Preparing method for ablation-resisting boron-modified thermoplastic phenolic resin

A phenolic resin and boron modification technology, which is applied in the field of phenolic resin preparation, can solve the problems of increased production cost, low product reliability and high curing temperature, and achieves low volatile content, good ablation performance and mechanical properties, high Effect of carbon residue rate

Inactive Publication Date: 2016-02-10
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthesis process of boron-modified phenolic resin is mainly used in thermosetting phenolic resin, but the preparation of C / C composite materials by domestic thermosetting phenolic resin still has the problems of high curing temperature, high void ratio and low product reliability. People began to use boron-containing Compound modified thermoplastic phenolic resin
In the research of boron-modified thermoplastic phenolic resins, toluene is usually used as a dehydrating agent for the reaction, or solvents are used to extract unreacted small molecules and then dehydrated under reduced pressure to obtain boron-containing thermoplastic phenolic resins. The use of solvents increases production costs and exists Environmental pollution and other issues

Method used

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  • Preparing method for ablation-resisting boron-modified thermoplastic phenolic resin
  • Preparing method for ablation-resisting boron-modified thermoplastic phenolic resin
  • Preparing method for ablation-resisting boron-modified thermoplastic phenolic resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] raw material:

[0024]

[0025] Process:

[0026] Pre-raise the temperature of the oil bath to 80°C, add phenol and zinc acetate in sequence, keep stirring for 5-10 minutes to make the mixture even, and then add a certain amount of paraformaldehyde. The temperature of the oil bath was raised to 100°C, and the reaction was carried out for 8-12 hours. Then add sodium hydroxide aqueous solution to make the mixture uniform, then slowly add phenylboronic acid and then raise the temperature to 140°C, and react for 2h. Raise the temperature to 150°C, carry out dehydration under reduced pressure, and last for about 20 minutes at -0.06~-0.09MPa, and determine the reaction end point according to the viscosity of the tree. A yellow or reddish-brown solid resin is finally obtained.

[0027] The performance index of the prepared resin:

[0028] Cured resin carbon residue rate (800 ° C, nitrogen atmosphere): 69% to 71%

[0029] Softening point: 98~103℃

[0030] Free phenol: ...

Embodiment 2

[0033] raw material:

[0034]

[0035] Process:

[0036] Pre-raise the temperature of the oil bath to 80°C, add phenol and acetic acid in sequence, keep stirring for 5-10 minutes to make the mixture even, and then add a certain amount of formaldehyde aqueous solution. The temperature of the oil bath was raised to 100°C, and the reaction was carried out for 8-12 hours. Then phosphoric acid was added to make the mixture uniform, and then phenylboronic acid was added slowly, and the reaction was 3h. Lower the temperature to 80°C, rinse the solution with distilled water, then raise the temperature to 100°C, and carry out dehydration condensation under reduced pressure, at -0.06~-0.09MPa for about 45min, and determine the reaction end point according to the tree viscosity. A reddish-brown solid resin was finally obtained.

[0037] The performance index of the prepared resin:

[0038] Cured resin carbon residue rate (800°C, nitrogen atmosphere): 64% to 66%

[0039] Softening...

Embodiment 3

[0043]

[0044] Process:

[0045] Pre-raise the temperature of the oil bath to 80°C, add phenol and oxalic acid in sequence, keep stirring for 5-10 minutes to make the mixture even, and then add a certain amount of paraformaldehyde. Raise the temperature of the oil bath to 100°C, carry out the reaction for 8-12 hours, and distill under reduced pressure to remove part of the water and small molecule volatiles. Then add sodium hydroxide aqueous solution to mix evenly, then slowly add 4-hydroxymethylbenzeneboronic acid and then heat up to 150°C, after 2 hours of reaction, carry out dehydration under reduced pressure, at -0.06~-0.09MPa for about 10min, specifically determined according to the viscosity of the tree end point of the reaction. A brown or reddish-brown solid resin is finally obtained.

[0046] The performance index of the prepared resin:

[0047] Cured resin carbon residue rate (800°C, nitrogen atmosphere): 66% to 68%

[0048] Softening point: 90~95℃

[0049] ...

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Abstract

The invention relates to a preparing method for ablation-resisting boron-modified thermoplastic phenolic resin. For solving the problems that at present, boron-modified phenolic resin is complex in production process and pollutes environment, and an obtained composite material product is high in porosity, solvent is not used in the synthetic process, an effective catalyst is adopted to make a boron-containing compound react fully, a resin structure is connected in a copolymerization mode, the suitable reaction temperature and the suitable time are controlled, and the boron-containing thermoplastic phenolic resin which is high in molecular weight, low in volatile content and low in curing volume shrinkage rate is synthesized, wherein the composite material of the resin is high in ablation performance and mechanical property. While the good heat resistance and ablation resistance of the boron-containing compound are brought into full play, the manufacturability and the mechanical property of the boron-containing phenolic resin are improved, and it is the research core to meet the requirement of aerospace development with the thermoplastic phenolic resin having a high carbon yield, a suitable softening point and good manufacturability.

Description

technical field [0001] The invention belongs to the preparation method of phenolic resin, in particular to a preparation method of ablation-resistant boron modified thermoplastic phenolic resin, which is a kind of boron-containing thermoplastic phenolic resin with excellent manufacturability, high softening point and high residual carbon rate. method. Background technique [0002] Phenolic resin is the earliest and still widely used ablation-resistant composite material matrix. Phenolic resin has excellent heat resistance and ablation performance, and is widely used in the aerospace field. Under the scouring of high-temperature and high-speed airflow, phenolic resin sacrifices itself to insulate heat to ensure the normal operation of the instrument as a whole. However, the molecular weight of traditional thermosetting phenolic resin is small, and the cured resin has a large number of ether bonds (-O-) and methylene (-CH 2 -) exists in the resin, small molecular compounds ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/32C08G8/10
Inventor 陈立新冯俊君衡杰
Owner NORTHWESTERN POLYTECHNICAL UNIV
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