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A kind of modified phenolic resin and its preparation method and application

A phenolic resin and modification technology, applied in the field of modified phenolic resin and its preparation, can solve the problem of reducing the thermal stability, residual carbon rate and flame retardant performance of the resin, reducing the thermal stability and flame retardant performance of the resin, and reducing the resin process performance. Deterioration and other problems, to shorten the gel time, increase the absolute molecular weight, and improve the effect of film-forming

Active Publication Date: 2021-09-28
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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  • A kind of modified phenolic resin and its preparation method and application
  • A kind of modified phenolic resin and its preparation method and application
  • A kind of modified phenolic resin and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Example 1 Preparation of RFI resin (RFI-10) with a thermoplastic phenolic resin content of 10%

[0062] (1) 30L reactor is preheated to 30 ℃, 9.5 kilograms of melted phenol and 11.2 kilograms of 37.5% aqueous formaldehyde are added to above-mentioned reactor, after stirring, add 95 grams of ammoniacal liquor, while stirring, heat up, When the temperature reached 65°C, the reaction was maintained 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 incubated at 80±1°C for 2 hours. The temperature of the reaction kettle was further heated up to 95°C at a rate of 2°C / min, and the reaction was kept at 95±1°C for 0.5 hours, and the addition condensation reaction stage was completed.

[0063] Cool the reactor material to 50°C, 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 begins. After most of the water in the...

Embodiment 2

[0070] Example 2 Preparation of RFI resin (RFI-20) with a thermoplastic phenolic resin content of 20%

[0071] (1) 30L reactor is preheated to 30 ℃, 9.5 kilograms of phenol after melting and 8.8 kilograms of 37.5% formaldehyde solution are added in above-mentioned reactor, after stirring, add 475 grams of barium hydroxide, while stirring, The temperature was raised, and when the temperature reached 65°C, the reaction was maintained 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 incubated at 80±1°C for 1 hour. The temperature of the reaction kettle was further heated up to reflux at a rate of 2°C / min, and the reaction was carried out for 1.0 hours, and the addition condensation reaction stage was completed.

[0072] Cool the reactor material 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...

Embodiment 3

[0080]Example 3 Preparation of RFI resin (RFI-30) with a thermoplastic phenolic resin content of 30%

[0081] (1) reactor is preheated to 30 ℃, 7.6 kilograms of phenol after melting, 545 grams of m-cresol, 735.4 grams of naphthol, 1.7 kilograms of 3-phenylphenol and 20 kilograms of aqueous formaldehyde solution of 37.5% are added to above-mentioned reaction In the kettle, after stirring evenly, 317.7 g of sodium hydroxide was added, and the temperature was raised while stirring. When the temperature reached 65° C., the reaction was incubated 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 incubated at 80±1°C for 1 hour. The temperature of the reactor was further heated up to 85±1°C at a rate of 2°C / min, and the reaction was carried out for 2.0 hours, and the addition condensation reaction stage was completed.

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

[0083] R...

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Abstract

The invention relates to a thermosetting phenolic resin and its preparation method and application. The phenolic resin of the present invention is prepared by reacting a thermosetting phenolic resin and a thermoplastic phenolic resin, which solves the contradiction between the high viscosity of the traditional phenolic resin and the narrow process window, and maintains the advantages of good heat resistance and high carbon residue rate of the phenolic resin. The thermosetting phenolic resin suitable for the resin film infiltration process (RFI) proposed by the invention has low cost, simple preparation method, strong operability, and is convenient for large-scale preparation. The phenolic resin has excellent molding and curing process performance, heat resistance and carbon residue performance. It is an excellent high-performance composite material matrix resin and has good application prospects in high-tech fields such as heat protection. At the same time, the resin It can be used to prepare phenolic resin flame-retardant prepreg by dry method, and has great application potential in the fields of flame-retardant and fire-resistant interior materials for large aircraft and high-speed trains.

Description

technical field [0001] The invention belongs to the field of phenolic resin preparation, in particular to a modified phenolic resin and a preparation method and application thereof. Background technique [0002] Phenolic resin is a kind of polymer material prepared by the polycondensation reaction between phenols and aldehydes, due to its excellent properties such as high temperature resistance, high carbon residue, excellent dimensional stability, flame retardant properties 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. 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) impregnation method to prepare a prepreg, and then a molding process of molding or winding. The main defects of t...

Claims

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Application Information

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Patent Type & Authority Patents(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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