High-performance high-temperature-resistant resin material as well as preparation method and application thereof

Abstract

The invention relates to the technical field of high polymer materials, in particular to a high-performance high-temperature-resistant resin material and a preparation method and application thereof.The preparation method comprises the steps that a biomass material is modified through epichlorohydrin, active groups are introduced, and a modified biomass material is obtained; carrying out full copolymerization reaction on the modified biomass material, dianhydride and diamine to obtain a copolymer; fully mixing the copolymer with the curing agent and the filler, and curing; and cooling to room temperature to obtain the high-performance high-temperature-resistant resin material. According to the technical scheme, biomass materials serve as raw materials and are wide in source, and the preparation method is low in processing temperature and low in cost and cannot generate secondary pollution to the environment; a certain proportion of filler is added for curing, so that the high-temperature resistance of the resin material is further improved, and the application of the resin material in the fields of aerospace, electronic packaging and mold manufacturing is met.

Description

Technical Field

[0001] The present invention relates to the technical field of polymer materials, and particularly to a high-performance high-temperature resistant resin material, a preparation method thereof, and an application thereof. Background Art

[0002] With the rapid development of fields such as aerospace, electronic information, and rail transit, the requirements for material properties are becoming increasingly stringent, especially the demand for materials that can still maintain excellent properties in high-temperature environments is becoming increasingly urgent. High-temperature resistant resin-based composites have shown great application potential in the above fields due to their advantages such as light weight, high strength, corrosion resistance, and strong designability, and have become a research hotspot in the field of materials science.

[0003] Currently, commonly used high-temperature resistant resins mainly include: polyimide (PI) resin, bismaleimide (BMI) resin, cyanate ester (CE) resin, benzoxazine (BOZ) resin, etc. Although the existing high-temperature resistant resins have certain heat resistance, they have disadvantages such as high processing temperature, high cost, and easy to cause secondary pollution to the environment. In view of this, we propose a high-performance high-temperature resistant resin material, a preparation method thereof, and an application thereof. Summary of the Invention

[0004] The purpose of the present invention is to provide a high-performance high-temperature resistant resin material, a preparation method thereof, and an application thereof, so as to solve the problems raised in the above background art.

[0005] To achieve the above purpose, the present invention provides the following technical solutions:

[0006] A preparation method of a high-performance high-temperature resistant resin material, comprising the following steps:

[0007] Step 1: Modify the biomass material with epichlorohydrin to introduce active groups to obtain a modified biomass material;

[0008] Step 2: Subject the modified biomass material to a full copolymerization reaction with dianhydride and diamine to obtain a copolymer;

[0009] Step 3: Fully mix the copolymer with a curing agent and a filler, and cure;

[0010] Step 4: Cool to room temperature to obtain a high-performance high-temperature resistant resin material.

[0011] Preferably, the said Step 1 includes the following steps:

[0012] Step 11: Dissolve the biomass material in a dilute acid solution to obtain a transparent solution;

[0013] Step 12: Add an alkaline reagent to the above transparent solution to adjust the pH of the solution to 8-10;

[0014] Step 13: Add epichlorohydrin and a catalyst to Step 12, and stir well. The molar ratio of epichlorohydrin, catalyst to the biomass material is 1 - 5: 0.05 - 0.5: 1;

[0015] Step 14: Heat to 50 - 70 °C and stir for reaction for 4 - 8 hours;

[0016] Step 15: Cool to room temperature and adjust the pH to neutral with dilute acid;

[0017] Step 16: Pour the reaction solution in Step 15 into ethanol or acetone for precipitation, filter and wash the precipitate;

[0018] Step 17: Vacuum dry the precipitate in Step 16 at 40 - 60 °C for 6 - 10 hours, and obtain the modified biomass material after cooling.

[0019] Preferably, the biomass material is one or more of lignin, cellulose, hemicellulose, chitosan, starch.

[0020] Preferably, the dilute acid solution is an acetic acid aqueous solution with a mass fraction of 0.2% - 5%, and the catalyst is tetrabutylammonium bromide.

[0021] Preferably, the volume ratio of ethanol or acetone to the reaction solution is 3 - 6: 1.

[0022] Preferably, Step 2 includes the following steps:

[0023] Step 21: Dissolve the modified biomass material, dianhydride, and diamine in an organic solvent, stir well, heat to 70 - 90 °C, and carry out a prepolymerization reaction for 2 - 6 hours under an inert atmosphere;

[0024] Step 22: Heat to 150 - 300 °C and react for 1 - 4 hours under an inert atmosphere;

[0025] Step 23: Wash the reaction product in Step 22 several times with the same polar solvent used in Step 21;

[0026] Step 24: Vacuum dry at 60 - 80 °C for 6 - 10 hours, and obtain the copolymer after cooling.

[0027] Preferably, the dianhydride is any one of pyromellitic dianhydride, biphenyltetracarboxylic dianhydride, hexafluorodiacid dianhydride, the diamine is any one of 4,4'-diaminodiphenyl ether, p-phenylenediamine, 4,4'-diaminodiphenylmethane, the molar ratio of dianhydride to diamine is 1: 1, the mass fraction of the modified biomass material is 10% - 30% of the total mass of the modified biomass material, dianhydride, and diamine, and the organic solvent is any one of N-methylpyrrolidone, dimethylformamide, dimethylacetamide, dimethyl sulfoxide, acetonitrile.

[0028] Preferably, the curing agent is any one of diethylenetriamine, m-phenylenediamine, and hexahydrophthalic anhydride, the filler is any one of montmorillonite, silica, alumina, boron nitride, silicon carbide, and zirconia, the mass ratio of the copolymer to the curing agent and the filler is 1:0.05 - 0.1:0.2 - 0.5, and the curing conditions are: pre-curing at 80 - 100 °C for 1 - 2 hours first, and then post-curing at 150 - 200 °C for 2 - 4 hours.

[0029] A high-performance high-temperature resistant resin material is prepared by the above preparation method.

[0030] The application of the high-performance high-temperature resistant resin material described in the present invention in the fields of aerospace, electronic packaging, and mold manufacturing.

[0031] Compared with the prior art, the beneficial effects of the present invention are:

[0032] The preparation method of the high-performance high-temperature resistant resin material includes: modifying the biomass material with epichlorohydrin to introduce active groups to obtain a modified biomass material; fully copolymerizing the modified biomass material with dianhydride and diamine to obtain a copolymer; fully mixing the copolymer with a curing agent and a filler and curing; cooling to room temperature to obtain a high-performance high-temperature resistant resin material. This technical solution uses biomass materials as raw materials, which are widely sourced. The preparation method has a low processing temperature, low cost, and does not cause secondary pollution to the environment; by adding a certain proportion of filler for curing, the high-temperature resistance of the resin material is further improved to meet its application in the fields of aerospace, electronic packaging, and mold manufacturing. Specific embodiments

[0033] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0034] In order to obtain a high-performance high-temperature resistant resin material, the inventor has conducted a large number of experimental studies and obtained the following technical solutions for the preparation of a high-performance high-temperature resistant resin material:

[0035] A preparation method of a high-performance high-temperature resistant resin material includes the following steps:

[0036] Step 1, modifying the biomass material with epichlorohydrin to introduce active groups to obtain a modified biomass material;

[0037] Step 2, fully copolymerizing the modified biomass material with dianhydride and diamine to obtain a copolymer;

[0038] Step 3: Thoroughly mix the copolymer with a curing agent and a filler, and cure them.

[0039] Step 4: Cool to room temperature to obtain a high-performance high-temperature resistant resin material.

[0040] Biomass materials are derived from biological resources such as plants and animals, and can be continuously obtained through natural cycles or artificial cultivation. They are renewable, environmentally friendly, and diverse, which can reduce the dependence on non-renewable resources, and reduce the pressure of environmental pollution and waste treatment. This technical solution uses biomass materials as raw materials. Biomass materials have rich functional groups, and their aromatic structure can improve the heat resistance of the resin. Epichlorohydrin is used to modify it to introduce active groups, and copolymerization reactions occur with dianhydride and diamine to introduce high-temperature resistant groups and improve its high-temperature resistance performance; and it is mixed and cured with high-temperature resistant fillers to further improve its high-temperature resistance performance. This technical solution can not only reduce the preparation cost of high-temperature resistant resin materials, but also be environmentally friendly and will not cause secondary pollution.

[0041] Preferably, Step 1 includes the following steps:

[0042] Step 11: Dissolve the biomass material in a dilute acid solution to obtain a transparent solution.

[0043] Step 12: Add an alkaline reagent to the above transparent solution to adjust the pH of the solution to 8 - 10.

[0044] Step 13: Add epichlorohydrin and a catalyst to Step 12, and stir evenly. The molar ratio of epichlorohydrin, the catalyst to the biomass material is 1 - 5:0.05 - 0.5:1.

[0045] Step 14: Heat to 50 - 70 °C and stir and react for 4 - 8 hours.

[0046] Step 15: Cool to room temperature and adjust the pH to neutral with dilute acid.

[0047] Step 16: Pour the reaction solution in Step 15 into ethanol or acetone for precipitation, and filter and wash the precipitate.

[0048] Step 17: Vacuum dry the precipitate in Step 16 at 40 - 60 °C for 6 - 10 hours, and cool to obtain a modified biomass material.

[0049] Preferably, the biomass material is one or more of lignin, cellulose, hemicellulose, chitosan, and starch.

[0050] Preferably, the dilute acid solution is an acetic acid aqueous solution with a mass fraction of 0.2% - 5%, and the catalyst is tetrabutylammonium bromide.

[0051] Preferably, the volume ratio of the ethanol or acetone to the reaction solution is 3-6:1.

[0052] Preferably, step 2 includes the following steps:

[0053] Step 21: Dissolve the modified biomass material, dianhydride, and diamine in an organic solvent, stir well, heat to 70-90 °C, and carry out a prepolymerization reaction for 2-6 hours under an inert atmosphere protection;

[0054] Step 22: Heat to 150-300 °C and react for 1-4 hours under an inert atmosphere protection;

[0055] Step 23: Wash the reaction product in step 22 several times with the same polar solvent used in step 21;

[0056] Step 24: Carry out vacuum drying at 60-80 °C for 6-10 hours, and obtain the copolymer after cooling.

[0057] Preferably, the dianhydride is any one of pyromellitic dianhydride, biphenyltetracarboxylic dianhydride, and hexafluorodiacid dianhydride, the diamine is any one of 4,4'-diaminodiphenyl ether, p-phenylenediamine, and 4,4'-diaminodiphenylmethane, the molar ratio of the dianhydride to the diamine is 1:1, the mass fraction of the modified biomass material is 10%-30% of the total mass of the modified biomass material, dianhydride, and diamine, and the organic solvent is any one of N-methylpyrrolidone, dimethylformamide, dimethylacetamide, dimethyl sulfoxide, and acetonitrile.

[0058] Preferably, the curing agent is any one of diethylenetriamine, m-phenylenediamine, and hexahydrophthalic anhydride, the filler is any one of montmorillonite, silica, alumina, boron nitride, silicon carbide, and zirconia, the mass ratio of the copolymer to the curing agent and the filler is 1:0.05-0.1:0.2-0.5, and the curing conditions are: first pre-cure at 80-100 °C for 1-2 hours, and then post-cure at 150-200 °C for 2-4 hours.

[0059] This technical solution also includes a high-performance high-temperature resistant resin material prepared by the above preparation method.

[0060] This technical solution also includes the application of the high-performance high-temperature resistant resin material described in the present invention in the fields of aerospace, electronic packaging, and mold manufacturing.

[0061] The following is a detailed description in combination with examples and comparative examples.

[0062] Example 1

[0063] A preparation method of a high-performance high-temperature resistant resin material includes the following steps:

[0064] Step 1. Modify lignin with epichlorohydrin to introduce active groups and obtain a modified lignin material;

[0065] It includes the following steps:

[0066] Step 11. Dissolve lignin in an aqueous acetic acid solution with a mass fraction of 0.2% to obtain a transparent solution;

[0067] Step 12. Add a basic reagent to the above transparent solution to adjust the pH of the solution to 8;

[0068] Step 13. Add epichlorohydrin and the catalyst tetrabutylammonium bromide to Step 12, stir well, and the molar ratio of epichlorohydrin, catalyst to the biomass material is 1:0.05:1;

[0069] Step 14. Heat to 50 °C and stir for 8 hours;

[0070] Step 15. Cool to room temperature and adjust the pH to neutral with dilute acid;

[0071] Step 16. Pour the reaction solution in Step 15 into ethanol for precipitation, the volume ratio of ethanol to the reaction solution is 3:1, filter and wash the precipitate;

[0072] Step 17. Vacuum dry the precipitate in Step 16 at 40 °C for 10 hours, and obtain the modified lignin material after cooling.

[0073] Step 2. Copolymerize the modified lignin material with pyromellitic dianhydride and 4,4'-diaminodiphenyl ether to obtain a copolymer;

[0074] It includes the following steps:

[0075] Step 21. Dissolve the modified lignin material, pyromellitic dianhydride, and 4,4'-diaminodiphenyl ether in N-methylpyrrolidone. The molar ratio of pyromellitic dianhydride to 4,4'-diaminodiphenyl ether is 1:1, and the mass fraction of the modified lignin material is 10% of the total mass of the modified lignin material, pyromellitic dianhydride, and 4,4'-diaminodiphenyl ether. Stir well, heat to 70 °C, and pre-polymerize for 6 hours under an inert atmosphere;

[0076] Step 22. Heat to 150 °C and react for 4 hours under an inert atmosphere;

[0077] Step 23. Wash the reaction product in Step 22 several times with the same polar solvent used in Step 21;

[0078] Step 24. Vacuum dry at 60 °C for 10 hours, and obtain the copolymer after cooling.

[0079] Step 3: Thoroughly mix the copolymer with the curing agent diethylenetriamine and the filler montmorillonite. The mass ratio of the copolymer to the curing agent and the filler is 1:0.05:0.2. Then cure it. The curing conditions are as follows: first pre-cure at 80°C for 2 hours, and then post-cure at 150°C for 4 hours;

[0080] Step 4: Cool to room temperature to obtain a high-performance high-temperature resistant resin material.

[0081] Example 2

[0082] A preparation method of a high-performance high-temperature resistant resin material, comprising the following steps:

[0083] Step 1: Modify cellulose with epichlorohydrin to introduce active groups to obtain a modified cellulose material;

[0084] Comprising the following steps:

[0085] Step 11: Dissolve cellulose in an aqueous acetic acid solution with a mass fraction of 1% to obtain a transparent solution;

[0086] Step 12: Add an alkaline reagent to the above transparent solution to adjust the pH of the solution to 9;

[0087] Step 13: Add epichlorohydrin and the catalyst tetrabutylammonium bromide to Step 12, and stir evenly. The molar ratio of epichlorohydrin, the catalyst to the biomass material is 2:0.1:1;

[0088] Step 14: Heat to 55°C and stir for 7 hours;

[0089] Step 15: Cool to room temperature and adjust the pH to neutral with dilute acid;

[0090] Step 16: Pour the reaction solution in Step 15 into ethanol for precipitation. The volume ratio of ethanol to the reaction solution is 4:1. Filter and wash the precipitate;

[0091] Step 17: Vacuum-dry the precipitate in Step 16 at 45°C for 9 hours, and cool to obtain a modified cellulose material.

[0092] Step 2: Thoroughly copolymerize the modified cellulose material with pyromellitic dianhydride and p-phenylenediamine to obtain a copolymer;

[0093] Comprising the following steps:

[0094] Step 21, dissolving the modified cellulose material, pyromellitic anhydride and p-phenylenediamine in dimethylformamide, wherein the molar ratio of pyromellitic anhydride to p-phenylenediamine is 1:1, and the mass fraction of the modified cellulose material is 15% of the total mass of the modified cellulose material, pyromellitic anhydride and p-phenylenediamine, stirring well, heating to 75° C., and prepolymerizing for 5 hours under inert atmosphere protection;

[0095] Step 22, heating to 200° C. and reacting for 3 hours under inert atmosphere protection;

[0096] Step 23, washing the reaction product in step 22 several times with the same polar solvent used in step 21;

[0097] Step 24, vacuum drying is performed at 65° C. for 9 hours, and a copolymer is obtained after cooling.

[0098] Step 3, fully mix the copolymer with the curing agent diethylenetriamine and the filler silica, the mass ratio of the copolymer to the curing agent and the filler is 1:0.06:0.25, and cure, the curing conditions are: pre-curing at 90°C for 1 hour, and then post-curing at 160°C for 3.5 hours;

[0099] Step 4: Cooling to room temperature to obtain a high-performance high-temperature resistant resin material.

[0100] Example 3

[0101] A method for preparing a high-performance high-temperature resistant resin material comprises the following steps:

[0102] Step 1, using epichlorohydrin to modify hemicellulose, introduce active groups, and obtain modified hemicellulose material;

[0103] The following steps are involved:

[0104] Step 11, dissolving hemicellulose in a 2% by mass acetic acid aqueous solution to obtain a transparent solution;

[0105] Step 12, adding an alkaline reagent to the above transparent solution to adjust the pH of the solution to 10;

[0106] Step 13, adding epichlorohydrin and catalyst tetrabutylammonium bromide to step 12, stirring thoroughly, the molar ratio of epichlorohydrin, catalyst and biomass material is 3:0.2:1;

[0107] Step 14, heating to 60°C, stirring and reacting for 6 hours;

[0108] Step 15, cooling to room temperature, and adjusting the pH to neutral with dilute acid;

[0109] Step 16, pouring the reaction solution in step 15 into ethanol for precipitation, wherein the volume ratio of ethanol to reaction solution is 6:1, filtering and washing the precipitate;

[0110] Step 17: vacuum-dry the precipitate in step 16 at 50° C. for 8 hours, and obtain a modified hemicellulose material after cooling.

[0111] Step 2, fully copolymerizing the modified hemicellulose material with pyromellitic anhydride and 4,4'-diaminodiphenylmethane to obtain a copolymer;

[0112] The following steps are involved:

[0113] Step 21, dissolving the modified hemicellulose material, pyromellitic anhydride, and 4,4'-diaminodiphenylmethane in dimethylacetamide, wherein the molar ratio of pyromellitic anhydride to 4,4'-diaminodiphenylmethane is 1:1, and the mass fraction of the modified hemicellulose material is 20% of the total mass of the modified hemicellulose material, pyromellitic anhydride, and 4,4'-diaminodiphenylmethane, stirring well, heating to 80° C., and prepolymerizing for 4 hours under inert atmosphere protection;

[0114] Step 22, heating to 250° C. and reacting for 2 hours under inert atmosphere protection;

[0115] Step 23, washing the reaction product in step 22 several times with the same polar solvent used in step 21;

[0116] Step 24, vacuum drying is performed at 70° C. for 8 hours, and a copolymer is obtained after cooling.

[0117] Step 3, fully mix the copolymer with the curing agent m-phenylenediamine and the filler alumina, the mass ratio of the copolymer to the curing agent and the filler is 1:0.08:0.3, and cure, and the curing conditions are: pre-curing at 90°C for 2 hours, and then post-curing at 170°C for 3 hours;

[0118] Step 4: Cooling to room temperature to obtain a high-performance high-temperature resistant resin material.

[0119] Example 4

[0120] A method for preparing a high-performance high-temperature resistant resin material comprises the following steps:

[0121] Step 1, using epichlorohydrin to modify chitosan, introduce active groups, and obtain modified chitosan material;

[0122] The following steps are involved:

[0123] Step 11, dissolving chitosan in a 4% by mass acetic acid aqueous solution to obtain a transparent solution;

[0124] Step 12, adding an alkaline reagent to the above transparent solution to adjust the pH of the solution to 9;

[0125] Step 13, adding epichlorohydrin and catalyst tetrabutylammonium bromide to step 12, stirring thoroughly, the molar ratio of epichlorohydrin, catalyst and biomass material is 4:0.4:1;

[0126] Step 14, heating to 65°C, stirring and reacting for 5 hours;

[0127] Step 15, cooling to room temperature, and adjusting the pH to neutral with dilute acid;

[0128] Step 16, precipitating the reaction solution in step 15 in acetone, wherein the volume ratio of acetone to reaction solution is 3:1, filtering and washing the precipitate;

[0129] Step 17: vacuum-dry the precipitate in step 16 at 55° C. for 7 hours, and obtain a modified chitosan material after cooling.

[0130] Step 2, fully copolymerizing the modified chitosan material with biphenyltetracarboxylic acid dianhydride and 4,4'-diaminodiphenyl ether to obtain a copolymer;

[0131] The following steps are involved:

[0132] Step 21, dissolving the modified chitosan material, biphenyltetracarboxylic acid dianhydride, and 4,4'-diaminodiphenyl ether in dimethyl sulfoxide, wherein the molar ratio of biphenyltetracarboxylic acid dianhydride to 4,4'-diaminodiphenyl ether is 1:1, and the mass fraction of the modified chitosan material is 25% of the total mass of the modified chitosan material, biphenyltetracarboxylic acid dianhydride, and 4,4'-diaminodiphenyl ether, stirring well, heating to 85° C., and prepolymerizing for 3 hours under inert atmosphere protection;

[0133] Step 22, heating to 300° C. and reacting for 1 hour under inert atmosphere protection;

[0134] Step 23, washing the reaction product in step 22 several times with the same polar solvent used in step 21;

[0135] Step 24, vacuum drying is performed at 75° C. for 7 hours, and a copolymer is obtained after cooling.

[0136] Step 3, fully mix the copolymer with the curing agent m-phenylenediamine and the filler boron nitride, the mass ratio of the copolymer to the curing agent and the filler is 1:0.09:0.4, and cure, and the curing conditions are: pre-curing at 100°C for 1 hour, and then post-curing at 180°C for 2.5 hours;

[0137] Step 4: Cooling to room temperature to obtain a high-performance high-temperature resistant resin material.

[0138] Example 5

[0139] A preparation method of a high-performance high-temperature resistant resin material, comprising the following steps:

[0140] Step 1: Modify starch with epichlorohydrin to introduce active groups, obtaining a modified starch material;

[0141] Comprising the following steps:

[0142] Step 11: Dissolve starch in an acetic acid aqueous solution with a mass fraction of 5% to obtain a transparent solution;

[0143] Step 12: Add an alkaline reagent to the above transparent solution to adjust the pH of the solution to 8;

[0144] Step 13: Add epichlorohydrin and the catalyst tetrabutylammonium bromide to Step 12, stir well, and the molar ratio of epichlorohydrin, the catalyst to the biomass material is 5:0.5:1;

[0145] Step 14: Heat to 70 °C and stir and react for 4 hours;

[0146] Step 15: Cool to room temperature and adjust the pH to neutral with dilute acid;

[0147] Step 16: Pour the reaction solution in Step 15 into acetone for precipitation, the volume ratio of acetone to the reaction solution is 5:1, filter and wash the precipitate;

[0148] Step 17: Vacuum-dry the precipitate in Step 16 at 60 °C for 6 hours, and obtain the modified starch material after cooling.

[0149] Step 2: Copolymerize the modified starch material with hexafluorodiacid anhydride and 4,4'-diaminodiphenylmethane fully to obtain a copolymer;

[0150] Comprising the following steps:

[0151] Step 21: Dissolve the modified starch material, hexafluorodiacid anhydride, and 4,4'-diaminodiphenylmethane in acetonitrile, the molar ratio of hexafluorodiacid anhydride to 4,4'-diaminodiphenylmethane is 1:1, and the mass fraction of the modified starch material is 30% of the total mass of the modified starch material, hexafluorodiacid anhydride, and 4,4'-diaminodiphenylmethane, stir well, heat to 90 °C, and pre-polymerize under an inert atmosphere for 2 hours;

[0152] Step 22: Heat to 200 °C and react for 4 hours under an inert atmosphere;

[0153] Step 23: Wash the reaction product in Step 22 several times with the same polar solvent used in Step 21;

[0154] Step 24: Perform vacuum drying at 80 °C for 6 hours, and obtain the copolymer after cooling.

[0155] Step 3: Thoroughly mix the copolymer with the curing agent hexahydrophthalic anhydride and the filler silicon carbide. The mass ratio of the copolymer to the curing agent and the filler is 1:0.1:0.5. Cure it, and the curing conditions are as follows: First, perform pre-curing at 100 °C for 2 hours, and then perform post-curing at 200 °C for 2 hours.

[0156] Step 4: Cool to room temperature to obtain the high-performance high-temperature resistant resin material.

[0157] Comparative Example 1

[0158] A preparation method of a high-performance high-temperature resistant resin material is carried out according to the method in Example 3. The difference is that the mass ratio of the copolymer to the curing agent and the filler is 1:0.08:0.

[0159] Comparative Example 2

[0160] A preparation method of a high-performance high-temperature resistant resin material is carried out according to the method in Example 3. The difference is that the mass ratio of the copolymer to the curing agent and the filler is 1:0.08:0.2.

[0161] Comparative Example 3

[0162] A preparation method of a high-performance high-temperature resistant resin material is carried out according to the method in Example 3. The difference is that the mass ratio of the copolymer to the curing agent and the filler is 1:0.08:0.25.

[0163] Comparative Example 4

[0164] A preparation method of a high-performance high-temperature resistant resin material is carried out according to the method in Example 3. The difference is that the mass ratio of the copolymer to the curing agent and the filler is 1:0.08:0.4.

[0165] Comparative Example 5

[0166] A preparation method of a high-performance high-temperature resistant resin material is carried out according to the method in Example 3. The difference is that the mass ratio of the copolymer to the curing agent and the filler is 1:0.08:0.5.

[0167] Performance Test

[0168] The thermal decomposition temperatures of Examples 1-5 and Comparative Examples 1-5 are measured by thermogravimetric analysis, and the measurement results are shown in the following table:

[0169] Test items Thermal decomposition temperature / (°C) Test items Thermal decomposition temperature / (°C) Example 1 510 Comparative Example 1 400 Example 2 525 Comparative Example 2 480 Example 3 520 Comparative Example 3 495 Example 4 514 Comparative Example 4 528 Example 5 sos Comparative Example 5 535

[0170] Through the determination results of thermogravimetric analysis, the thermal decomposition temperature of the high-temperature resistant resin material of this technical solution can reach above 500 °C, which is beneficial to its application in the fields of aerospace, electronic packaging, and mold manufacturing. In addition, from the determination results of the comparative examples, increasing the proportion of the filler in the resin material is beneficial to improving the high-temperature resistance of the resin material.

[0171] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments, and the above embodiments and descriptions in the specification are only preferred examples of the present invention and are not used to limit the present invention. Without departing from the spirit and scope of the present invention, the present invention will have various changes and improvements, and these changes and improvements all fall within the scope of the present invention claimed. The scope of protection claimed by the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a high-performance high-temperature resistant resin material, characterized in that: The following steps are involved: Step 1: using epichlorohydrin to modify the biomass material, introducing active groups, and obtaining a modified biomass material; Step 2, fully copolymerizing the modified biomass material with dianhydride and diamine to obtain a copolymer; Step 3, fully mixing the copolymer with the curing agent and the filler, and curing; Step 4: Cooling to room temperature to obtain a high-performance high-temperature resistant resin material.

2. The method for preparing a high-performance high-temperature resistant resin material according to claim 1, characterized in that: The step 1 comprises the following steps: Step 11, dissolving the biomass material in a dilute acid solution to obtain a transparent solution; Step 12, adding an alkaline reagent to the above transparent solution to adjust the pH of the solution to 8-10; Step 13, adding epichlorohydrin and a catalyst to step 12, and stirring thoroughly, wherein the molar ratio of epichlorohydrin, catalyst and biomass material is 1-5:0.05-0.5:1; Step 14, heating to 50-70°C, stirring and reacting for 4-8 hours; Step 15, cooling to room temperature, and adjusting the pH to neutral with dilute acid; Step 16, pouring the reaction solution in step 15 into ethanol or acetone for precipitation, filtering and washing the precipitate; Step 17: vacuum-dry the precipitate in step 16 at 40-60° C. for 6-10 hours, and obtain a modified biomass material after cooling.

3. The method for preparing a high-performance high-temperature resistant resin material according to claim 2, characterized in that: The biomass material is one or more of lignin, cellulose, hemicellulose, chitosan and starch.

4. The method for preparing a high-performance high-temperature resistant resin material according to claim 2, characterized in that: The dilute acid solution is an acetic acid aqueous solution with a mass fraction of 0.2% to 5%, and the catalyst is tetrabutylammonium bromide.

5. The method for preparing a high-performance high-temperature resistant resin material according to claim 2, characterized in that: The volume ratio of the ethanol or acetone to the reaction liquid is 3 to 6:

1.

6. The method for preparing a high-performance high-temperature resistant resin material according to claim 1, characterized in that: The step 2 comprises the following steps: Step 21, dissolving the modified biomass material, dianhydride and diamine in an organic solvent, fully stirring, heating to 70-90° C., and prepolymerizing for 2-6 hours under an inert atmosphere; Step 22, heating to 150-300° C., reacting for 1-4 hours under inert atmosphere protection; Step 23, washing the reaction product in step 22 several times with the same polar solvent used in step 21; Step 24, vacuum drying at 60-80° C. for 6-10 hours, and cooling to obtain a copolymer.

7. The method for preparing a high-performance high-temperature resistant resin material according to claim 6, characterized in that: The dianhydride is any one of pyromellitic dianhydride, biphenyltetracarboxylic dianhydride, and hexafluorodianhydride; the diamine is any one of 4,4'-diaminodiphenyl ether, p-phenylenediamine, and 4,4'-diaminodiphenylmethane; the molar ratio of the dianhydride to the diamine is 1:1; the mass fraction of the modified biomass material is 10% to 30% of the total mass of the modified biomass material, the dianhydride, and the diamine; and the organic solvent is any one of N-methylpyrrolidone, dimethylformamide, dimethylacetamide, dimethyl sulfoxide, and acetonitrile.

8. The method for preparing a high-performance, high-temperature resistant resin material according to claim 1, characterized in that: The curing agent is any one of diethylenetriamine, metaphenylenediamine, and hexahydrophthalic anhydride; the filler is any one of montmorillonite, silicon dioxide, aluminum oxide, boron nitride, silicon carbide, and zirconium oxide; the mass ratio of the copolymer to the curing agent and the filler is 1:0.05-0.1:0.2-0.5; and the curing conditions are: pre-curing at 80-100°C for 1-2 hours, and then post-curing at 150-200°C for 2-4 hours.

9. A high-performance, high-temperature resistant resin material, characterized in that: Prepared by the preparation method according to any one of claims 1 to 8.

10. Application of the high-performance, high-temperature resistant resin material according to claim 9 in the fields of aerospace, electronic packaging, and mold manufacturing.