CN111921489A - Composite material for removing lead ions in solution and preparation method and application thereof - Google Patents
Composite material for removing lead ions in solution and preparation method and application thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0218—Compounds of Cr, Mo, W
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0285—Sulfides of compounds other than those provided for in B01J20/045
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a composite material for removing lead ions in a solution, a preparation method and application thereof, wherein ammonium molybdate tetrahydrate (NH)4)6Mo7O24·4H2O and Thiourea (CN)2H4S) dissolving in deionized water, and stirring until the solution is completely dissolved; weighing kaolinite, adding the kaolinite into the mixed solution, and mixing and stirring for a certain time to form uniform suspension; transferring the mixed suspension into a reaction kettle with a polytetrafluoroethylene lining, heating to a target temperature, preserving heat for a certain time, and naturally cooling to room temperature; centrifuging the reaction product by using a centrifuge, and alternately washing the reaction product for more than three times by using deionized water and absolute ethyl alcohol; the washed product is placed inAnd (4) completely drying the sample in a vacuum drying oven under a certain temperature condition, and grinding to obtain the composite material. Composite material for Pb in solution2+The adsorption performance of the ions is obviously superior to that of single MoS2And kaolinite, the maximum adsorption capacity can reach 275.38mg/g, the adsorption rate in 20min can reach more than 92%, the adsorption rate in 50min can reach 99.9%, and Pb can be maintained in a wider pH range2+The adsorption rate is higher than 99%.
Description
Technical Field
The invention belongs to the technical field of mineral materials and environmental protection, and particularly relates to a material for removing lead ions in a solution, and a preparation method and application thereof.
Background
Lead ion is a poisonous heavy metal ion, can be gathered in animals and plants and is difficult to be discharged out of the bodies, and causes great harm to the ecological environment and human health. The lead ions in the aqueous solution are generally removed by adsorption, ion exchange, chemical reduction, membrane separation, electrochemical treatment, reverse osmosis, distillation electrodialysis, and the like. The adsorption method is simple and convenient to operate, high in efficiency and low in cost, and has great application potential in the aspect of removing lead ions in the aqueous solution.
Yan spring and autumn and the like adopt a double-nozzle electrospinning technology to prepare an amidoxime polyacrylonitrile/nylon composite nanofiber membrane (AOPAN/PA-66) for Pb2+Adsorption gave an adsorbed amount of 75.4 mg/g. Zuge et al prepared the polyvinyl alcohol/polyethyleneimine (PVA/PEI) nanofiber membrane through a high-voltage electrostatic spinning technology, and realized the purposes of quick adsorption of lead ions, high adsorption capacity and good regeneration adsorption capacity. Preparing a P-Pb catalyst from Chenxing2+Novel magnetic imprinted polymers (MWNTs/MIIPs) with specific adsorption capacity for Pb2+Has good adsorption and selective recognition capability, and the maximum adsorption capacity is 25.9 mg/g. Duffin (Yu) et al treat the rape straw by an organic acid method and regenerate acid-insoluble lignin solid from the pretreated waste liquid for adsorption of cadmium and lead ions, but the yield thereof still needs to be improved. Modified bagasse was studied and its pair of Pb was studied by Wangliyan et al2+The dynamic adsorption performance of the adsorbent is 118.9-148.6 mg/gAnd (4) attaching capacity. The adsorption effect of rape straws on Pb (II) in a multi-element ionic water system is researched by using a Huangxuejing and the like. The Zhang Like and the like take agricultural wastes, namely flax straws and rape straws as raw materials to prepare the oil crop straw biochar, and the biochar has good adsorption performance on lead ions. The influence of a magnetic field on the adsorption of heavy metal lead ions by chitosan Schiff base is researched by the Shanlihong and the like, and the proper magnetic field treatment can be found to strengthen the adsorption capacity of the chitosan and the Schiff base on the metal ions. He assist et al studied the adsorption performance of kaolinite on lead ions in water and obtained the maximum adsorption amount of about 10 mg/g. Shenyanbai et al studied Pb in diatomite in water phase2+Can almost completely adsorb Pb in the solution under the optimal adsorption condition2+. Zhangtianlin and the like prepared quaternary ammonium salt type chelate resin for Pb2+The adsorption capacity of (A) was 96.1 mg/g.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a material for removing lead ions in a solution and a preparation method and application thereof. MoS with cheap kaolinite as substrate of composite adsorbing material2As a lead ion adsorption monomer, a simple one-step hydrothermal method is adopted to assemble molybdenum disulfide nanosheets on flaky kaolinite to prepare the kaolinite and molybdenum disulfide composite adsorption material, so that the synergistic adsorption of lead ions by molybdenum disulfide and kaolinite is realized, and meanwhile, the composite adsorption material solves the problem of poor hydrophilicity of single molybdenum disulfide and has the advantages of good stability, low cost, wide applicable pH range and the like. Is a lead ion adsorption material in solution with wide application prospect.
In order to achieve the technical effects, the invention provides the following technical scheme:
a preparation method of a composite material for removing lead ions in a solution comprises the following specific steps:
the method comprises the following steps: ammonium molybdate tetrahydrate (NH) is weighed according to a certain molar ratio4)6Mo7O24 .4H2O and Thiourea (CN)2H4S) dissolving the mixture in a certain amount of deionized water, and stirring the mixture by using a magnetic stirrer until the mixture is completely dissolved; weighing a certain amount of kaoliniteAdding the mixture into the mixed solution, and mixing and stirring the mixture for a certain time to form uniform suspension; transferring the mixed suspension into a reaction kettle with a polytetrafluoroethylene lining, heating to a target temperature, preserving heat for a certain time, and naturally cooling to room temperature;
step two: carrying out centrifugal separation on the reaction product in the step one by adopting a centrifugal machine, and alternately washing the reaction product for more than three times by using deionized water and absolute ethyl alcohol;
step three: and (3) placing the washed product in a vacuum drying oven at a certain temperature until the sample is completely dried, and grinding to obtain the composite material.
According to the preparation method, in the step one, the mole ratio of ammonium molybdate tetrahydrate to thiourea is fixed to be 1:14, and the mass of deionized water is 10-30 times that of ammonium molybdate tetrahydrate.
According to the preparation method, in the first step, the mass ratio of the kaolinite to the ammonium molybdate tetrahydrate is 1: 1-1: 3, and the stirring time is 30-60 min.
According to the preparation method, in the first step, the target temperature is 210-230 ℃, and the heat preservation time is 6-24 hours.
The preparation method comprises the following steps of a, controlling the certain temperature to be 80-100 ℃;
a composite material prepared according to any of the preparation methods.
The application of the composite material is used for removing lead ions in a solution.
The application of the composite material comprises the following steps: 10-1000 mg/L.
The application of the composite material is that dilute nitric acid and sodium hydroxide are used for adjusting the pH value of a solution, the pH value is 1-5.5, and the using amount of the composite material is 0.4-2 g/L.
The invention has the beneficial effects that: (1) the SK @ MoS is prepared by taking kaolinite as a substrate and adopting a simple one-step hydrothermal method2The composite material has low synthesis cost and simple synthesis method; (2) the molybdenum disulfide nanosheets form a composite adsorption material by self-assembly on the surface of kaolinite, the kaolinite serves as a composite material substrate to provide a growth foundation for the molybdenum disulfide nanosheets, and the composite material is formed under a hydrothermal condition. Kaolinite has one to lead ionThe adsorption was constant, but the performance was weak (see FIG. 4). Molybdenum disulfide is used as an excellent adsorption material of metal ions, has high cost and poor hydrophilicity, and is easy to agglomerate in a synthetic product, thereby being not beneficial to the adsorption process. The adsorption performance of the adsorption material formed by compounding the kaolinite and the molybdenum disulfide is obviously superior to the sum of single adsorption effects of the kaolinite and the molybdenum disulfide, which shows that the composite adsorption material realizes the synergistic adsorption of the kaolinite and the molybdenum disulfide on lead ions. Meanwhile, the composite material solves the problem of poor hydrophilicity of the molybdenum disulfide. (3) SK @ MoS2Composite material for Pb in solution2+The adsorption performance of the ions is obviously superior to that of single MoS2And kaolinite, the maximum adsorption capacity can reach 275.38mg/g, the adsorption rate in 20min can reach more than 92%, the adsorption rate in 50min can reach 99.9%, and Pb can be maintained in a wider pH range2+The adsorption rate is higher than 99%.
Drawings
FIG. 1 SK @ MoS synthesized by the present invention based on the conditions of example 12XRD pattern of (a);
FIG. 2 SK @ MoS synthesized by the present invention based on the conditions of example 12SEM image of (d).
FIG. 3 SK @ MoS synthesized by the present invention based on the conditions of example 22XRD pattern of (a);
FIG. 4 SK @ MoS under different adsorption time conditions in example 1 of the present invention2、MoS2And kaolinite to Pb2+Adsorption rate curve chart;
FIG. 5 is a schematic diagram of an embodiment 2 of the present invention with different SK @ MoS2In the amount of Pb2+A graph of adsorption rate and adsorption capacity;
FIG. 6 SK @ MoS under different pH conditions in example 3 of the present invention2For Pb2+Adsorption rate curve chart;
FIG. 7 example 4 of the present invention shows different Pb2+SK @ MoS under initial concentration condition2For Pb2+A graph of adsorption rate and adsorption capacity;
FIG. 8 is an XRD pattern of kaolin clay used in the present invention;
FIG. 9 is an SEM image of kaolin clay used in the present invention;
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
Weighing 1.24g of ammonium molybdate tetrahydrate and 1.07g of thiourea, dissolving in 60mL of deionized water, and stirring by using a magnetic stirrer until the ammonium molybdate tetrahydrate and the thiourea are completely dissolved; weighing 1g of kaolinite, adding the kaolinite into the mixed solution, and mixing and stirring for 30min to form uniform suspension; transferring the mixed suspension into a reaction kettle with a polytetrafluoroethylene lining, heating to 210 ℃, preserving heat for 6 hours, and naturally cooling to room temperature; centrifuging the reaction product by using a centrifuge, and alternately washing the reaction product for more than three times by using deionized water and absolute ethyl alcohol; putting the washed product in a vacuum drying oven at 80 ℃ until the sample is completely dried, and grinding for later use with the code number SK @ MoS2。
FIG. 1 shows the SK @ MoS synthesized in this embodiment2According to the XRD pattern of the composite material, in addition to the characteristic diffraction peak of the kaolinite substrate, the characteristic diffraction peaks of (002), (100) and (110) surfaces which characterize molybdenum disulfide appear at 13.96 degrees, 33.34 degrees and 59 degrees of 2 theta on the XRD pattern of the synthesized product, which indicates that the molybdenum disulfide is successfully compounded with the kaolinite. FIG. 2 shows SK @ MoS2SEM image of the composite material. The molybdenum disulfide nanosheets are assembled on the surface of the kaolinite to form SK @ MoS2And (3) the composite material verifies the XRD result.
Example 2
Weighing 2.48g of ammonium molybdate tetrahydrate and 2.14g of thiourea, dissolving in 60mL of deionized water, and stirring by using a magnetic stirrer until the ammonium molybdate tetrahydrate and the thiourea are completely dissolved; weighing 2g of kaolinite, adding the kaolinite into the mixed solution, and mixing and stirring for 30min to form uniform suspension; transferring the mixed suspension into a reaction kettle with a polytetrafluoroethylene lining, heating to 220 ℃, preserving heat for 8 hours, and naturally cooling to room temperature; centrifuging the reaction product by using a centrifuge, and alternately washing the reaction product for more than three times by using deionized water and absolute ethyl alcohol; and (4) placing the washed product in a vacuum drying oven at the temperature of 80 ℃ until the sample is completely dried, and grinding the product for XRD test.
FIG. 3 shows SK @ MoS synthesized under the conditions of the present embodiment2The XRD pattern of the composite material shows that characteristic diffraction peaks of kaolinite and molybdenum disulfide appear on the XRD pattern of the synthetic product under the synthetic conditions of the embodiment at the same time, which shows thatSK@MoS2The composite material is successfully prepared.
Example 3
For comparing SK @ MoS2Composite adsorbent and unitary MoS2And kaolinite to Pb2+The difference in adsorption performance of (a). At Pb2 +0.08g SK @ MoS was added to a 50mL solution having a concentration of 4.0 mg/L, pH2、MoS2And placing the kaolinite sample on a magnetic stirrer, stirring for 10min, 20min, 30min, 40min, 50min and 60min respectively, taking down, performing solid-liquid separation by adopting a centrifugal machine to obtain supernatant and a solid sample, and performing ICP (inductively coupled plasma) on Pb in the supernatant2+Detecting the concentration to obtain Pb2+Concentration, calculating Pb of three adsorbing materials under different stirring time conditions by adopting a residual method2+The adsorption rate of (3).
FIG. 4 shows SK @ MoS under different stirring time conditions in this example2、MoS2And kaolinite to Pb respectively2+The graph of adsorption rate shows that SK @ MoS is obtained when the stirring time is 10min, 20min, 30min, 40min, 50min and 60min2For Pb2 +Has adsorption rates of 88.82%, 92.08%, 96.24%, 99.89%, 99.90% and 99.54%, respectively, and SK @ MoS increases with the increase of stirring time2For Pb2+The adsorption rate increases and finally approaches to a stable value, and Pb is generated when the stirring time is 50min2+The adsorption rate reaches more than 99 percent. In contrast, a single MoS2And kaolinite to Pb under the same time condition2+The adsorption capacity of the adsorbent is lower than SK @ MoS2Indicates MoS2After the composite material is compounded with kaolinite, the adsorption performance of the composite material on lead ions in a solution is greatly improved.
Example 4
Pb in group 52+0.02g, 0.04g, 0.06g, 0.08g, 0.1g SK @ MoS are respectively added into a solution with the concentration of 100mg/L, pH of 4.0 and the volume of 50mL2Placing the sample on a water bath oscillator, oscillating for 60min, taking off, performing solid-liquid separation with a centrifuge to obtain supernatant and solid sample, and performing ICP on Pb in the supernatant2+Detecting the concentration to obtain Pb2+Concentration, calculated by the residue methodSame SK @ MoS2In the amount of Pb2+The adsorption rate and the adsorption amount of (3).
FIG. 5 shows SK @ MoS with different dosages in the present embodiment2For Pb2+The graphs of adsorption rate and adsorption quantity show that SK @ MoS2In the case of using 0.02g, 0.04g, 0.06g, 0.08g, 0.1g, for Pb2+The adsorption rates of (A) were 24.18%, 48.58%, 77.55%, 99.54%, 99.75%, respectively, and the adsorption amounts were 60, 60.28, 55.81, 61.73, 49.5mg/g, respectively. With SK @ MoS2Increased amount of the compound for Pb2+The adsorption rate increases and finally tends to a stable value, and the adsorption quantity increases firstly and then decreases. When SK @ MoS2When the amount is 0.08g, Pb2+The adsorption rate reaches more than 99 percent, and the adsorption capacity reaches 61.73 mg/g.
Example 5
Pb in group 62+Adding a small amount of dilute nitric acid or sodium hydroxide solution into a solution with the concentration of 100mg/L and the volume of 50mL, respectively adjusting the pH to 1, 2, 3, 4, 5 and 5.5, and respectively adding 0.08g of SK @ MoS2Placing the sample on a water bath constant temperature oscillator, oscillating for 50min respectively, taking off, performing solid-liquid separation with a centrifuge to obtain supernatant and solid sample, and performing ICP on Pb in the supernatant2+Detecting to obtain Pb2+The concentration is calculated by adopting a residue method to calculate SK @ MoS under different pH conditions2For Pb2+The adsorption rate of (3).
FIG. 6 shows SK @ MoS under different pH conditions in this example2For Pb2+As can be seen from the graph of the adsorption rate, the pH values at 1, 2, 3, 4, 5 and 5.5 are against Pb2+Has an adsorption ratio of 22.8, 99.95, 99.92, 99.95, 99.9, respectively, and thus, SK @ MoS2Realize the high-efficiency adsorption of Pb2+The process has a large span corresponding to the pH range of the solution, and when the pH is higher than 2, the SK @ MoS is changed along with the change of the pH value2For Pb2+The adsorption rate of the adsorbent can reach more than 99.9 percent.
Example 6
Pb in group 92+0.08g of SK @ MoS is added into a solution with the concentration of 10mg/L, 20mg/L, 40mg/L, 80mg/L, 100mg/L, 200mg/L, 400mg/L, 800mg/L and 1000mg/L, the pH of 4.0 and the volume of 50mL2Placing the sample on a water bath constant temperature oscillator, oscillating for 50min, taking off, performing solid-liquid separation with a centrifuge to obtain supernatant and solid sample, and performing ICP on Pb in the supernatant2+Detecting the concentration to obtain Pb2+Concentration, calculating different Pb by residue method2+SK @ MoS under concentration condition2For Pb2+The adsorption rate and the adsorption amount of (3).
FIG. 7 shows Pb in the present example2+SK @ MoS under concentration condition2For Pb2+The adsorption rate and the amount of adsorption were plotted, and it is understood from the graph that Pb is2+SK @ MoS at a concentration of 10mg/L, 20mg/L, 40mg/L, 80mg/L, 100mg/L, 200mg/L, 400mg/L, 800mg/L, 100mg/L2For Pb2+The adsorption rates of (A) are respectively 99.5%, 99.7%, 99.9%, 99.7%, 95.2%, 55.1% and 40.9%, and the adsorption amounts are respectively 6.22, 12.47, 24.97, 49.97, 62.43, 124.65, 238.08, 275.38 and 255.75 mg/g. With Pb2+Increase in concentration, SK @ MoS2For Pb2+The adsorption rate is gradually reduced, the adsorption quantity is increased and then reduced, when Pb is formed2+At a concentration of 400mg/g, the adsorption rate was maintained at 95% or more, and the adsorption amount was 238.08 mg/g.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (9)
1. A preparation method of a composite material for removing lead ions in a solution is characterized by comprising the following specific steps:
the method comprises the following steps: ammonium molybdate tetrahydrate (NH) is weighed according to a certain molar ratio4)6Mo7O24 .4H2O and Thiourea (CN)2H4S) dissolving the raw materials in a certain amount of deionized water, and stirring until the raw materials are completely dissolved; weighing a certain amount of kaolinite, adding the kaolinite into the mixed solution, and mixing and stirring for a certain time to form uniform suspension; transferring the mixed suspension into a reaction kettle with a polytetrafluoroethylene lining, heating to a target temperature, keeping the temperature for a certain time, and then carrying out heat preservation on the mixtureNaturally cooling to room temperature;
step two: carrying out centrifugal separation on the reaction product in the step one by adopting a centrifugal machine, and alternately washing the reaction product for more than three times by using deionized water and absolute ethyl alcohol;
step three: and (3) placing the washed product in a vacuum drying oven at a certain temperature until the sample is completely dried, and grinding to obtain the composite material.
2. The preparation method according to claim 1, wherein the mole ratio of ammonium molybdate tetrahydrate to thiourea in the first step is fixed to be 1:14, and the mass of the deionized water is 10-30 times that of the ammonium molybdate tetrahydrate.
3. The preparation method according to claim 1, wherein the mass ratio of the kaolinite to the ammonium molybdate tetrahydrate in the first step is 1: 1-1: 3, and the stirring time is 30-60 min.
4. The method according to claim 1, wherein the target temperature in the first step is 210-230 ℃ and the holding time is 6-24 hours.
5. The method according to claim 1, wherein the temperature in step three is 80-100 ℃.
6. A composite material produced by the production method according to any one of claims 1 to 5.
7. Use of the composite material according to claim 6 for removing lead ions from a solution.
8. Use according to claim 7, wherein the lead ion concentration is: 10-1000 mg/L.
9. The application of claim 7, wherein the pH value of the solution is adjusted by using dilute nitric acid and sodium hydroxide, the pH value is 1-5.5, and the dosage of the composite material is 0.4-2 g/L.
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| CN112675805A (en) * | 2021-01-25 | 2021-04-20 | 西北师范大学 | Preparation method of hydroxyapatite nanowire composite molybdenum disulfide adsorbent |
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| CN114259981A (en) * | 2021-12-23 | 2022-04-01 | 武汉大学(肇庆)资源与环境技术研究院 | Clay mineral loaded molybdenum disulfide composite material and preparation method and application thereof |
| CN114618425A (en) * | 2021-12-23 | 2022-06-14 | 武汉大学(肇庆)资源与环境技术研究院 | Molybdenum disulfide/diatomite composite material and preparation method and application thereof |
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