CN109880290B - Preparation method of epoxy resin/MXene composite material - Google Patents
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Abstract
The preparation method of the epoxy resin/MXene composite material comprises the steps of preparing single-layer MXene, determining the addition amount of the single-layer MXene, compounding the single-layer MXene and the epoxy resin material and the like; the preparation method has the advantages of simple process, short time, high efficiency and low cost, and the prepared epoxy resin/MXene composite material has the advantages of obviously improved tensile breaking strength and good mechanical property.
Description
Technical Field
The invention belongs to the field of material science, and particularly relates to a preparation method of an epoxy resin/MXene composite material.
Background
In recent years, with the discovery of graphene and its unique physical and chemical properties, the research heat of two-dimensional crystals is raised. The two-dimensional layered nano compound is a material with a graphene-like structure, has various excellent performances due to the characteristic of high specific surface area, and comprises transition metal disulfides, metal oxides and the like besides graphene; in recent years, Barsum and the like selectively etch away Al atoms in a three-dimensional layered compound MAX by using hydrofluoric acid to obtain a two-dimensional crystal compound with a graphene-like structure and is named as MXene; having the chemical formula Mn+1XnN =1,2,3, M is an early transition metal element, and X is a carbon/nitrogen element. The MXene precursor is MAX which is a ternary layered structure with the excellent properties of metal and ceramic, M, X, n is the same as the above, A is a main group element, more than 60 MAX phases are known at present, and a large amount of MXene with special properties can be prepared by etching, which is of great significance for the preparation and research of two-dimensional crystal materials.
The epoxy resin is a generic name of compounds which contain two or more epoxy groups in one molecule and are capable of forming a three-dimensional crosslinked network-like cured product in the presence of an appropriate chemical agent; wherein, the epoxy group is a group consisting of carbon atoms and oxygen atoms, and the epoxy group is also a reactive group of the epoxy resin. However, macromolecular chains in the cured epoxy resin are mutually crosslinked and agglomerated together and cannot move, the structure is three-dimensional net-shaped, and the bonds of C-C bonds and C-O bonds are small in energy and high in surface energy, so that the epoxy resin is very brittle, has weak strong bearing capacity, is very easy to crack under the action of external force, and the like, thereby greatly limiting the application of the epoxy resin in engineering.
As a novel two-dimensional layered nano compound, MXene has a plurality of unique physical and chemical properties and is expected to become an excellent material for modified epoxy resin; the MXene is prepared in a water environment at the present stage, and because the MXene surface has extremely high chemical activity and is difficult to store for a long time, how to extract a monolayer MXene material from the water environment and the accurate determination of the quality becomes the key for compounding the MXene material with a hydrophobic epoxy resin material.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problems in the prior art and provide a safe, reliable, simple and feasible preparation method of the epoxy resin/MXene composite material.
The technical scheme is as follows: the preparation method of the epoxy resin/MXene composite material is characterized by comprising the following steps:
step 2, preparation of single-layer MXene: m to be prepared in step onen+1AlCnGrinding the ceramic material to obtain Mn+1AlCnCeramic powder, M preparedn+1AlCnSieving ceramic powder to 100-1200 mesh, corroding with mixed solution of hydrochloric acid and lithium fluoride or hydrofluoric acid, washing the corrosion product with clear water, and ultrasonic treating with methyl tetrahydrophthalic anhydride suspensionLayering and centrifuging to obtain the product, wherein the step 1 specifically comprises the following steps:
step 2.1 preparation of 1g of Mn+1AlCnAdding the ceramic powder into 5-25 ml of a mixed solution of 9-12 mol/ml hydrochloric acid and 0.2-2 g of lithium fluoride, or adding 5-25 ml of an aqueous solution with 10-70% HF content, adding a magnetic rotor, stirring for 12-96 h in an oil bath environment at 20-70 ℃, and removing Mn+1AlCnAn Al atomic layer of (1);
step 2.2, washing the corroded mixture suspension by using 5-100 ml of deionized water, centrifuging, pouring out the supernatant, and repeating for multiple times until the pH value of the supernatant is more than or equal to 6;
step 2.3, washing with 5-100 ml of absolute ethyl alcohol, centrifuging, pouring out supernatant, and repeating for 1-3 times;
step 2.4, adding 5-30 ml of methyl tetrahydrophthalic anhydride into the obtained precipitate, introducing Ar gas for protection, performing ultrasonic treatment for 0.5-3 h, centrifuging the obtained suspension for 10-120 min, and obtaining the upper layer solution which is the required single-layer Mn+1Cn（n=1,2, 3) colloidal solution mixed with methyl tetrahydrophthalic anhydride.
Step 3, determining the addition amount of single-layer MXene: and (3) obtaining the mass of the single-layer MXene in the suspension with the volume difference between the mass of the single-layer MXene and the mass of the methyl tetrahydrophthalic anhydride with the volume difference and the mass of the pure methyl tetrahydrophthalic anhydride with the same volume difference, wherein the step 3 specifically comprises the following steps:
step 3.1, extracting a certain amount of mass of the methyl tetrahydrophthalic anhydride, and calculating the mass M of the used methyl tetrahydrophthalic anhydride in unit volume1；
Step 3.2, extracting a certain amount of MXene colloidal solution, and calculating the mass M of the MXene colloidal solution in unit volume2；
Step 3.3, by calculating M2-M1The mass of MXene in the colloidal solution per unit volume can be obtained.
Step 4, preparation of the epoxy resin/MXene composite material: uniformly mixing the monolayer MXene quantitatively obtained in the third step with the suspension of the methyl tetrahydrophthalic anhydride, the curing agent, the accelerator and the epoxy resin, pouring the mixture into a mold after vacuum defoaming, and heating and curing the mixture by using an oven to obtain the epoxy resin modified MXene modified master batch; the tensile breaking stress of the epoxy resin/MXene composite material can be increased by more than 40%, the tensile breaking strain can be increased by more than 100%, and the step 4 specifically comprises the following steps:
step 4.1, calculating the amount of the needed MXene colloidal solution according to the mass of the prepared epoxy resin and the designed MXene addition amount;
4.2, calculating the mass of the E51 resin and the methyl tetrahydrophthalic anhydride according to the ratio of 80-90 parts of the E51 resin to 100 parts of the methyl tetrahydrophthalic anhydride;
4.3, in order to accelerate the curing speed, 0.1-0.5% by mass of tris- (dimethylaminomethyl) phenol can be added;
step 4.4, uniformly mixing the E51 resin, the MXene colloidal solution, the methyl tetrahydrophthalic anhydride and the tris- (dimethylaminomethyl) phenol, and defoaming for 10-60 min in vacuum;
and 4.5, preheating a casting mold at 80-100 ℃, curing at 80-130 ℃ for 2-4 h after casting, heating to 100-160 ℃, curing for 6-10 h, and cooling in a furnace to obtain the epoxy resin/MXene composite material.
And further, after casting, curing for 1h at 90 ℃, heating to 110 ℃ and curing for 4h, and then cooling along with the furnace to obtain the epoxy resin/MXene composite material.
Furthermore, the addition amount of MXene in the epoxy resin/MXene composite material is 0-600% by mass.
Further, the epoxy resin is E51 type resin, and the curing agent is methyl tetrahydrophthalic anhydride.
Further, the mass ratio of the E51 type resin to the methyl tetrahydrophthalic anhydride is 100: 70-100; preferably, the mass ratio of the E51 type resin to the methyl tetrahydrophthalic anhydride is 100: 85.
Further, the accelerator is tris- (dimethylaminomethyl) phenol, and the mass percent of the tris- (dimethylaminomethyl) phenol is 0.1-0.5%; preferably, the mass percent of the tris- (dimethylaminomethyl) phenol is 0.3%.
Compared with the prior art, the invention has the following outstanding advantages:
(1) the preparation method of the novel epoxy resin/Mxene composite material effectively compounds the single-layer MXene and the hydrophobic epoxy resin material which are originally produced in the water environment, and is simple in process, short in time, high in efficiency and low in cost.
(2) The method has easily-controlled conditions, can accurately quantify the addition amount of the single-layer MXene, and can prepare the composite materials with different MXene addition proportions.
(3) The epoxy resin/Mxene composite material prepared by the method has the advantages of obviously improved tensile breaking strength, increased elastic modulus and excellent mechanical property.
Drawings
FIG. 1 is a photograph of a tensile specimen of an epoxy resin/Mxene composite material prepared by the method of the present invention and pure epoxy resin, along with Ti in the composite material3C2The mass fraction of (2) is increased, and the color of the sample is deepened;
FIG. 2 is the tensile stress at break of the epoxy resin/Mxene composite material prepared by the method of the present invention, wherein the ordinate is the tensile stress at break and the abscissa is Ti in the composite material3C2Mass fraction of (c).
Detailed Description
The following detailed description of the embodiments of the invention, which is provided as part of the specification and which is intended to illustrate the principles of the invention by way of example, features and advantages of the invention will become apparent from the detailed description.
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination between the specific embodiments.
Example 1: the preparation method of the epoxy resin/Mxene composite material comprises the following steps:
(1) uniformly mixing Ti, Al and C powder according to a molar ratio of 3:1.2:2, preparing a high-purity ternary layered Ti3AlC2 ceramic block material at 1500 ℃ through a pressureless sintering process, drilling the prepared Ti3AlC2 ceramic material into powder by using a drilling machine to obtain Ti3AlC2 ceramic powder, and sieving the prepared Ti3AlC2 ceramic powder with a 200-mesh sieve;
(2) adding 1g of prepared Ti3AlC2 ceramic powder into 10ml of mixed solution of hydrochloric acid with the concentration of 12mol/ml and 1g of lithium fluoride, adding a magnetic rotor, stirring for 48 hours in an oil bath environment at 40 ℃, and corroding an Al atomic layer in Ti3AlC 2;
(3) washing the corroded suspension of the mixture with 40ml of deionized water, centrifuging, pouring out the supernatant, and repeating the steps until the pH value of the supernatant is more than or equal to 6;
(4) washing with 40ml of absolute ethanol, centrifuging, pouring out the supernatant, and repeating for 2 times;
(5) adding 20ml of methyl tetrahydrophthalic anhydride into the obtained precipitate, introducing Ar gas for protection, performing ultrasonic treatment for 2h, centrifuging the obtained suspension for 2h, and extracting the upper-layer colloidal solution for sealing and storing.
Step 2, determination of MXene quality:
(1) the mass of 1.0ml of methyl tetrahydrophthalic anhydride was extracted, and the mass of 1.0ml of methyl tetrahydrophthalic anhydride used was calculated to be 1.2262 g;
(2) extracting 1.0ml of MXene colloidal solution, and calculating the mass of 1.0ml of the prepared MXene colloidal solution to be 1.2488 g;
(3) calculated to give 0.0226g of MXene in 1.0ml of colloidal solution.
Step 3, preparation of MXene-epoxy resin composite material
(1) The prepared epoxy resin is 35g, and the planned added MXene mass fractions are 0.01%, 0.05%, 0.1%, 0.2% and 0.5%, so that the MXene colloidal solution needs 0.15ml, 0.77ml, 1.55ml, 3.10ml and 7.75ml respectively;
(2) taking E51 resin: methyl tetrahydrophthalic anhydride =100:85, 18.92g of E51 resin is required to prepare 35g of epoxy resin; after the methyl tetrahydrophthalic anhydride is removed from the MXene colloidal solution, 15.90g, 15.14g, 14.18g, 12.28g and 6.58g are needed;
(3) 0.3 mass% of tris- (dimethylaminomethyl) phenol, 0.105g was added;
(4) uniformly mixing E51 resin, MXene colloidal solution, methyl tetrahydrophthalic anhydride and tris- (dimethylaminomethyl) phenol, and placing in a vacuum defoaming bucket for standing for 30 min;
(5) preheating a casting mold at 100 ℃, carrying out vacuum treatment on the mixed solution, then carrying out casting, respectively curing at 130 ℃ for 2h and 160 ℃ for 8h, cooling along with a furnace, and taking out the MXene-epoxy resin composite material.
In this example, after 5 composite material samples with different Ti3C2 mass fractions are prepared and stretched, as shown in fig. 1, as the mass fraction of Ti3C2 in the composite material increases, the color of the sample deepens; the tensile breaking stress test of the composite material is carried out, and the result is shown in figure 2, the tensile breaking stress and the tensile breaking strain of the epoxy resin-MXene composite material prepared by the method are obviously increased, the elastic modulus can be improved, and the mechanical property is good.
Example 2: the preparation method of the MXene-epoxy resin composite material comprises the following steps:
(1) uniformly mixing Ti, Al and C powder according to a molar ratio of 3:1.2:2, preparing a high-purity ternary layered Ti3AlC2 ceramic block material at 1500 ℃ by a pressureless sintering process, and drilling the prepared Ti3AlC2 ceramic material into powder by a drilling machine to obtain Ti3AlC2 ceramic powder. The prepared Ti3AlC2 ceramic powder is sieved by a 325-mesh sieve;
(2) preparing two parts in total, adding 15ml of a mixed solution of hydrochloric acid with the concentration of 10mol/ml and 1g of lithium fluoride into each part of Ti3AlC2 ceramic powder prepared by 1g, adding a magnetic rotor, stirring for 72 hours in an oil bath environment at 50 ℃, and corroding an Al atomic layer in Ti3AlC 2;
(3) washing the corroded suspension of the mixture with 45ml of deionized water, centrifuging, pouring out the supernatant, and repeating the steps until the pH value of the supernatant is more than or equal to 6;
(4) transferring the two precipitates into a centrifuge tube, washing with 45ml of absolute ethyl alcohol and centrifuging, pouring out the supernatant, and repeating for 2 times;
(5) adding 20ml of methyl tetrahydrophthalic anhydride into the obtained precipitate, introducing Ar gas for protection, performing ultrasonic treatment for 0.5h, centrifuging the obtained suspension for 30min, and extracting the upper layer colloidal solution for sealing and storing.
Step 2, determination of MXene quality:
(1) the mass of 1.0ml of methyl tetrahydrophthalic anhydride was extracted, and the mass of 1.0ml of methyl tetrahydrophthalic anhydride used was calculated to be 1.2262 g;
(2) extracting 1.0ml of MXene colloidal solution, and calculating the mass of 1.0ml of the prepared MXene colloidal solution to be 1.2713 g;
(3) calculated to give a mass of MXene of 0.0451g in 1.0ml of colloidal solution.
Step 3, preparation of MXene-epoxy resin composite material
(1) The prepared epoxy resin is 35g, and the planned added MXene mass fractions are 0.05%, 0.1%, 0.2%, 0.5% and 1.0%, so that the MXene colloidal solution needs 0.39ml, 0.78ml, 1.55ml, 3.88ml and 7.76ml respectively;
(2) taking E51 resin: methyl tetrahydrophthalic anhydride =100:85, 18.92g of E51 resin is required to prepare 35g of epoxy resin; 15.60g, 15.12g, 14.18g, 11.32g and 6.56g are respectively needed after the methyl tetrahydrophthalic anhydride is removed from the MXene colloidal solution;
(3) 0.3 mass% of tris- (dimethylaminomethyl) phenol, 0.105g was added;
(4) uniformly mixing E51 resin, MXene colloidal solution, methyl tetrahydrophthalic anhydride and tris- (dimethylaminomethyl) phenol, and placing in a vacuum defoaming barrel for standing for 30 min;
(5) preheating a casting mold at 80 ℃, carrying out vacuum treatment on the mixed solution, then carrying out casting, respectively curing at 80 ℃ for 4h and 120 ℃ for 10h, cooling along with a furnace, and taking out the MXene-epoxy resin composite material.
Example 3: the preparation method of the epoxy resin/Mxene composite material comprises the following steps:
(1) uniformly mixing Ta, Al and C powder according to the molar ratio of 2:1.2:1, preparing a high-purity ternary layered Ta2AlC ceramic block material at 1200 ℃ through a pressureless sintering process, and drilling the prepared Ta2AlC ceramic material into powder by using a drilling machine to obtain Ta2AlC ceramic powder. Sieving the prepared Ta2AlC ceramic powder with a 200-mesh sieve;
(2) adding 1g of prepared Ta2AlC ceramic powder into 10ml of aqueous solution with the HF content of 50%, adding a magnetic rotor, stirring for 72 hours in an oil bath environment at 50 ℃, and corroding an Al atomic layer in the Ta2 AlC;
(3) washing the corroded suspension of the mixture with 40ml of deionized water, centrifuging, pouring out the supernatant, and repeating the steps until the pH value of the supernatant is more than or equal to 6;
(4) washing with 40ml of absolute ethanol, centrifuging, pouring out the supernatant, and repeating for 2 times;
(5) adding 20ml of methyl tetrahydrophthalic anhydride into the obtained precipitate, introducing Ar gas for protection, performing ultrasonic treatment for 2h, centrifuging the obtained suspension for 2h, and extracting the upper-layer colloidal solution for sealing and storing.
Step 2, determination of MXene quality:
(1) the mass of 1.0ml of methyl tetrahydrophthalic anhydride was extracted, and the mass of 1.0ml of methyl tetrahydrophthalic anhydride used was calculated to be 1.2262 g;
(2) extracting 1.0ml of MXene colloidal solution, and calculating the mass of 1.0ml of the prepared MXene colloidal solution to be 1.2488 g;
(3) the mass of MXene in 1.0ml of colloidal solution was found to be 0.0226g by calculation.
Step 3, preparation of MXene-epoxy resin composite material
(1) The prepared epoxy resin is 35g, and the planned added MXene mass fractions are 0.01%, 0.05%, 0.1%, 0.2% and 0.5%, so that the MXene colloidal solution needs 0.15ml, 0.77ml, 1.55ml, 3.10ml and 7.75ml respectively;
(2) taking E51 resin: methyl tetrahydrophthalic anhydride =100:85, 18.92g of E51 resin is required to prepare 35g of epoxy resin; after the methyl tetrahydrophthalic anhydride is removed from the MXene colloidal solution, 15.90g, 15.14g, 14.18g, 12.28g and 6.58g are needed;
(3) 0.3 mass% of tris- (dimethylaminomethyl) phenol, 0.105g was added;
(4) uniformly mixing E51 resin, MXene colloidal solution, methyl tetrahydrophthalic anhydride and tris- (dimethylaminomethyl) phenol, and placing in a vacuum defoaming barrel for standing for 30 min;
(5) preheating a casting mold at 100 ℃, carrying out vacuum treatment on the mixed solution, then casting, respectively curing at 130 ℃ for 2h and 160 ℃ for 8h, cooling along with a furnace, and taking out the MXene-epoxy resin composite material
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any simple modifications of the above embodiments according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (6)
1. The preparation method of the epoxy resin/MXene composite material is characterized by comprising the following steps:
step 1, preparing metal ceramic MAX: mixing Ti, Al and C powder, and sintering at high temperature and no pressure to obtain Ti3AlC2A block body;
step 2, preparation of single-layer MXene: ti prepared in the step one3AlC2Grinding the block by milling, etching Ti with a mixture of hydrochloric acid and lithium fluoride or hydrofluoric acid3AlC2Washing the corrosion product with clear water for multiple times on the Al atomic layer, and carrying out ultrasonic layering and centrifugation on the methyl tetrahydrophthalic anhydride suspension to obtain the Al atomic layer;
step 3, determining the addition amount of single-layer MXene: the mass of the single-layer MXene and the suspension of the methyl tetrahydrophthalic anhydride prepared in the second step is different from the mass of the pure methyl tetrahydrophthalic anhydride with the same volume, so that the mass of the single-layer MXene in the suspension with the volume is obtained;
step 4, preparation of the epoxy resin/MXene composite material: uniformly mixing the monolayer MXene quantitatively obtained in the third step with the suspension of the methyl tetrahydrophthalic anhydride, the curing agent, the accelerator and the epoxy resin, pouring the mixture into a mold after vacuum defoaming, and heating and curing the mixture by using an oven to obtain the epoxy resin modified MXene modified master batch;
the epoxy resin is E51 type resin, the curing agent is methyl tetrahydrophthalic anhydride, and the mass ratio of the E51 type resin to the methyl tetrahydrophthalic anhydride is 100: 70-100;
the accelerant is tris- (dimethylaminomethyl) phenol, and the mass percentage of the tris- (dimethylaminomethyl) phenol is 0.1-0.5%.
2. The method for preparing the epoxy resin/MXene composite material according to claim 1, wherein the step 2 comprises the steps of:
step 2.1,1g of prepared Ti3AlC2Adding the ceramic powder into 5-25 ml of a mixed solution of 9-12 mol/ml hydrochloric acid and 0.2-2 g of lithium fluoride, or adding 5-25 ml of an aqueous solution with 10-70% HF content, adding a magnetic rotor, stirring for 12-96 h in an oil bath environment at 20-70 ℃, removing Ti3AlC2An Al atomic layer;
step 2.2, washing the corroded mixture suspension by using 5-100 ml of deionized water, centrifuging, pouring out the supernatant, and repeating for multiple times until the pH value of the supernatant is more than or equal to 6;
step 2.3, washing with 5-100 ml of absolute ethyl alcohol, centrifuging, pouring out the supernatant, and repeating for 1-3 times;
step 2.4, adding 5-30 ml of methyl tetrahydrophthalic anhydride into the obtained precipitate, introducing Ar gas for protection, performing ultrasonic treatment for 0.5-3 h, centrifuging the obtained suspension for 10-120 min, and obtaining the upper layer solution which is the required single-layer Ti3C2Colloidal solution mixed with methyl tetrahydrophthalic anhydride.
3. The method for preparing the epoxy resin/MXene composite material according to claim 1, wherein the step 3 comprises the steps of:
step 3.1, extracting a certain amount of mass of the methyl tetrahydrophthalic anhydride, and calculating the mass M of the used methyl tetrahydrophthalic anhydride in unit volume1；
Step 3.2, extracting a certain amount of MXene colloidal solution, and calculating the mass M of the MXene colloidal solution in unit volume2；
Step 3.3, by calculating M2-M1The mass of MXene in the colloidal solution per unit volume can be obtained.
4. The method for preparing the epoxy resin/MXene composite material according to claim 1, wherein the mass ratio of the E51 type resin to the methyl tetrahydrophthalic anhydride is 100: 85.
5. The method for preparing the epoxy resin/MXene composite material according to claim 1, wherein tris- (dimethylaminomethyl) phenol is present in an amount of 0.3% by weight.
6. The method for preparing the epoxy resin/MXene composite material according to claim 1, wherein the step 4 comprises the steps of:
step 4.1, calculating the amount of the needed MXene colloidal solution according to the mass of the prepared epoxy resin and the designed MXene addition amount;
4.2, calculating the mass of the required E51 resin and the required methyl tetrahydrophthalic anhydride according to the ratio of 80-90 parts of methyl tetrahydrophthalic anhydride to 100 parts of E51 resin;
4.3, in order to accelerate the curing speed, 0.1-0.5% by mass of tris- (dimethylaminomethyl) phenol can be added;
step 4.4, uniformly mixing the E51 resin, the MXene colloidal solution, the methyl tetrahydrophthalic anhydride and the tris- (dimethylaminomethyl) phenol, and defoaming in vacuum for 10-60 min;
and 4.5, preheating a casting mold at 80-100 ℃, curing at 80-130 ℃ for 2-4 h after casting, heating to 100-160 ℃, curing for 6-10 h, and cooling in a furnace to obtain the epoxy resin/MXene composite material.
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| CN110452497B (en) * | 2019-09-12 | 2021-07-09 | 清华大学 | Insulating material and preparation method thereof |
| CN112226644B (en) * | 2020-09-25 | 2021-12-28 | 河海大学 | MXene reinforced copper-based composite material and preparation method thereof |
| CN112111131B (en) * | 2020-09-25 | 2021-11-30 | 河海大学 | Carbon fiber-epoxy resin composite material with improved MXene and improving method |
| CN112142472B (en) * | 2020-09-25 | 2021-10-15 | 河海大学 | Cr (chromium)2AlC/MXene composite material and preparation method thereof |
| CN114874585A (en) * | 2022-05-05 | 2022-08-09 | 哈尔滨工业大学 | Preparation method of MXene reinforced resin matrix composite material |
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