CN113546663A - Macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material and preparation method thereof - Google Patents
Macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 92
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 76
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 49
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 34
- 239000010439 graphite Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000006185 dispersion Substances 0.000 claims abstract description 77
- 239000007788 liquid Substances 0.000 claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 34
- 239000000017 hydrogel Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 238000000227 grinding Methods 0.000 claims abstract description 19
- 239000002211 L-ascorbic acid Substances 0.000 claims abstract description 17
- 235000000069 L-ascorbic acid Nutrition 0.000 claims abstract description 17
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 61
- 238000004108 freeze drying Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 3
- 229910052961 molybdenite Inorganic materials 0.000 description 41
- 238000003756 stirring Methods 0.000 description 23
- 239000008367 deionised water Substances 0.000 description 22
- 229910021641 deionized water Inorganic materials 0.000 description 22
- 238000010438 heat treatment Methods 0.000 description 12
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 11
- 238000003801 milling Methods 0.000 description 10
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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Abstract
The invention discloses a macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material and a preparation method thereof, and relates to the technical field of material forming modes. Mixing graphite phase carbon nitride and molybdenum disulfide, grinding, adding a solvent, and continuing grinding to obtain a dispersion liquid of the graphite phase carbon nitride and the molybdenum disulfide; uniformly dispersing graphene oxide in water to obtain a dispersion liquid of the graphene oxide; uniformly mixing the dispersion liquid of graphite-phase carbon nitride and molybdenum disulfide and the dispersion liquid of graphene oxide, adding L-ascorbic acid, and uniformly dispersing to obtain a uniform dispersion liquid; reacting the uniform dispersion liquid to obtain a hydrogel sample; and washing and drying the hydrogel sample to obtain the molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material. The invention solves the problem that graphite phase carbon nitride is easy to agglomerate, and the prepared composite material avoids the problem that the traditional powder photocatalytic material is difficult to recycle.
Description
Technical Field
The invention relates to the technical field of material forming modes, in particular to a macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material and a preparation method thereof.
Background
With the rapid development of productivity, large-scale industrial production processes generate a large amount of industrial wastewater, and the discharge of the wastewater not only pollutes the ecological environment, but also has great harm to human health, and the wastewater can be discharged after being treated. The traditional industrial wastewater treatment method mainly comprises a physical method, a chemical method and a biological method, and has the defects of limited treatment capacity, higher treatment cost and the like. In addition to the discharge of waste water, industrial production consumes a large amount of fossil energy, and hydrogen has high combustion heat value, zero pollution and easy storage, and is considered as an ideal substitute of fossil fuel. Has immeasurable prospect in the aspects of solving the increasingly scarce earth energy and environmental pollution, etc. The traditional hydrogen production method mainly comprises the steps of producing hydrogen by a water gas method, preparing natural gas by petroleum thermal cracking, producing hydrogen, producing electrolyzed water and the like, but the traditional hydrogen production method has the defects of high treatment cost, more byproducts and the like.
g-C3N4(graphite phase carbon nitride) as a metal-free visible light photocatalyst has been widely studied due to its unique semiconductor band structure and excellent chemical stability, but its g-C is limited due to its easy aggregation between sheets and easy recombination of electrons and holes3N4The application in the field of photocatalysis.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material and a preparation method thereof, so that the problem that graphite phase carbon nitride is easy to agglomerate is solved, and the prepared composite material avoids the problem that the conventional powder photocatalytic material is difficult to recover.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a preparation method of a macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material, which comprises the following steps:
1) mixing graphite phase carbon nitride and molybdenum disulfide, grinding to obtain a mixed sample, adding a solvent into the mixed sample, and continuing grinding to obtain a dispersion liquid of the graphite phase carbon nitride and the molybdenum disulfide; uniformly dispersing graphene oxide in water to obtain a dispersion liquid of the graphene oxide; 2) uniformly mixing the obtained dispersion liquid of graphite-phase carbon nitride and molybdenum disulfide and the obtained dispersion liquid of graphene oxide, adding L-ascorbic acid, and uniformly dispersing to obtain a uniform dispersion liquid; 3) reacting the obtained uniform dispersion liquid to obtain a hydrogel sample; 4) and washing and drying the obtained hydrogel sample to obtain the macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material.
Preferably, in the step 1), the molar ratio of the graphite phase carbon nitride to the molybdenum disulfide is 1: 2-1: 6.
Preferably, in step 1), the solvent is ethylene glycol.
Preferably, in the step 1), the mixing ratio of the graphene oxide to the water is 0.05-0.1 g: 20 mL.
Further preferably, the feeding ratio of the graphene oxide to the L-ascorbic acid is 0.05-0.1 g: 0.5 to 1 g.
Preferably, in the step 3), the reaction temperature is 85-95 ℃ and the reaction time is 40-60 min.
Preferably, in step 4), the drying is performed by freeze drying.
The invention discloses a macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material prepared by adopting the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of a macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material, which is characterized in that MoS is prepared by adopting a water-bath heating method2/g-C3N4Graphene oxide hydrogel. Graphene oxide with g-C3N42D/2D contact of (a) inhibits g-C3N4The sheet layer is agglomerated, and the electron is improved in g-C3N4And MoS2Transfer rate between, MoS2And g-C3N4The formed Z-type heterojunction inhibits the recombination of electrons and holes and improves the oxidation-reduction capability. The preparation method is simple and low in cost, and the graphene oxide is molybdenum disulfide (MoS)2) And graphite phase carbon nitride (g-C)3N4) The combination of (A) provides a medium for inhibiting g-C3N4Agglomeration between lamellae and improved MoS2And g-C3N4The transmission speed of electrons between the two electrodes is reduced, and MoS is suppressed2/g-C3N4The heterojunction photoproduces electron-hole recombination. Therefore, the preparation method effectively solves the problem that the graphite phase carbon nitride is easy to agglomerate.
The macro-recoverable molybdenum disulfide/graphite-phase carbon nitride/graphene oxide composite material prepared by the preparation method is a macro-photocatalytic material, avoids the problem that the conventional powder photocatalytic material is difficult to recover, can be cut according to the working environment, has the advantages of wide photoresponse range, recyclability and low cost, and can realize sustainable development and recycling of resources.
Drawings
FIG. 1 is an SEM image and an energy spectrum of a macro-recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material according to the invention under the conditions of 18KV and 5 mL/h; wherein, (a) an SEM image magnified 20000 times, (b) an SEM image magnified 150000 times, (C) an SEM image magnified 200000 times, (d) Mo, (e) S, (f) N, and (g) C;
figure 2 is a macroscopic sample view of a macroscopically recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material according to the present invention; wherein (a) is a front view photograph and (b) is a side view photograph.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
Macro-recoverable molybdenum disulfide/graphite-phase carbon nitride/graphene oxide (MoS)2/g-C3N4Graphene oxide) composite material, comprising the following steps: the fired g-C3N4After ultrasonic dispersion, with MoS2Mixing and fully grinding, adding the mixture into the graphene oxide dispersion liquid, fully stirring, and then putting the mixture into a water bath kettle to heat in a water bath manner to obtain MoS2/g-C3N4Graphene oxide hydrogel sample, MoS obtained2/g-C3N4Oxidized stoneLyophilization of hydrogel samples of graphene to obtain macroscopically recoverable MoS2/g-C3N4Graphene oxide composite material. The method comprises the following specific steps:
step 1: dispersing ultrasonically dispersed g-C3N4And MoS2Mixing according to a certain proportion and fully grinding to obtain a mixed sample;
step 2: adding 3mL of ethylene glycol into the ground mixed sample, and continuing grinding to obtain g-C3N4And MoS2The dispersion of (1);
and step 3: g to C3N4And MoS2Adding the dispersion liquid into the dispersion liquid of the graphene oxide, and stirring for 30min to obtain a mixed dispersion liquid;
and 4, step 4: adding a certain amount of L-ascorbic acid into the mixed dispersion liquid, and stirring for 20min to obtain a uniform dispersion liquid;
and 5: putting the uniform dispersion liquid into a water bath kettle, and heating at 85-95 ℃ for 40 min-1 h to obtain a hydrogel sample;
step 6: washing the obtained hydrogel sample with deionized water for 2-3 times to remove glycol;
and 7: after washing, continuously freezing and drying to obtain MoS2/g-C3N4Graphene oxide composite material.
MoS in the step 12And g-C3N4In a molar ratio of 1: 2-1: 6 or more;
the solution of the graphene oxide dispersion liquid in the step 3 is 20mL of deionized water, and the amount of solute graphene oxide is 0.05-0.1 g.
The feeding ratio of the mass of the L-ascorbic acid in the step 4 to the mass of the graphene oxide in the step 3 is 0.05-0.1 g: 0.5 to 1 g.
The present invention is described in further detail below with reference to specific examples:
example 1
(1) The processed MoS2And g-C3N4According to a molar ratio of 1: 2, mixing and fully grinding;
(2) the milled mixed sample was added to 3mL of ethylene glycol and milling was continued.
(3) G to C3N4And MoS2Adding the dispersion liquid into a dispersion liquid of graphene oxide (the solution of the graphene oxide dispersion liquid is 20mL of deionized water, and the solute of graphene oxide is 0.05 g.), and stirring for 30 min;
(4) adding 0.5g L-ascorbic acid into the mixed dispersion, and stirring for 20 min;
(5) putting the uniform dispersion liquid into a water bath kettle, and heating for 1h at 95 ℃;
(6) washing the obtained hydrogel sample with deionized water for 2-3 times to remove glycol;
(7) freeze drying for 48h to obtain macroscopically recoverable MoS2/g-C3N4Graphene oxide composite material.
Example 2
(1) The processed MoS2And g-C3N4According to a molar ratio of 1: 3 mixing and fully grinding;
(2) the milled mixed sample was added to 3mL of ethylene glycol and milling was continued.
(3) G to C3N4And MoS2Adding the dispersion liquid into a dispersion liquid of graphene oxide (the solution of the graphene oxide dispersion liquid is 20mL of deionized water, and the solute of graphene oxide is 0.05 g.), and stirring for 30 min;
(4) adding 0.7g L-ascorbic acid into the mixed dispersion, and stirring for 20 min;
(5) putting the uniform dispersion liquid into a water bath kettle, and heating for 1h at 85 ℃;
(6) washing the obtained hydrogel sample with deionized water for 2-3 times to remove glycol;
(7) freeze drying for 48h to obtain macroscopically recoverable MoS2/g-C3N4Graphene oxide composite material.
Example 3
(1) The processed MoS2And g-C3N4According to a molar ratio of 1: 4 mixing and fully grinding;
(2) the milled mixed sample was added to 3mL of ethylene glycol and milling was continued.
(3) G to C3N4And MoS2Adding the dispersion liquid into a dispersion liquid of graphene oxide (the solution of the graphene oxide dispersion liquid is 20mL of deionized water, and the solute of graphene oxide is 0.1 g.), and stirring for 30 min;
(4) adding 0.6g L-ascorbic acid into the mixed dispersion, and stirring for 20 min;
(5) putting the uniform dispersion liquid into a water bath kettle, and heating for 1h at 90 ℃;
(6) washing the obtained hydrogel sample with deionized water for 2-3 times to remove glycol;
(7) freeze drying for 48h to obtain macroscopically recoverable MoS2/g-C3N4Graphene oxide composite material.
Example 4
(1) The processed MoS2And g-C3N4According to a molar ratio of 1: 5 mixing and fully grinding;
(2) the milled mixed sample was added to 3mL of ethylene glycol and milling was continued.
(3) G to C3N4And MoS2Adding the dispersion liquid into a dispersion liquid of graphene oxide (the solution of the graphene oxide dispersion liquid is 20mL of deionized water, and the solute of graphene oxide is 0.1 g.), and stirring for 30 min;
(4) adding 0.7g L-ascorbic acid into the mixed dispersion, and stirring for 20 min;
(5) placing the uniform dispersion into a water bath, and heating at 95 deg.C for 40 min;
(6) washing the obtained hydrogel sample with deionized water for 2-3 times to remove glycol;
(7) freeze drying for 48h to obtain macroscopically recoverable MoS2/g-C3N4Graphene oxide composite material.
Example 5
(1) The processed MoS2And g-C3N4According to a molar ratio of 1: 6 mixing and fully grinding;
(2) the milled mixed sample was added to 3mL of ethylene glycol and milling was continued.
(3) G to C3N4And MoS2Adding the dispersion liquid into a dispersion liquid of graphene oxide (the solution of the graphene oxide dispersion liquid is 20mL of deionized water, and the solute of graphene oxide is 0.08 g.), and stirring for 30 min;
(4) adding 0.7g L-ascorbic acid into the mixed dispersion, and stirring for 20 min;
(5) placing the uniform dispersion into a water bath, and heating at 88 deg.C for 50 min;
(6) washing the obtained hydrogel sample with deionized water for 2-3 times to remove glycol;
(7) freeze drying for 48h to obtain macroscopically recoverable MoS2/g-C3N4Graphene oxide composite material.
Example 6
(1) The processed MoS2And g-C3N4According to a molar ratio of 1: 2, mixing and fully grinding;
(2) the milled mixed sample was added to 3mL of ethylene glycol and milling was continued.
(3) G to C3N4And MoS2Adding the dispersion liquid into a dispersion liquid of graphene oxide (the solution of the graphene oxide dispersion liquid is 20mL of deionized water, and the solute of graphene oxide is 0.05 g.), and stirring for 30 min;
(4) adding 1g L-ascorbic acid into the mixed dispersion, and stirring for 20 min;
(5) placing the uniform dispersion into a water bath, and heating at 92 deg.C for 45 min;
(6) washing the obtained hydrogel sample with deionized water for 2-3 times to remove glycol;
(7) freeze drying for 48h to obtain macroscopically recoverable MoS2/g-C3N4Graphene oxide composite material.
Example 7
(1) The processed MoS2And g-C3N4According to a molar ratio of 1: 3 mixing and fully grinding;
(2) the milled mixed sample was added to 3mL of ethylene glycol and milling was continued.
(3) G to C3N4And MoS2Adding the dispersion liquid into a dispersion liquid of graphene oxide (the solution of the graphene oxide dispersion liquid is 20mL of deionized water, and the solute of graphene oxide is 0.06 g.), and stirring for 30 min;
(4) adding 1g L-ascorbic acid into the mixed dispersion, and stirring for 20 min;
(5) placing the uniform dispersion into a water bath, and heating at 95 deg.C for 55 min;
(6) washing the obtained hydrogel sample with deionized water for 2-3 times to remove glycol;
(7) freeze drying for 48h to obtain macroscopically recoverable MoS2/g-C3N4Graphene oxide composite material.
Example 8
(1) The processed MoS2And g-C3N4According to a molar ratio of 1: 4 mixing and fully grinding;
(2) the milled mixed sample was added to 3mL of ethylene glycol and milling was continued.
(3) G to C3N4And MoS2Adding the dispersion liquid into a dispersion liquid of graphene oxide (the solution of the graphene oxide dispersion liquid is 20mL of deionized water, and the solute of graphene oxide is 0.05 g.), and stirring for 30 min;
(4) adding 0.8g L-ascorbic acid into the mixed dispersion, and stirring for 20 min;
(5) placing the uniform dispersion into a water bath, and heating at 85 deg.C for 45 min;
(6) washing the obtained hydrogel sample with deionized water for 2-3 times to remove glycol;
(7) freeze drying for 48h to obtain macroscopically recoverable MoS2/g-C3N4Graphene oxide composite material.
Example 9
(1) The processed MoS2And g-C3N4According to a molar ratio of 1: 5 mixing and fully grinding;
(2) the milled mixed sample was added to 3mL of ethylene glycol and milling was continued.
(3) G to C3N4And MoS2Adding the dispersion liquid into a dispersion liquid of graphene oxide (the solution of the graphene oxide dispersion liquid is 20mL of deionized water, and the solute of graphene oxide is 0.07 g.), and stirring for 30 min;
(4) adding 0.9g L-ascorbic acid into the mixed dispersion, and stirring for 20 min;
(5) placing the uniform dispersion into a water bath, and heating at 90 deg.C for 50 min;
(6) washing the obtained hydrogel sample with deionized water for 2-3 times to remove glycol;
(7) freeze drying for 48h to obtain macroscopically recoverable MoS2/g-C3N4Graphene oxide composite material.
Example 10
(1) The processed MoS2And g-C3N4According to a molar ratio of 1: 6 mixing and fully grinding;
(2) the milled mixed sample was added to 3mL of ethylene glycol and milling was continued.
(3) G to C3N4And MoS2Adding the dispersion liquid into a dispersion liquid of graphene oxide (the solution of the graphene oxide dispersion liquid is 20mL of deionized water, and the solute of graphene oxide is 0.09 g.), and stirring for 30 min;
(4) adding 1g L-ascorbic acid into the mixed dispersion, and stirring for 20 min;
(5) placing the uniform dispersion into a water bath, and heating at 87 deg.C for 40 min;
(6) washing the obtained hydrogel sample with deionized water for 2-3 times to remove glycol;
(7) freeze drying for 48h to obtain macroscopically recoverable MoS2/g-C3N4Graphene oxide composite material.
The invention is described in further detail below with reference to the accompanying drawings:
as can be seen from (a), (b) and (C) in FIG. 1, g-C3N4And graphene oxide provides a two-dimensional sheet layered structure for the whole material, and MoS can be seen from (d), (e), (f) and (g) in FIG. 12And g-C3N4Uniformly distributed in graphene oxide。
Referring to FIG. 2, MoS2/g-C3N4Graphene oxide is a composite material which can be easily recycled macroscopically.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (8)
1. A preparation method of a macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material is characterized by comprising the following steps:
1) mixing graphite phase carbon nitride and molybdenum disulfide, grinding to obtain a mixed sample, adding a solvent into the mixed sample, and continuing grinding to obtain a dispersion liquid of the graphite phase carbon nitride and the molybdenum disulfide;
uniformly dispersing graphene oxide in water to obtain a dispersion liquid of the graphene oxide;
2) uniformly mixing the obtained dispersion liquid of graphite-phase carbon nitride and molybdenum disulfide and the obtained dispersion liquid of graphene oxide, adding L-ascorbic acid, and uniformly dispersing to obtain a uniform dispersion liquid;
3) reacting the obtained uniform dispersion liquid to obtain a hydrogel sample;
4) and washing and drying the obtained hydrogel sample to obtain the macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material.
2. The method for preparing the macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material according to claim 1, wherein in the step 1), the molar ratio of the graphite phase carbon nitride to the molybdenum disulfide is 1: 2-1: 6.
3. The method for preparing the macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material according to claim 1, wherein in the step 1), the solvent is ethylene glycol.
4. The preparation method of the macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material according to claim 1, wherein in the step 1), the mixing ratio of graphene oxide to water is 0.05-0.1 g: 20 mL.
5. The preparation method of the macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material according to claim 4, wherein the feeding ratio of graphene oxide to L-ascorbic acid is 0.05-0.1 g: 0.5 to 1 g.
6. The preparation method of the macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material according to claim 1, wherein in the step 3), the reaction temperature is 85-95 ℃ and the reaction time is 40-60 min.
7. The method for preparing the macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material according to claim 1, wherein in the step 4), the drying is performed by freeze drying.
8. A macroscopic recoverable molybdenum disulfide/graphite phase carbon nitride/graphene oxide composite material prepared by the preparation method of any one of claims 1-7.
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