CN115466898B - Preparation method of graphene oxide intercalation two-dimensional high-entropy alloy - Google Patents
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Abstract
The invention provides a preparation method of graphene oxide intercalation two-dimensional high-entropy alloy, which comprises the following steps: mixing the graphene with the functionalized surface with a solvent to form a graphene solution; and mixing the metal salt solution with the graphene solution, heating and refluxing, centrifuging, drying, and calcining in air to obtain the graphene oxide intercalation two-dimensional high-entropy alloy. According to the preparation method, the graphene is subjected to surface modification by glucose with polyhydroxy, the graphene with polyhydroxy on the two-dimensional surface is used as a lamellar structure inducer, and metal salts are uniformly and high-density dispersed on the surface of the graphene through coordination and electrostatic attraction, so that the graphene intercalation two-dimensional lamellar high-entropy alloy material is prepared by a one-step roasting method. Compared with the traditional preparation method of the high-entropy alloy, the grinding process is avoided, the obtained material is a lamellar material, the porous structure is provided, the specific surface area is relatively high, and the effect of cocktail is obvious. This improves the application potential of the high-entropy alloy in the fields of catalysis, sensing and the like.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a preparation method and application of graphene oxide intercalation two-dimensional high-entropy alloy.
Background
The high-entropy alloy is a novel metal material which appears in recent decades, is generally composed of 5 or more elements with equal atomic ratio or near equal atomic ratio, and is used for preparing devices and special mechanical materials under extreme conditions due to multiple effects such as high mixed entropy, slow diffusion of atoms, cocktail effect and the like, and the high-entropy alloy shows high strength, high toughness, high hardness and exceptionally excellent low-temperature toughness. In recent years, the internal multi-electron effect and redox behavior thereof have been found to be useful in the field of electrocatalysis and thermocatalysis.
The existing preparation of the high-entropy alloy generally comprises the steps of roasting metal powder at high temperature to obtain solid solution, and then ball milling to obtain powder, so that the process energy consumption is high, the equipment loss is high, and the obtained high-entropy alloy has high surface energy nano particles, easy agglomeration and low specific surface area, so that the application of the high-entropy alloy in the catalysis field is restricted.
Qiao et al in 2020 utilize graphene and metal salts to generate electrostatic interaction, and prepare two-dimensional high-entropy alloy Co through roasting 0.2 Ni 0.2 Cu 0.2 Mg 0.2 Zn 0.2 O, however, the graphene surface has fewer functional groups and weak interaction with metal.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a preparation method of graphene oxide intercalation two-dimensional high-entropy alloy. The preparation method can avoid a complicated grinding process, and meanwhile, the obtained high-entropy alloy material is a two-dimensional lamellar material, has a pore structure, relatively high specific surface area and obvious cocktail effect. The application potential of the high-entropy alloy in the fields of catalysis, sensing and the like is improved.
The first aspect of the invention provides a preparation method of graphene oxide intercalation two-dimensional high-entropy alloy, which comprises the following steps:
s1, mixing surface functionalized graphene with a solvent to form a graphene solution;
s2, respectively adding a Ti metal salt solution, a Mn metal salt solution, a Ce metal salt solution, a Ni metal salt solution and a W metal salt solution into the graphene solution obtained in the S1 to form uniform turbid liquid;
s3, mixing the turbid liquid obtained in the step S2 with the graphene solution obtained in the step S1, heating and refluxing, centrifuging and drying to obtain a solid 1;
and S4, calcining the solid 1 obtained in the step S3 in air to obtain the graphene oxide intercalation two-dimensional high-entropy alloy.
According to some preferred embodiments of the preparation method of the present invention, in S1, the surface functionalized graphene has a thickness of 0.5 to 2nm; and/or the surface functionalized graphene surface contains at least one of hydroxyl and carboxyl functional groups.
According to some preferred embodiments of the preparation method of the present invention, in S1, the surface functionalized graphene is prepared according to the following method: adding polyhydroxy saccharides into the water dissolved with the graphene, heating, stirring for a period of time, and centrifuging to obtain the graphene with the functionalized surface; preferably, the mass fraction of the polyhydroxy saccharide solution is 5-15%.
According to some preferred embodiments of the preparation method of the present invention, in S1, the reaction conditions include: heating to 60-90 ℃; and/or stirring for 2-4 h.
According to some preferred embodiments of the preparation method of the present invention, in S1, the solvent is selected from at least one of water, ethanol, ethylene glycol and glycerol.
According to some preferred embodiments of the preparation method of the present invention, in S2, a metal salt solution of Ti is addedMetal salt solution of Mn, metal salt solution of Ce, metal salt solution of Ni, and metal salt solution of w, ti contained in 4+ 、Mn 2+ 、Ce 3+ 、Ni 2+ And W 6+ Having the same molar amount.
According to some preferred embodiments of the preparation method of the present invention, the metal salt of Ti is selected from at least one of isopropyl titanate and n-butyl titanate.
According to some preferred embodiments of the preparation method of the present invention, the metal salt of Mn is selected from at least one of manganese nitrate, manganese acetate, manganese chloride.
According to some preferred embodiments of the preparation method of the present invention, the metal salt of Ce is at least one selected from cerium nitrate, cerium chloride and cerium acetate.
According to some preferred embodiments of the preparation method of the present invention, the metal salt of Ni is selected from at least one of nickel chloride, nickel acetate and nickel nitrate.
According to some preferred embodiments of the preparation method of the present invention, the metal salt of W is selected from at least one of tungsten hexachloride and ammonium metatungstate.
According to some preferred embodiments of the preparation method of the present invention, in S3, the reaction conditions include: the heating reflux temperature is 80-140 ℃; and/or heating reflux time is 4-10 h.
According to some preferred embodiments of the preparation method of the present invention, in S4, the reaction conditions include: the calcination temperature is 800-1000 ℃.
The second aspect of the invention provides application of the graphene oxide intercalation two-dimensional high-entropy alloy prepared by the preparation method in the field of denitration.
The invention has the beneficial effects that:
according to the preparation method, glucose with polyhydroxy is adopted to carry out surface modification on graphene, so that the surface of the graphene is covered with a large number of hydroxyl groups, then graphene with two-dimensional surface polyhydroxy is used as a lamellar structure inducer, metal salts are uniformly and high-density dispersed on the surface of the graphene through coordination and electrostatic attraction, and the graphene intercalation two-dimensional lamellar high-entropy alloy material is prepared through a one-step roasting method. Compared with the traditional high-entropy alloy preparation method, the graphene induction method can avoid the grinding process, and meanwhile, the obtained material is a lamellar material, has a pore structure, is relatively high in specific surface area and has an obvious "cocktail" effect. This improves the application potential of the high-entropy alloy in the fields of catalysis, sensing and the like.
Drawings
FIG. 1 (a) is an XRD pattern of the graphene intercalated high-entropy alloy prepared in example 1;
FIG. 1 (b) is N of the graphene intercalated high-entropy alloy prepared in example 1 2 Adsorption-desorption isotherms.
Detailed Description
The present invention will be described in detail with reference to examples, but the scope of the present invention is not limited to the following description.
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products available commercially without the manufacturer's knowledge.
In the following embodiments, the preparation method of the graphene oxide intercalation two-dimensional high-entropy alloy is as follows, if not specifically described, including:
1. adding polyhydroxy saccharides into the water dissolved with the graphene, heating, stirring for a period of time, and centrifuging to obtain the graphene with the functionalized surface; heating at 60-90 deg.c and stirring for 2-4 hr.
2. Mixing the surface functionalized graphene with a solvent to form a graphene solution.
3. Respectively adding a Ti metal salt solution, a Mn metal salt solution, a Ce metal salt solution, a Ni metal salt solution and a W metal salt solution into the graphene solution obtained in the step 2 to form turbid liquid;
4. mixing the turbid liquid obtained in the step 3 with the graphene solution obtained in the step 2, heating and refluxing, centrifuging and drying to obtain a solid 1; the heating reflux temperature is 80-120 ℃, and the heating reflux time is 4-10 h.
5. Calcining the solid 1 obtained in the step 4 in air to obtain the graphene oxide intercalation two-dimensional high-entropy alloy.
[ example 1 ]
1. 1.0g of graphene oxide is added into 200mL of glucose solution (5 wt%) and stirred for 3 hours at 80 ℃, cooled and centrifuged to obtain the surface hydroxyl modified graphene.
2. Ultrasonically dispersing 0.5g of surface modified graphene powder in 200mL of mixed solvent of water and ethylene glycol to form graphene solution; wherein the volume ratio of water to glycol is 1:9.
3. Adding 0.170g of n-butyl titanate, 0.0865g of manganese acetate, 0.158g of cerium acetate, 0.088g of nickel acetate and 0.198g of tungsten hexachloride into 500mL of ethylene glycol, and uniformly stirring to form a turbid liquid;
4. slowly and dropwise adding the solution obtained in the step 3 into the graphene solution obtained in the step 2, heating to 100 ℃ and carrying out reflux reaction for 4 hours. And (3) centrifuging to obtain a solid 1, and drying in vacuum at the temperature of 60-80 ℃.
5. And (3) calcining the solid 1 obtained in the step (4) in air at 900 ℃ for 1h to obtain the graphene intercalation two-dimensional high-entropy alloy.
Fig. 1 (a) is an XRD pattern of the prepared two-dimensional high-entropy alloy, and it can be seen that characteristic diffraction peaks appear at 2θ=38.6, 44.9, 65.3, 78.2, belonging to multiphase crystals of the alloy, and proving that the synthesized point metal is a high-entropy alloy material.
FIG. 1 (b) is N of a graphene intercalated two-dimensional high-entropy alloy prepared 2 Adsorption and desorption isothermal curves, it can be seen that the prepared alloy has a pore structure, and the specific surface area of the sample is 39.3m2/g.
[ example 2 ]
1. 1.0g of graphene oxide is added into 200mL of fructose solution (5 wt%) and stirred for 3 hours at 80 ℃, cooled and centrifuged to obtain the surface hydroxyl modified graphene.
2. Ultrasonically dispersing 0.5g of surface modified graphene powder in 200mL of mixed solvent of water and glycerol to form graphene solution; wherein the volume ratio of water to glycerol is 1:9.
3. Adding 0.170g of n-butyl titanate, 0.0865g of manganese acetate, 0.158g of cerium acetate, 0.088g of nickel acetate and 0.198g of tungsten hexachloride into 500mL of ethylene glycol, and uniformly stirring to form a turbid liquid;
4. slowly dripping the turbid liquid obtained in the step 3 into the graphene solution obtained in the step 2, heating to 100 ℃ and carrying out reflux reaction for 4 hours. And (3) centrifuging to obtain a solid 1, and drying in vacuum at the temperature of 60-80 ℃.
5. And (3) calcining the solid 1 obtained in the step (4) in air at 900 ℃ for 1h to obtain the graphene intercalation two-dimensional high-entropy alloy.
[ example 3 ]
1. 1.0g of graphene oxide is added into 200mL of chitosan solution (5 wt%) and stirred for 3 hours at 80 ℃, cooled and centrifuged to obtain the surface hydroxyl modified graphene.
2. Ultrasonically dispersing 0.5g of surface modified graphene powder in 200mL of a mixed solvent of ethylene glycol and glycerol to form a graphene solution; wherein the volume ratio of the glycol to the glycerol is 1:4.
3. Adding 0.170g of n-butyl titanate, 0.0865g of manganese acetate, 0.158g of cerium acetate, 0.088g of nickel acetate and 0.198g of tungsten hexachloride into 500mL of ethylene glycol, and uniformly stirring to form a turbid liquid;
4. slowly dripping the turbid liquid obtained in the step 3 into the graphene solution obtained in the step 2, heating to 100 ℃ and carrying out reflux reaction for 4 hours. And (3) centrifuging to obtain a solid 1, and drying in vacuum at the temperature of 60-80 ℃.
5. And (3) calcining the solid 1 obtained in the step (4) in air at 900 ℃ for 1h to obtain the two-dimensional high-entropy alloy.
[ example 4 ]
1. 1.0g of graphene oxide is added into 200mL of glucose solution (5 wt%) and stirred for 3 hours at 80 ℃, cooled and centrifuged to obtain the surface hydroxyl modified graphene.
2. Ultrasonically dispersing 0.5g of surface modified graphene powder in 200mL of a mixed solvent of ethylene glycol and glycerol to form a graphene solution; wherein the volume ratio of water to glycerol is 1:4.
3. Adding 0.170g of n-butyl titanate, 0.063g of manganese chloride, 0.158g of cerium acetate, 0.067g of nickel chloride and 0.198g of tungsten hexachloride into 500mL of ethylene glycol, and uniformly stirring to form turbid liquid;
4. slowly dripping the turbid liquid obtained in the step 3 into the graphene solution obtained in the step 2, heating to 100 ℃ and carrying out reflux reaction for 4 hours. And (3) centrifuging to obtain a solid 1, and drying in vacuum at the temperature of 60-80 ℃.
5. And (3) calcining the solid 1 obtained in the step (4) in air at 900 ℃ for 1h to obtain the two-dimensional high-entropy alloy.
[ example 5 ]
Example 5 is essentially the same as example 1, except that the heating reflux temperature in step 4 is 120 ℃. Finally, the two-dimensional high-entropy alloy is obtained.
[ example 6 ]
Example 6 is substantially the same as example 1 except that the heating reflux temperature in step 4 is 140 ℃. Finally, the two-dimensional high-entropy alloy is obtained.
[ example 7 ]
Example 7 is essentially the same as example 1, except that the calcination temperature in step 5 is 1000 ℃. Finally, the two-dimensional high-entropy alloy is obtained.
[ example 8 ]
Example 8 is essentially the same as example 1, except that the calcination temperature in step 5 is 800 ℃. Finally, the two-dimensional high-entropy alloy is obtained.
[ example 9 ]
Example 9 is substantially the same as example 1 except that the heating reflux temperature in step 4 is 80 ℃. Finally, the two-dimensional high-entropy alloy is obtained.
[ example 10 ]
Example 10 was substantially the same as example 1 except that the heating reflux temperature in step 4 was 60 ℃. Finally, the two-dimensional high-entropy alloy is obtained.
[ example 11 ]
Example 11 is essentially the same as example 8, except that the calcination temperature in step 5 is 700 ℃. Finally, the two-dimensional high-entropy alloy is obtained.
[ example 12 ]
Example 12 is essentially the same as example 8, except that the calcination temperature in step 5 is 600 ℃. Finally, the two-dimensional high-entropy alloy is obtained.
Comparative example 1
Comparative example 5 is substantially the same as example 4 except that graphene oxide whose surface is not modified is used. Finally, the two-dimensional high-entropy alloy with the block structure is prepared.
The two-dimensional high-entropy alloys prepared in examples 1-8 and comparative examples 1-5 were used in SCR denitration reactions, and the specific steps are as follows:
at a temperature in the range of 300 ℃, the inlet NO concentration is 2000mg/Nm 3 Under the condition of catalyst Ti 0.2 Mn 0.2 Ce 0.2 Ni 0.2 W 0.2 The filling volume of O is 10mL, the test temperature is 300-350 ℃, and the test airspeed is 20000h -1 The system pressure was 0.10Mpa.
Table 1 table of preparation parameters and denitration properties of different examples of high entropy alloys
As can be seen from Table 1, the high entropy alloys prepared by using different saccharides in examples 1-3 all have good denitration activity, which indicates that the saccharides with polyhydroxy groups can effectively improve the anchoring effect of graphene on metal salts. It is seen from the denitration performance of the samples of examples 9 and 10 that the heating reflux temperature of the metal salt solution is lower than 80 ℃, resulting in a decrease in the denitration performance of the prepared high-entropy alloy. As is evident from the denitration performance of the samples of examples 11 and 12, it is demonstrated that the denitration activity of the high-entropy alloy is also lowered when the firing temperature is lower than 800 ℃. Compared with the method 1, the graphene oxide with the unmodified surface is used, the denitration performance of the high-entropy alloy prepared from the common graphene is obviously reduced, and the surface modified graphene can effectively promote the formation of the two-dimensional high-entropy alloy, so that the anchoring effect of the graphene on metal salt can be effectively improved by indirectly proving the saccharides with polyhydroxy.
It should be noted that the above-described embodiments are only for explaining the present invention and do not constitute any limitation of the present invention. The invention has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. Modifications may be made to the invention as defined in the appended claims, and the invention may be modified without departing from the scope and spirit of the invention. Although the invention is described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, as the invention extends to all other means and applications which perform the same function.
Claims (9)
1. A preparation method of graphene oxide intercalation two-dimensional high-entropy alloy applied to the field of denitration comprises the following steps:
s1, mixing surface functionalized graphene with a solvent to form a graphene solution;
s2, respectively adding a Ti metal salt solution, a Mn metal salt solution, a Ce metal salt solution, a Ni metal salt solution and a W metal salt solution into the graphene solution obtained in the S1 to form turbid liquid;
s3, mixing the turbid liquid obtained in the step S2 with the graphene solution obtained in the step S1, heating and refluxing, centrifuging and drying to obtain a solid 1; the heating reflux temperature is 80-140 ℃; and/or heating reflux time is 4-10 h;
s4, calcining the solid 1 obtained in the step S3 in air to obtain graphene oxide intercalation two-dimensional high-entropy alloy; the calcination temperature is 800-1000 ℃.
2. The method according to claim 1, wherein in S1, the surface-functionalized graphene has a thickness of 0.5 to 2nm.
3. The method of claim 1, wherein in S1, the surface-functionalized graphene surface contains at least one of hydroxyl and carboxyl functional groups.
4. The preparation method according to claim 2, wherein in S1, the surface-functionalized graphene is prepared according to the following method: and adding polyhydroxy saccharides into the water in which the graphene is dissolved, heating, stirring and centrifuging to obtain the graphene with the functionalized surface.
5. The process according to claim 4, wherein the mass fraction of the polyhydric sugar in the solution obtained after adding the polyhydric sugar is 5 to 15% by weight.
6. The method according to claim 4, wherein in S1, the reaction conditions include: the heating temperature is 60-90 ℃; and/or heating and stirring for 2-4 h.
7. The method according to claim 1, wherein in S1, the solvent is at least one selected from the group consisting of water, ethanol, ethylene glycol and glycerol.
8. The preparation method according to claim 1, wherein in S2, ti is contained in the added metal salt solution of Ti, the added metal salt solution of Mn, the added metal salt solution of Ce, the added metal salt solution of Ni and the added metal salt solution of W 4+ 、Mn 2+ 、Ce 3+ 、Ni 2+ And W 6+ In equimolar amounts.
9. The production method according to claim 1, wherein in S2, the metal salt of Ti is selected from at least one of isopropyl titanate and n-butyl titanate; and/or the number of the groups of groups,
the metal salt of Mn is selected from at least one of manganese nitrate, manganese acetate and manganese chloride; and/or the number of the groups of groups,
the metal salt of Ce is at least one of cerium nitrate, cerium chloride and cerium acetate; and/or the number of the groups of groups,
the metal salt of Ni is selected from at least one of nickel chloride, nickel acetate and nickel nitrate; and/or the number of the groups of groups,
the metal salt of W is at least one selected from tungsten hexachloride and ammonium metatungstate.
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