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A kind of boronization addition curing type phenolic resin and its preparation method and application

An addition curing type, phenolic resin technology, applied in the field of phenolic resin preparation, can solve problems such as difficult to ensure uniform phenolic resin, increase in viscosity of phenolic resin, agglomeration, etc., achieve excellent molding and curing process performance, improve oxidation resistance, excellent Solubility effect

Active Publication Date: 2019-03-08
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 addition of boron carbide powder will lead to an increase in the viscosity of the phenolic resin, making it prone to agglomeration problems during the blending process, making it difficult to ensure the uniformity of the phenolic resin, and problems such as delamination will occur after long-term storage. The existence of the above shortcomings limits the Applications of the resin

Method used

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  • A kind of boronization addition curing type phenolic resin and its preparation method and application
  • A kind of boronization addition curing type phenolic resin and its preparation method and application
  • A kind of boronization addition curing type phenolic resin and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1 degree of etherification is the preparation of 20% boronization addition curing type phenolic resin (BPN20):

[0045] (1) Put 33.68 grams of 4-hydroxyphenylboronic acid, 11.20 grams of 37.5% formaldehyde solution, and 100 mL of tetrahydrofuran into a 500 mL four-necked flask equipped with a stirrer, a thermometer, a condenser and a dropping funnel, and stir until the monomer is completely dissolved . While stirring, the temperature was raised, and when the temperature reached 60°C, 0.20 g of concentrated hydrochloric acid was added to the system, and the temperature was continued to rise to 75°C, and the reaction was maintained for 8 hours. After the reaction, remove the solvent by rotary evaporation, then dissolve the resin in an appropriate amount of ethyl acetate, and then add distilled water to wash until the water layer is neutral, then let go of the water layer, and finally remove the ethyl acetate by rotary evaporation to obtain boronized thermoplast...

Embodiment 2

[0047] Embodiment 2 The degree of etherification is the preparation of 40% boronization addition curing type phenolic resin (BPN40):

[0048] (1) 16.80 grams of 3-hydroxyphenylboronic acid, 16.80 grams of 4-hydroxyphenylboronic acid, 12.8 grams of 37.5% formaldehyde solution, and 100 mL of tetrahydrofuran were placed in a 250 mL four-necked flask equipped with a stirrer, a thermometer, a condenser tube and a dropping funnel In, stir until the monomer is completely dissolved. While stirring, the temperature was raised, and when the temperature reached 60°C, 0.50 g of oxalic acid was added to the system, and the temperature was continued to rise to 85°C, and the reaction was kept for 6 hours. After the reaction, remove the solvent by rotary evaporation, then dissolve the resin in an appropriate amount of ethyl acetate, and then add distilled water to wash until the water layer is neutral, then release the water layer, and remove the ethyl acetate by rotary evaporation to obtain ...

Embodiment 3

[0050] Embodiment 3 The degree of etherification is the preparation of boronation addition curing type phenolic resin (BPN60) of 60%

[0051] (1) 16.80 grams of 4-hydroxyphenylboronic acid, 6.80 grams of 37.5% formaldehyde solution, and 50 mL of dioxane are placed in a 100 mL four-necked bottle equipped with a stirrer, a thermometer, a condenser tube and a dropping funnel, and stirred until The monomer is completely dissolved. While stirring, the temperature was raised, and when the temperature reached 60°C, 0.51 g of p-toluenesulfonic acid was added to the system, and the temperature was continued to rise to 90°C, and the reaction was kept for 4 hours. After the reaction, remove the solvent by rotary evaporation, then dissolve the resin in an appropriate amount of ethyl acetate, and then add distilled water to wash until the water layer is neutral, then let go of the water layer, and finally remove the ethyl acetate by rotary evaporation to obtain boronized thermoplastic 16 ...

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Abstract

The invention belongs to the field of preparation of phenolic resin, and in particular relates to boron hybridization addition curing type phenolic resin. Molecular structures of the phenolic resin are shown as formulas (I ) and (II) in the description. The invention also relates to a preparation method and application of the boron hybridization addition curing type phenolic resin. The boron hybridization addition curing type phenolic resin disclosed by the invention has excellent forming and curing process performance, heat resistance and residual carbon performance, is excellent high-performance composite material matrix resin with high temperature resistance and ablation resistance, and can be applied to the field of high-performance composite material matrix resin with high temperature resistance, oxidation resistance and easiness in forming, i.e., the boron hybridization addition curing type phenolic resin has a good application prospect in the fields such as ablation heat prevention, refractory materials, precoated sand and the like.

Description

technical field [0001] The invention belongs to the field of phenolic resin preparation, and in particular relates to a boronation addition curing type 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. However, a large number of phenolic hydroxyl groups contained in the molecular structure of phenolic resin l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/36C08G8/08C08L61/14
CPCC08G8/08C08G8/36C08L61/14C08L2201/02C08L2201/08
Inventor 罗振华
Owner INST OF CHEM CHINESE ACAD OF SCI
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