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Synthesis method of rubber modified solid thermosetting phenolic resin

A technology of rubber modification and phenolic resin, applied in the field of phenolic resin, can solve the problems of shortened polymerization speed of phenolic resin, poor compatibility and stability of phenolic resin and rubber, no improvement in heat resistance of phenolic resin, etc. The effect of good heat resistance and flexibility, good compatibility and stability, and excellent performance reliability

Active Publication Date: 2020-11-24
ZHEJIANG HANGMO SYNTHETIC MATERIAL +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1. Rubber and phenolic resin are physically mixed. Since the phenolic resin has not undergone grafting reaction with rubber, the compatibility and stability of phenolic resin and rubber are poor.
In addition, since the rubber did not participate in the reaction, the degree of crosslinking of the phenolic resin did not increase, and the flexibility of the phenolic resin improved, but the heat resistance of the phenolic resin did not improve.
[0004] 2. The acid-catalyzed thermoplastic phenolic resin needs to be added with urotropine during curing. The ammonia gas released by the phenolic resin during the curing process will corrode the metal parts in the molding compound and affect the performance of the molding compound.
[0005] 3. Rubber and phenolic resin are chemically grafted, so that the rubber-modified thermoplastic phenolic resin has a micro-crosslinked structure. Although this structure can increase the degree of crosslinking of the phenolic resin and improve the heat resistance of the phenolic resin, the polymerization speed of the phenolic resin Significantly shorter, resulting in limited application of phenolic resins

Method used

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  • Synthesis method of rubber modified solid thermosetting phenolic resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Put 1000kg of preheated and melted phenol into the high-level metering tank with a special pump, and then add 50kg of styrene-butadiene rubber with a number average molecular weight of 45,000 and 5kg of p-toluenesulfonic acid into the reactor, and heat it up to 160°C for heat preservation. After reacting for 3 hours and the temperature dropped to 80°C, 1.25 kg of sodium hydroxide was added to adjust the pH to 3-4. Then add 1500kg of formaldehyde aqueous solution with a mass fraction of 37%, 0.5kg of catalyst barium chloride, raise the temperature to 100°C, and keep it under reflux for 6 hours. After the heat preservation is over, dehydrate at normal pressure to 120°C, vacuum dehydrate to 130°C (vacuum degree is less than 0.095Mpa), and when the polymerization speed of the phenolic resin is detected to be 105-135s, stop the reaction, release the product, and obtain a light yellow solid 1030kg after cooling .

Embodiment 2

[0045] Put 1000kg of preheated and melted phenol into the high-level metering tank with a special pump, and measure it into the reactor, then add 100kg of nitrile rubber with a number average molecular weight of 4000, and 1kg of concentrated sulfuric acid into the reactor, heat up to 80°C and keep it warm for 5 hour, after the insulation finishes, add sodium hydroxide 0.8kg, adjust pH to 3-4. Then add 1350kg of formaldehyde solution with a mass fraction of 37%, 10kg of catalyst calcium acetate, raise the temperature to 100°C, and keep it under reflux for 3 hours. After the heat preservation is over, the dehydration temperature under normal pressure reaches 120°C, vacuum dehydration reaches 130°C (vacuum degree is less than 0.095Mpa), and when the polymerization speed of the phenolic resin is detected to be 105-135s, the reaction is stopped, the product is released, and 1270kg of a light yellow solid is obtained after cooling.

Embodiment 3

[0047] Put 1000kg of preheated and molten phenol into the high-level metering tank with a special pump, and then add 200kg of butyl rubber with a number-average molecular weight of 13,000 and 15kg of p-toluenesulfonic acid into the reactor, and heat it up to 110°C for heat preservation. React for 4 hours. After the heat preservation is completed, add 2.5 kg of sodium hydroxide to adjust the pH to 3-4. Then add 200kg of paraformaldehyde, 400kg of formaldehyde solution with a mass fraction of 37%, 50kg of catalyst zinc acetate, raise the temperature to 100°C, and keep it under reflux for 2 hours. After the heat preservation is over, dehydrate at normal pressure to 120°C, and vacuum dehydrate to 130°C (vacuum degree less than 0.095Mpa). When the polymerization speed of the phenolic resin is detected to be 105-135s, the reaction is stopped, and the product is released. After cooling, 1380Kg of a light yellow solid is obtained. .

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Abstract

The invention discloses a synthesis method of rubber modified solid thermosetting phenolic resin. The method comprises the following steps of 1, reacting phenol and rubber under the action of an acidcatalyst to generate rubber modified phenol; and 2, reacting the rubber modified phenol with excessive formaldehyde by using divalent metal salt as a catalyst, and sequentially carrying out normal-pressure dehydration, vacuum phenol removal and cooling after the reaction is ended, thereby obtaining the solid thermosetting phenolic resin. According to the synthesis method of the rubber modified solid thermosetting phenolic resin, the heat resistance and flexibility of the phenolic resin can be remarkably improved, the process is easy to control, and the gel risk cannot be found.

Description

technical field [0001] The present application relates to the technical field of phenolic resins, in particular to a synthetic method of a rubber-modified solid thermosetting phenolic resin. Background technique [0002] In the prior art, the rubber modified phenolic resin mainly has the following problems: [0003] 1. Rubber and phenolic resin are physically mixed. Since the phenolic resin has not undergone grafting reaction with rubber, the compatibility and stability of phenolic resin and rubber are poor. In addition, since the rubber did not participate in the reaction, the degree of crosslinking of the phenolic resin did not increase, and the flexibility of the phenolic resin improved, but the heat resistance of the phenolic resin did not improve. [0004] 2. The acid-catalyzed thermoplastic phenolic resin needs to be added with urotropine during curing. The ammonia released by the phenolic resin during the curing process will corrode the metal parts in the molding com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28
CPCC08G8/28
Inventor 孟付良周大鹏陈建国陈利王松松徐利彬赵昕雅林华胡翔玮乔坤沈琛聪
Owner ZHEJIANG HANGMO SYNTHETIC MATERIAL
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