the material i...

Embodiment 2

[0034] Add 50g (37%) formaldehyde into a 1000ml reactor, then add 9g oxalic acid, add 550g phenol after stirring for 5 minutes, then start stirring and heat up, when the temperature reaches: 80°C, then continue dropwise within 1 hour 233g formaldehyde, heat preservation reaction after addition: 4 hours, then continuously add the remaining 50g formaldehyde dropwise within 30 minutes, heat preservation reaction for 30 minutes after addition, and the reaction ends. Then add 300g deionized water into the reactor, wash with water, vacuum dehydrate after washing 5 times, when the vacuum degree reaches: -0.09Mpa, when the temperature reaches: 100°C, steam distillation starts, and after 12 hours of distillation, the secondary dehydration, when Vacuum degree reaches: -0.1Mpa, temperature reaches: 120°C, then the reactants are continuously added to the thin-film evaporator, the internal pressure of the evaporator: -0.1Mpa, temperature: 160°C. After the material was added, the material i...

Embodiment 3

[0036] Add 57g (37%) formaldehyde into a 1000ml reactor, then add 9g oxalic acid, add 550g phenol after stirring for 5 minutes, then start stirring and heat up, when the temperature reaches: 80°C, then continue dropwise within 1 hour 269g formaldehyde, heat preservation reaction after addition: 4 hours, then continuously add the remaining 57g formaldehyde dropwise within 30 minutes, heat preservation reaction for 30 minutes after addition, and the reaction ends. Then add 300g deionized water into the reactor, wash with water, vacuum dehydrate after washing 5 times, when the vacuum degree reaches: -0.09Mpa, when the temperature reaches: 100°C, steam distillation starts, and after 12 hours of distillation, the secondary dehydration, when Vacuum degree reaches: -0.1Mpa, temperature reaches: 120°C, then the reactants are continuously added to the thin-film evaporator, the internal pressure of the evaporator: -0.1Mpa, temperature: 160°C. After the material was added, the material i...

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PUM

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Abstract

The invention discloses a production method for electronic-grade phenolic resin. The production method includes the steps as follows: suctioning 10%-20% total amount of formaldehyde solution into a reaction kettle with a vacuum method, adding catalyst, stirring for 4-6 minutes, adding phenol, starting increasing temperature after charging materials, starting timing when the temperature achieves 70-100 DEG C, continuously dropping 65%-75% total amount of the formaldehyde solution within 1-2 hours, conducting temperature-insulation reaction for 1-10 hours after dropping is finished, then continuously and totally dropping the residual formaldehyde solution within 1-2 hours, and finishing reaction after conducting temperature-insulation reaction for 1-2 hours after dropping is finished. By adding formaldehyde solution in batches to react and by washing, vacuum dewatering, distillation, second vacuum dewatering and final refining, the electronic-grade phenolic resin with high purity can be prepared. The phenolic resin produced by the method is low in impurity content, free phenol content and volatile matter content, has good electrical property and can serve as a curing agent for 'epoxy moulding compounds for encapsulating semiconductor devices and integrated circuits'.

Description

technical field [0001] The invention relates to a production method of high-performance and high-purity electronic-grade phenolic resin used for semiconductor diodes, triodes and integrated circuit packaging materials, in particular to a production method of electronic-grade phenolic resin. Background technique [0002] Phenolic resin is widely used in rubber tires, grinding wheels, coatings, casting and aerospace fields due to its excellent heat resistance, electrical insulation, especially good flame retardancy and adhesion. As an epoxy resin curing agent, novolac resin can make the epoxy cured product have high heat resistance, water resistance, chemical resistance and mechanical strength, so it has been widely used in the fields of electronics and electrical appliances. [0003] Novolac resins are generally obtained by reacting phenols (phenol, cresol, xylenol, m-cresol, etc.) and aldehydes (formaldehyde, acetaldehyde, furfural, etc.) in the presence of acidic catalysts,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/10C08G59/62H01L23/29
Inventor 介振锁
Owner LIANYUNGANG ZHONGHE SCI & TECH
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