CN110698816B - Wear-resistant heat-resistant epoxy composite material and preparation method thereof - Google Patents

Abstract

The invention relates to a wear-resistant heat-resistant epoxy composite material and a preparation method thereof, wherein the wear-resistant heat-resistant epoxy composite material comprises an epoxy resin matrix material and ZrO uniformly dispersed in the epoxy resin matrix material₂/Ti₃C₂A nanocomposite material of said ZrO₂/Ti₃C₂0.1-3 wt% of a nanocomposite material with respect to an epoxy resin matrix material, the epoxy composite material being ZrO 2₂/Ti₃C₂The nano composite material and the epoxy resin are cured in the presence of quaternary ammonium salt. The wear-resistant heat-resistant epoxy composite material is simple in preparation method and easy in obtaining of raw materials. Compared with the common epoxy material, the wear-resistant heat-resistant epoxy composite material prepared by the invention has lower wear rate, higher glass transition temperature and higher tensile strength, and is particularly suitable for being used as a wear-resistant device in a high-temperature environment.

Description

A kind of wear-resistant and heat-resistant epoxy composite material and preparation method thereof

technical field

The invention belongs to the field of preparation of polymer-based composite materials, and particularly relates to a preparation method for wear-resistant and heat-resistant epoxy composite materials.

Background technique

Epoxy resin is a kind of thermosetting resin with outstanding mechanical properties, high chemical stability and low shrinkage rate. As a composite material made of matrix resin, it is widely used in aerospace, rail transit, sports equipment and other fields. However, the three-dimensional cross-linked network structure formed by curing makes the epoxy resin exhibit certain brittleness and poor abrasion resistance. In addition, the poor heat resistance of epoxy resin is difficult to meet the requirements of the increasingly developed engineering technology, which also limits its application. Therefore, improving wear resistance and heat resistance is of great significance for the practical application of epoxy resins.

The main way to improve the wear resistance of epoxy resins is to increase the wear resistance of epoxy resins by adding wear-resistant fillers to the epoxy resins to increase the strength of the epoxy resin's cross-linked network or reduce the friction coefficient. Studies have shown that nano-rubber, TiO ₂ , Al ₂ O ₃ and so on can effectively improve the wear resistance of epoxy resin. The main methods for improving the heat resistance of epoxy resins include: developing epoxy resins with heat-resistant skeletons; synthesizing epoxy resin curing agents with novel structures; blending or copolymerizing with inorganic nanomaterials. Studies have shown that the surface-treated nanomaterials play the role of cross-linking points in the matrix, which increases the cross-linking density of the system and the glass transition temperature Tg, thereby improving the heat resistance.

MXene is a kind of two-dimensional transition metal carbonitride material with excellent electrical, thermal, mechanical and optical properties. It can be expressed as M _n+1 X _n (n=1～3) by the general formula, where M represents the pre-transition Metals, where X is carbon, nitrogen, or both, have abundant termination groups on their surfaces, such as -OH, -F, etc. Among them, _Ti3C2 is a typical _MXene material with high mechanical strength and low friction coefficient. The study found that adding Ti ₃ C ₂ particles to ultra-high molecular weight polyethylene (UHMWPE) can effectively reduce the friction coefficient of UHMWPE and improve the wear resistance of UHMWPE. Therefore, it is expected that the wear resistance of epoxy resins can be effectively improved by adding _{Ti3C2 particles} .

ZrO2 is a class of commonly used metal _oxide inorganic fillers, which have excellent wear resistance, chemical resistance, high hardness and high heat resistance. Research shows that nano ZrO ₂ filler can not only improve the wear resistance of epoxy resin, but also can effectively improve its heat resistance. However, due to the extremely easy agglomeration phenomenon of nanoscale materials, the improvement effect of nano-ZrO2 _on epoxy resin wear resistance and heat resistance is severely restricted. Therefore, improving the dispersion degree of nano _- ZrO2 in epoxy resin is one of the key issues in the process of preparing wear-resistant and heat-resistant epoxy composites.

Some of the prior art studies the composite material of epoxy resin and MXene. Patent document CN102977745A discloses a room temperature-curable and ultra-high temperature resistant coating and a preparation method thereof, which is a two-component product, and component A includes phenolic epoxy resin, titanium carbide, zirconia and filler, and the filler includes clay, Carbon fiber, polyimide and polyether ether ketone, the B component of the coating is an amine curing agent, and the ultra-high temperature resistant coating is prepared according to this method, but the amount of MXene used in it is very large, far exceeding the amount of epoxy resin , does not have industrial practical value. Patent document CN10980290A discloses an epoxy resin/MXene composite material, wherein the MXene material is obtained by sintering, grinding, etching, and ultrasonic layering of Ti, Nb, V, Cr or Ta metal, aluminum powder, and carbon powder. After a single layer of MXene is mixed with methyl tetrahydrophthalic anhydride, curing agent, accelerator and epoxy resin, it is prepared by heating and curing. However, this method is complicated, and the yield of monolayer MXene after ultrasonication is usually low, the obtained MXene is a monolayer/multilayer mixture, and the mass ratio of monolayer/multilayer MXene is extremely difficult to control, thus making the final prepared MXene/multilayer MXene extremely difficult to control. The performance stability of epoxy resin composite products is poor. Patent CN110105711A discloses a method for improving the friction performance of epoxy resin, which is to prepare a uniform _{Ti3C MXene} /cellulose solution from _Ti3C2 nanosheets and nanocellulose, and obtain _Ti3C after freezing in one direction A 3D network structural block of ₂ nanosheets. Adding epoxy resin, fully immersing the three-dimensional structure, the epoxy resin composite material is prepared, and the friction coefficient, wear rate and wear volume of the obtained material have been greatly improved. However, the patented method has defects such as complicated technological process and difficulty in industrialized production, and does not have the conditions for large-scale industrialized production. Moreover, in these methods, simply physically mixing or impregnating epoxy resin and MXene cannot effectively combine the two materials, and cannot effectively improve various properties of epoxy resin.

SUMMARY OF THE INVENTION

In order to overcome the above-mentioned defects of the prior art, the purpose of the present invention is to provide a wear-resistant and heat-resistant epoxy composite material and a preparation method thereof. The inventor unexpectedly found that after the ZrO ₂ /Ti ₃ C ₂ nanocomposite particles were treated with a certain amount of quaternary ammonium salt, and then cured with liquid epoxy resin under suitable conditions, the wear resistance and heat resistance of the composite material were obtained. The tensile strength is also improved to a certain extent.

The technical scheme of the present invention is as follows:

An object of the present invention is to provide a wear-resistant and heat-resistant epoxy composite material, comprising an epoxy resin matrix material and a ZrO ₂ /Ti ₃ C ₂ nanocomposite material uniformly dispersed in the epoxy resin matrix material, the ZrO 0.1-3wt% of ₂ /Ti ₃ C ₂ nanocomposite relative to epoxy resin matrix material, the epoxy composite material is ZrO ₂ /Ti ₃ C ₂ nanocomposite and epoxy resin in the presence of quaternary ammonium salt solidified.

Preferably, the ZrO ₂ /Ti ₃ C ₂ nanocomposite material accounts for 0.5-1 wt % of the epoxy resin matrix material.

Ti ₃ C ₂ has a unique accordion-like lamella structure, the surface area of the lamella is large, there is a certain gap between the lamellae, and the surface of the lamella is rich in functional groups such as -OH, which is suitable for nano-ZrO ₂ in its surface growth. The nano ZrO ₂ was directly grown on the Ti ₃ C ₂ lamella structure by the hydrothermal method, and the ZrO ₂ /Ti ₃ C ₂ nanocomposite particles obtained were surface modified, which greatly improved the wear resistance of the epoxy resin. and heat resistance, and its tensile strength is also improved to a certain extent. The research on using ZrO ₂ /Ti ₃ C ₂ nanocomposite particles to modify epoxy resin has not been reported publicly.

The wear-resistant and heat-resistant epoxy composite material provided by the invention uses ZrO ₂ /Ti ₃ C ₂ nano-composite material as filler, firstly treats the ZrO ₂ /Ti ₃ C ₂ nano-composite material with quaternary ammonium salt, and then mixes it with liquid ring The oxygen is fully mixed, and then mixed with the curing agent and the accelerator to obtain a pre-cured epoxy precursor mixture, and then the epoxy precursor mixture is cured and crosslinked at high temperature to obtain the epoxy composite material.

The epoxy resin matrix material is a mixture of liquid epoxy, curing agent and accelerator.

Preferably, the liquid epoxy is selected from at least one of E-51, E-55, E-44, E-42; and/or

The curing agent is an acid anhydride curing agent, selected from at least one of tetrahydrophthalic anhydride, methyltetrahydrophthalic anhydride, hexahydrophthalic anhydride, methylhexahydrophthalic anhydride, phthalic anhydride, and maleic anhydride; and/or

The accelerator is an amine accelerator selected from tetraethylammonium bromide, dimethylbenzylamine, 2-ethyl-4-methylimidazole, 2,4,6-tris(dimethylaminomethyl) base) at least one of phenol, triethanolamine, N,N-dimethylformamide, N,N-dimethylacetamide, N,N-dimethylaniline, and N,N-dimethylbenzylamine.

The quaternary ammonium salt is an ammonium halide with a long-chain alkyl or aryl group, preferably cetyltrimethylammonium bromide, dodecyldimethylbenzylammonium bromide, N,N dimethyl ammonium bromide. dodecyl ammonium bromide, octadecyl trimethyl ammonium chloride, dodecyl trimethyl ammonium bromide, dodecyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium bromide Ammonium, octadecyltrimethylammonium bromide, didecyldimethylammonium bromide, dodecyldimethylbenzylammonium chloride, cetyltrimethylammonium chloride, dodecyldimethylammonium chloride Alkyldimethylphenoxyethylammonium bromide, bis(dodecyldimethyl)ethylene ammonium bromide.

Preferably, the mass ratio of the quaternary ammonium salt and the ZrO ₂ /Ti ₃ C ₂ nanocomposite is 1:2-5, specifically adding the prepared ZrO ₂ /Ti ₃ C ₂ nanocomposite to the quaternary ammonium salt aqueous solution Mix well, the concentration of the quaternary ammonium salt aqueous solution is not particularly limited, generally the mass fraction of the quaternary ammonium salt aqueous solution is 0.2-2%.

The ZrO ₂ /Ti ₃ C ₂ nanocomposite is prepared by in-situ hydrothermal growth of ZrO ₂ nanoparticles on Ti ₃ C by using ZrOCl ₂ ·8H ₂ O as the precursor of ZrO ₂ in the Ti ₃ C ₂ dispersion. ₂ surfaces, the molar ratio of ZrOCl ₂ ·8H ₂ O to Ti ₃ C ₂ is 1:1-5.

The ZrO ₂ /Ti ₃ C ₂ nanocomposite material of the present invention is prepared by a preparation method comprising the following steps:

1) Add Ti ₃ C ₂ powder and ZrOCl ₂ 8H ₂ O to 30 ml of deionized water, ultrasonicate for 30 min to form a dispersion, slowly add the alkaline solution dropwise to the dispersion, stir well at room temperature to obtain uniform mixing solution;

2) Transfer the mixed solution obtained in step 1) into a polytetrafluoroethylene liner autoclave, and fully react at 100-220° C. for 6-36 hours;

3) After the reaction in step 2) is finished and naturally cooled, the powder obtained from the reaction is collected by centrifugation, then washed with deionized water and dehydrated ethanol, respectively, and then the washed powder is placed in a vacuum drying box to dry, and the obtained powder product is ZrO ₂ /Ti ₃ C ₂ nanocomposites.

The particle size of the Ti ₃ C ₂ powder used is not particularly limited, and the particle size and size of the Ti ₃ C ₂ obtained by general conventional methods can be used to prepare the TiO ₂ /Ti ₃ C ₂ nanocomposite material in this application. Preferably, the Ti ₃ C ₂ is 5-10 μm in diameter and 3-6 μm in thickness.

The ZrOCl ₂ ·8H ₂ O precursor solution and the Ti ₃ C ₂ dispersion are uniformly mixed, and can be added dropwise separately or one of the solutions can be added dropwise to the other solution in a manner well known in the art. In the present invention, the method of slowly dropping the precursor solution into the Ti ₃ C ₂ dispersion liquid is preferred.

The second object of the present invention is to provide a method for preparing the above-mentioned wear-resistant and heat-resistant epoxy composite material, comprising the following steps:

1) The ZrO ₂ /Ti ₃ C ₂ nanocomposite is added to the quaternary ammonium salt aqueous solution, ultrasonically dispersed, and then added to the liquid epoxy, and distilled under reduced pressure to obtain a ZrO ₂ /Ti ₃ C ₂ /epoxy mixed solution , then add curing agent and accelerator, and stir under vacuum to obtain epoxy mixed system;

2) pouring the epoxy mixed system obtained in step 1) into a stainless steel mold, heating and curing to obtain the wear-resistant and heat-resistant epoxy composite material.

Wherein, the mass ratio between liquid epoxy, curing agent and accelerator is 100:60-100:1-5, preferably 100:80-90:1-2.

The advantages and characteristics of the present invention are:

1. In the present invention, the nano-scale ZrO ₂ grown by in-situ hydrothermal is evenly distributed on the surface of Ti ₃ C ₂ , and Ti ₃ C ₂ has higher mechanical strength and lower friction coefficient, and can improve the wear resistance of epoxy resin; ZrO ₂ has excellent wear resistance and heat resistance, which can improve the wear resistance and heat resistance of epoxy resin.

2. The inventors also unexpectedly found that after the ZrO ₂ /Ti ₃ C ₂ /nanocomposite particles are treated with a certain amount of quaternary ammonium salt, and then cured with epoxy resin, the mechanical and chemical bonding between the two materials is better. , the wear resistance and heat resistance of the obtained epoxy composite material are greatly improved, and the tensile strength is also improved to a certain extent.

3. The preparation method of the wear-resistant and heat-resistant epoxy composite material provided by the present invention is simple, and the raw materials are easily obtained, which is a method suitable for industrialized large-scale production of epoxy resin.

Description of drawings

Fig. ₁ is the SEM photograph of the _Ti3C2 nanomaterial of the present invention

FIG. 2 is a SEM photograph of the ZrO ₂ /Ti ₃ C ₂ nanocomposite in Example 1

Detailed ways

The technical content of the present invention will be further explained below with reference to specific embodiments. However, the present invention is not limited to the following examples. Unless otherwise defined, all technical terms used hereinafter have the same meaning as commonly understood by those skilled in the art. The technical terms used herein are only for the purpose of describing specific embodiments, and are not intended to limit the protection scope of the present invention.

The experimental methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials can be obtained from commercial sources unless otherwise specified.

The Ti ₃ C ₂ used in the examples of the present invention was obtained by self-production. Its preparation method has been widely adopted in the industry, namely adding commercial Ti ₃ AlC ₂ powder to hydrofluoric acid, stirring at room temperature, and etching to obtain Ti ₃ C ₂ powder with a diameter of about 8 μm and a thickness of about 8 μm. 4μm. The E51 epoxy resin used was purchased from Phoenix.

Example 1

1) Add 3 mmol of Ti ₃ C ₂ powder with a diameter of 4.5 μm and a thickness of 2.4 μm and 1.25 mmol of ZrOCl ₂ ·8H ₂ O into 30 ml of deionized water, and ultrasonically for 30 min to form dispersion A; add 2.5 mmol of NaOH to 45ml of deionized water, stirred to obtain solution B;

2) Slowly add solution B dropwise to dispersion A, and stir vigorously for 2 hours at room temperature to obtain a uniform mixed solution;

3) Transfer the mixed solution obtained in step 2) into a polytetrafluoroethylene liner autoclave, and react at 160° C. for 24 hours;

4) After the reaction in step 3) is completed and naturally cooled, the powder obtained from the reaction is collected by centrifugation at 6000 r/min, and then washed with deionized water and absolute ethanol, respectively, and then the washed powder is placed in a vacuum drying box at 60° C. After drying for 12h, the obtained powder product is ZrO ₂ /Ti ₃ C ₂ nanocomposite;

5) Accurately weigh 0.945 g of the ZrO ₂ /Ti ₃ C ₂ nanocomposite material obtained in step 4, add it to 50 mL of an aqueous solution containing 0.41 g of hexadecyltrimethylammonium bromide (CTAB), and ultrasonically for 0.5 h to form a dispersion liquid , and then added to 100 g of liquid epoxy E51, and distilled under reduced pressure at 100° C. for 5 h to obtain a ZrO ₂ /Ti ₃ C ₂ /epoxy mixed solution. After cooling to room temperature, 88 g of methyl hexahydrophthalic anhydride solution and 1 g of tetraethylammonium bromide were added, and the mixture was stirred under vacuum for 0.5 h to obtain an epoxy mixed system. 0.5wt% of ZrO ₂ /Ti ₃ C ₂ nanocomposite relative to epoxy resin matrix (the sum of the mass of liquid epoxy, methylhexahydrophthalic anhydride and tetraethylammonium bromide);

6) The epoxy mixed system obtained in step 5) is poured into a stainless steel mold, and cured at 150° C. for 2 hours to obtain a ZrO ₂ /Ti ₃ C ₂ /epoxy composite material.

FIG. 1 is the SEM photograph of the Ti ₃ C ₂ nanomaterial used in Example 1, and FIG. 2 is the SEM photograph of the ZrO ₂ /Ti ₃ C ₂ nanocomposite prepared in Preparation Example 1. It can be seen from the figure that after the in-situ growth _of ZrO2 _on the _Ti3C2 nanosheets, a large number of uniformly distributed ZrO2 particles appeared _on the _{Ti3C2 nanosheets} , and the surface _of the _Ti3C2 nanosheets was significantly roughened. It may make the mechanical bond between the ZrO ₂ /Ti ₃ C ₂ nanocomposite particles and the epoxy resin matrix stronger, and improve the mechanical strength and wear resistance of the ZrO ₂ /Ti ₃ C ₂ epoxy composite material prepared subsequently.

Example 2

The other steps are the same as those in Example 1, except that the amount of ZrOCl ₂ ·8H ₂ O in step 1) is changed to 2.5 mmol.

Example 3

The other steps are the same as those in Example 1, except that the amount of ZrOCl ₂ ·8H ₂ O in step 1) is changed to 0.625 mmol.

Example 4

The other steps are the same as those in Example 2, except that the amount of ZrO ₂ /Ti ₃ C ₂ nanocomposite in step 5) is 1.42 g, which is 0.75 wt % relative to the epoxy resin matrix.

Example 5

The other steps are the same as in Example 2, except that the amount of ZrO ₂ /Ti ₃ C ₂ nanocomposite in step 5) is 1.89 g, that is, 1 wt % relative to the epoxy resin matrix.

Example 6

Others are the same as Example 2, except that in step 5), the quaternary ammonium salt is replaced by dodecyltrimethylammonium bromide.

Example 7

Others are the same as in Example 2, except that in step 5), the quaternary ammonium salt is replaced by octadecyltrimethylammonium bromide.

Example 8

Others are the same as in Example 2, except that in step 5), the quaternary ammonium salt is replaced by dodecyldimethylbenzylammonium chloride.

Comparative Example 1

Others are the same as in Example 1, except that no quaternary ammonium salt is added in step 5).

Comparative Example 2

Others are the same as in Example 1, except that in step 5), the quaternary ammonium salt is replaced with a silane coupling agent.

Comparative Example 3

Others are the same as in Example 1, except that in step 5), sodium dodecylsulfonate (SDS) is used to replace the quaternary ammonium salt.

Comparative Example 4

Others are the same as in Example 1, except that in step 5), the ZrO ₂ /Ti ₃ C ₂ nanocomposite material is replaced by the Ti ₃ C ₂ nanomaterial.

Comparative Example 5

Commercially available epoxy resin E51 was used, without adding ZrO ₂ /Ti ₃ C ₂ nanocomposite material, and curing was performed according to the same curing conditions as in Example 1.

Application example

The epoxy resin material obtained by the above-mentioned embodiment check example is tested for abrasion resistance and heat resistance, the results are shown in Table 1, and the test method is as follows:

(1) Wear resistance

The wear resistance of the sample was tested by a friction and wear testing machine: friction was performed for 1 h under the conditions of a load of 8 N, a rotational speed of 780 r/min, and a friction torque of 500 N m, and the test results were expressed as specific wear.

(2) Heat resistance

The thermal resistance of the sample was evaluated by a dynamic mechanical thermal analyzer: the temperature was raised to 220 °C under the conditions of a vibration frequency of 1 Hz and a heating rate of 3 °C/min, and the test results were expressed as glass transition temperature.

(3) Tensile strength

Tested according to the national standard GB/T2568-1995.

Table 1

It can be seen from the data in Table ₁ that the wear resistance and heat resistance _of the epoxy composite obtained by the present invention are better _than those of the commercially available common ring Oxygen resin has been greatly improved, and the tensile strength has also been improved to a certain extent. By comparing with the examples and comparative examples 1-3, if no quaternary ammonium salt is added, or other types of modifiers are added, the composite material with ZrO ₂ /Ti ₃ C ₂ nanocomposite particles and epoxy resin well dispersed cannot be obtained , so that its wear resistance and heat resistance are limited and cannot meet the actual needs.

The preparation method of the invention is simple, the raw materials are cheap and easy to obtain, the obtained epoxy resin composite material has excellent comprehensive properties, and has outstanding wear resistance compared with the epoxy resin not modified by the ZrO ₂ /Ti ₃ C ₂ nanocomposite material. And the advantages of heat resistance, with market competitiveness.

The above specific embodiments are only schematic illustrations of the content of the present invention, and do not represent the limitation of the content of the present invention. Those skilled in the art can think of other variations of the specific structures in the present invention. The above detailed description is a specific description of one of the feasible embodiments of the present invention, which is not intended to limit the scope of the present invention. Any equivalent implementation or modification that does not depart from the present invention shall be included in the present invention. within the scope of the technical solution.

Claims (9)

1. A wear-resistant and heat-resistant epoxy composite material comprises an epoxy resin matrix material and ZrO uniformly dispersed in the epoxy resin matrix material₂/Ti₃C₂Nanocomposite of the said ZrO₂/Ti₃C₂0.1-3 wt% of a nanocomposite material with respect to an epoxy resin matrix material, the epoxy composite material being ZrO 2₂/Ti₃C₂The nano composite material and the epoxy resin are obtained by curing in the presence of quaternary ammonium salt;

the epoxy resin matrix material is a mixture of liquid epoxy, a curing agent and an accelerator;

the ZrO₂/Ti₃C₂The nano composite material is obtained by a preparation method comprising the following steps: at Ti₃C₂In the dispersion, ZrOCl is added₂·8H₂O is ZrO₂Precursor of (a) in situ hydrothermal growth of ZrO₂Nanoparticles in Ti₃C₂Obtained on the surface, ZrOCl₂·8H₂O and Ti₃C₂The molar ratio of (A) to (B) is 1: 1-5;

the wear-resistant heat-resistant epoxy composite material is prepared by a preparation method comprising the following steps:

1)ZrO 2 is mixed with₂/Ti₃C₂Adding the nano composite material into a quaternary ammonium salt aqueous solution, performing ultrasonic dispersion, then adding the nano composite material into liquid epoxy, and performing reduced pressure distillation to obtain ZrO₂/Ti₃C₂Adding a curing agent and an accelerator into the epoxy mixed solution, and stirring under vacuum to obtain an epoxy mixed system;

2) pouring the epoxy mixed system obtained in the step 1) into a stainless steel mold, and heating and curing to obtain the wear-resistant heat-resistant epoxy composite material.

2. The epoxy composite of claim 1, wherein the ZrO 2₂/Ti₃C₂The nano composite material accounts for 0.5-1 wt% of the epoxy resin matrix material.

3. The epoxy composite of claim 1, wherein the liquid epoxy is selected from at least one of E-51, E-55, E-44, E-42; and/or

The curing agent is an anhydride curing agent and is selected from at least one of tetrahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, hexahydrophthalic anhydride, methyl hexahydrophthalic anhydride, phthalic anhydride and maleic anhydride; and/or

The accelerator is an amine accelerator and is selected from at least one of tetraethylammonium bromide, dimethylbenzylamine, 2-ethyl-4-methylimidazole, 2,4, 6-tri (dimethylaminomethyl) phenol, triethanolamine, N-dimethylformamide, N-dimethylacetamide, N-dimethylaniline and N, N-dimethylbenzylamine.

4. The epoxy composite of claim 1, wherein the ZrO 2₂/Ti₃C₂The nano composite material is prepared by a preparation method comprising the following steps:

1) mixing Ti₃C₂Powder and ZrOCl₂·8H₂Adding O into 30ml of deionized water, carrying out ultrasonic treatment for 30min to form a dispersion liquid, slowly dropwise adding an alkaline solution into the dispersion liquid, and fully stirring at room temperature to obtain a uniform mixed solution;

2) transferring the mixed solution obtained in the step 1) into a polytetrafluoroethylene liner high-pressure reaction kettle, and fully reacting at 100-220 ℃;

3) after the reaction in the step 2) is finished and naturally cooled, centrifugally collecting powder obtained by the reaction, respectively washing the powder by using deionized water and absolute ethyl alcohol, and then placing the washed powder in a vacuum drying oven for drying to obtain a powder product, namely ZrO₂/Ti₃C₂A nanocomposite material.

5. The epoxy composite of claim 1, wherein the quaternary ammonium salt is an ammonium halide with long chain alkyl or aryl groups.

6. The epoxy composite of claim 5, wherein the quaternary ammonium salt is selected from the group consisting of cetyltrimethylammonium bromide, dodecyldimethylbenzylammonium bromide, N-dimethyldodecylammonium bromide, octadecyltrimethylammonium chloride, decaalkyltrimethylammonium bromide, dodecyltrimethylammonium bromide, tetradecyltrimethylammonium bromide, octadecyltrimethylammonium bromide, didecyldimethylammonium bromide, dodecyldimethylbenzylammonium chloride, hexadecyltrimethylammonium chloride, dodecyldimethylphenoxyethylammonium bromide, and bis (dodecyldimethyl) ethyleneammonium bromide.

7. The epoxy composite of claim 1, wherein the quaternary ammonium salt and ZrO₂/Ti₃C₂The mass ratio of the nano composite material is 1: 2-5.

8. The epoxy composite material of claim 1, wherein the mass ratio of the liquid epoxy, the curing agent, and the accelerator is 100:60 to 100:1 to 5.

9. The epoxy composite of claim 8, wherein the mass ratio of the liquid epoxy, curing agent, accelerator is 100:80-90: 1-2.

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