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Modified phenolic resin as well as preparation method and application thereof

A phenolic resin and modification technology, applied in the field of modified phenolic resin and its preparation, can solve the problems of reducing the thermal stability and flame retardant performance of the resin, decreasing the quality stability, complicated preparation process, etc. The effect of gel time and extension of dehydration time

Active Publication Date: 2020-10-09
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation process of the resin is relatively complicated. First, the solution of the thermosetting phenolic resin needs to be vacuum-dried at 40-80°C for 6-15 hours, and then polyurethane and boron phenolic resin are added to the dried resin and stirred for 5-30 minutes. , and finally react at 90-150°C for 10-90min to obtain ablation-resistant resin for resin film infiltration process
However, for thermosetting phenolic resin, its reactivity is high, even if it is stored at room temperature, its viscosity still increases rapidly, so the above-mentioned treatment at a high temperature for a long time increases the viscosity of the resin and narrows the processing window, resulting in resin The process performance of the resin will deteriorate, the quality stability will decrease, and the addition of thermoplastic polyurethane components will significantly reduce the thermal stability and flame retardancy of the resin, and there will be compatibility problems between components
[0006] In summary, most of the reported thermosetting phenolic resin films and their preparation methods currently use the technical solutions of adding polyvinyl alcohol, polyvinyl acetal, polyurethane and other aliphatic chain thermoplastic resins to improve the film-forming properties of phenolic resins. The common problem is that the thermal stability, carbon residue rate and flame retardancy of the resin are greatly reduced, and the processes used all involve high temperature treatment, which leads to narrowing of the processing window of the resin, and the preparation process is more cumbersome. Facilitate batch preparation

Method used

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  • Modified phenolic resin as well as preparation method and application thereof
  • Modified phenolic resin as well as preparation method and application thereof
  • Modified phenolic resin as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] The preparation of the RFI resin (RFI-10) of embodiment 1 thermoplastic phenolic resin consumption 10%

[0062] (1) Preheat the 30L reactor to 30°C, add 9.5 kg of melted phenol and 11.2 kg of 37.5% formaldehyde solution into the above reactor, stir evenly, add 95 grams of ammonia water, and heat up while stirring. When the temperature reaches 65°C, keep the reaction for 0.5 hours. At a speed of 2°C / min, the temperature of the reactor was raised to 80°C, and the reaction was further kept at 80±1°C for 2 hours. The temperature of the reactor was further raised to 95° C. at a rate of 2° C. / min, and the temperature was kept at 95±1° C. for 0.5 hours, and the addition and condensation reaction stage ended.

[0063] Cool the contents of the reactor to 50°C, and add hydrochloric acid to neutralize to pH 4.0.

[0064] Reheat the material. When the temperature of the material rises to 55°C, vacuum dehydration starts. When most of the water in the system is removed, the system ...

Embodiment 2

[0070] The preparation of the RFI resin (RFI-20) of embodiment 2 thermoplastic phenolic resin consumption 20%

[0071] (1) Preheat the 30L reactor to 30°C, add 9.5 kg of melted phenol and 8.8 kg of 37.5% formaldehyde solution into the above reactor, stir evenly, add 475 grams of barium hydroxide, and stir while stirring. The temperature was raised, and when the temperature reached 65° C., the reaction was kept for 0.5 hours. At a speed of 2°C / min, the temperature of the reactor was raised to 85°C, and the reaction was further kept at 80±1°C for 1 hour. The temperature of the reactor was further raised, and the temperature was raised to reflux at a rate of 2° C. / min, and the reaction was carried out for 1.0 hour, and the addition and condensation reaction stage ended.

[0072] Cool the contents of the reactor to 50°C, add phosphoric acid to neutralize to pH 7.5, and filter to remove the precipitate.

[0073] Reheat the material. When the temperature of the material rises to 5...

Embodiment 3

[0080]The preparation of the RFI resin (RFI-30) of embodiment 3 thermoplastic phenolic resin consumption 30%

[0081] (1) The reactor is preheated to 30°C, 7.6 kg of melted phenol, 545 g of m-cresol, 735.4 g of naphthol, 1.7 kg of 3-phenylphenol and 20 kg of 37.5% formaldehyde solution are added to the above reaction In the kettle, after stirring evenly, add 317.7 grams of sodium hydroxide, stir while raising the temperature, when the temperature reaches 65°C, keep the temperature for 1 hour. At a speed of 2°C / min, the temperature of the reactor was raised to 80°C, and the reaction was further kept at 80±1°C for 1 hour. The temperature of the reactor was further raised to 85±1° C. at a rate of 2° C. / min, and reacted for 2.0 hours. The addition and condensation reaction stage ended.

[0082] Cool the contents of the reactor to 50°C, and add hydrochloric acid to neutralize to pH 5.0.

[0083] Reheat the material. When the temperature of the material rises to 55°C, start vacuum...

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Abstract

The invention relates to thermosetting phenolic resin as well as a preparation method and application thereof. The phenolic resin is prepared by reaction of thermosetting phenolic resin and thermoplastic phenolic resin, the contradiction between high viscosity of traditional phenolic resin and a narrow process window is solved, and the advantages of good heat resistance and high carbon residue rate of phenolic resin are maintained. The thermosetting phenolic resin suitable for a resin film infiltration process (RFI) provided by the invention is low in cost, simple in preparation method, high in operability and convenient for large-scale preparation. The phenolic resin has excellent forming and curing process performance, heat resistance and carbon residue performance, is good high-performance composite material matrix resin, has a good application prospect in the high-tech fields of thermal protection and the like, can be used for preparing phenolic resin flame-retardant prepreg clothby a dry method, and has a great application potential in the fields of flame-retardant and fireproof interior materials of large airplanes and high-speed trains and the like.

Description

technical field [0001] The invention belongs to the field of phenolic resin preparation, and in particular relates to a modified phenolic resin and its preparation method and application. Background technique [0002] Phenolic resin is a kind of polymer material prepared by the polycondensation reaction between phenols and aldehydes, because it has a series of excellent properties, such as high temperature resistance, high carbon residue, excellent dimensional stability, flame retardancy and low smoke Therefore, it is widely used in construction (thermal insulation materials), transportation (large aircraft, high-speed train interior parts), metallurgy (refractory materials) and other fields. At the same time, phenolic resin is also the most commonly used burning material in high-tech fields. Corrosion and heat-resistant composite matrix resin. [0003] At present, the manufacture of phenolic resin-based composite materials mostly adopts a solution (about 60% concentration)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L61/10C08L61/06
CPCC08L61/06C08L2205/025
Inventor 罗振华杜有培赵彤李昊王倩
Owner INST OF CHEM CHINESE ACAD OF SCI
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