Industrial production method of high-purity linear phenolic resin

A novolac resin and production method technology, which is applied in the refining process field of novolac resin, can solve the problems of not being able to meet the purity requirements of novolac resin, difficult engineering scale-up and continuous production, and vague description, so as to reduce the generation of waste water Quantity, material residence time is short, the effect of improving efficiency

Inactive Publication Date: 2019-02-22
SHANDONG TIANCHENG CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the existing production technology of novolac resin in China, the resin is mostly purified through raw material synthesis, steam distillation, hot filtration and vacuum drying, but the process is complicated, inefficient, time-consuming and energy-consuming, difficult to scale up...

Method used

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  • Industrial production method of high-purity linear phenolic resin

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Embodiment 1

[0035] An industrial production method of high-purity novolac resin, the steps are as follows: (1) Measure 108kg of phenol through a mass flow meter, put the delivery pump into the reaction kettle, start stirring at a speed of 60 rpm, and then add 1kg For oxalic acid, when the temperature was raised to 90° C., 73 kg of formaldehyde solution with a mass fraction of 37% was added dropwise to the reactor by a mass flow meter, and the titration was complete within 2 hours;

[0036] (2) After adding formaldehyde aqueous solution dropwise, keep the reaction at 100 ℃ for 6 hours, and then add oxalic acid until the pH of the mixed solution in the reaction kettle is 4~6;

[0037] (3) Continue to add 100Kg of solvent to the reaction kettle, and maintain the temperature of the kettle material at 79~81°C;

[0038] (4) Transfer all the materials in the reaction kettle in step (3) to the extraction kettle, add 70kg of water at 70~90°C to the extraction kettle, stir and wash for 30 minutes, ...

Embodiment 2

[0050] An industrial production method of high-purity novolac resin, the steps are as follows: (1) Measure 94kg of phenol through a mass flow meter, put the delivery pump into the reaction kettle, start stirring at a speed of 70 rpm, and then add 1kg For oxalic acid, when the temperature was raised to 90° C., 68 kg of formaldehyde solution with a mass fraction of 37% was added dropwise to the reactor by a mass flow meter, and the titration was complete within 2 hours;

[0051] (2) After adding formaldehyde aqueous solution dropwise, keep the reaction at 95 ℃ for 8 hours, and then add oxalic acid until the pH of the mixed solution in the reaction kettle is 4~6;

[0052] (3) Continue to add 80kg of solvent to the reaction kettle, and maintain the temperature of the kettle material at 80°C;

[0053] (4) Transfer all the materials in the reaction kettle in step (3) into the extraction kettle, add 70kg of water at 90°C to the extraction kettle, stir and wash with water for 30 minut...

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Abstract

The invention relates to the technical field of polymer synthesis of phenolic resin, in particular to a refinement process of linear phenolic resin. The process comprises the steps as follows: (1) putting phenol in a reactor, adding oxalic acid, heating the reactor to 80-100 DEG C, and dropwise adding formalin to the reactor; (2) after dropwise adding the formalin, keeping the temperature, and adding oxalic acid until the pH of the mixed solution in the reactor is 4-6; (3) adding a solvent to the reactor continuously; (4) transferring all materials in the reactor into an extraction kettle, adding water to the extraction kettle for extraction, and separating a water phase; (5) repeating washing operation in step (4) until the pH value of the materials is 6-7 to obtain a crude phenolic resinsolution; (6) transferring the crude phenolic resin solution into a dehydration kettle, and removing residual water under negative pressure; (7) coarsely removing the solvent and small-molecular impurities out of the phenolic resin by a multistage falling-film evaporator, and refining the phenolic resin by a multistage wiped-film evaporator group; (8) granulating the phenolic resin by a drum granulator to obtain a high-purity linear phenolic resin product.

Description

technical field [0001] The invention relates to the technical field of phenolic resin polymer synthesis, in particular to a refining process of novolac resin. Background technique [0002] Integrated circuit packaging is an important part of the integrated circuit industry chain. Its role is to undertake the process of integrated circuit manufacturing, protect the chip and provide signal transmission between the chip and other system components. With the high integration of integrated circuits, the increase of chip and packaging area, and the thinning of packaging layers, higher and more comprehensive requirements are put forward for packaging materials. [0003] Novolac epoxy resin is the main material of integrated circuit packaging, because it needs to be in direct contact with the etched very fine silicon chip and aluminum leads during packaging, so the purity of novolac epoxy resin is highly required. [0004] Novolak resin is the main raw material for preparing novola...

Claims

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Application Information

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IPC IPC(8): C08G8/32
CPCC08G8/32
Inventor 朱年德郭海东赵福举张银广程飞杨存新
Owner SHANDONG TIANCHENG CHEM CO LTD
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