CN116199317A - Molybdenum disulfide/porous carbon sphere composite material for capacitive desalination and preparation method thereof - Google Patents
Molybdenum disulfide/porous carbon sphere composite material for capacitive desalination and preparation method thereof Download PDFInfo
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- CN116199317A CN116199317A CN202310228909.1A CN202310228909A CN116199317A CN 116199317 A CN116199317 A CN 116199317A CN 202310228909 A CN202310228909 A CN 202310228909A CN 116199317 A CN116199317 A CN 116199317A
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- 238000010612 desalination reaction Methods 0.000 title claims abstract description 67
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 49
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 49
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000003764 ultrasonic spray pyrolysis Methods 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims description 26
- 239000003245 coal Substances 0.000 claims description 24
- 238000000197 pyrolysis Methods 0.000 claims description 23
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000002243 precursor Substances 0.000 claims description 16
- 238000004108 freeze drying Methods 0.000 claims description 14
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 14
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- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 230000007935 neutral effect Effects 0.000 claims description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000012159 carrier gas Substances 0.000 claims description 10
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 claims description 10
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- 239000007791 liquid phase Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
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- 150000002500 ions Chemical class 0.000 abstract description 8
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- 238000001179 sorption measurement Methods 0.000 abstract description 7
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- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 238000011033 desalting Methods 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- -1 salt ions Chemical class 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 239000002096 quantum dot Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
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- 238000005265 energy consumption Methods 0.000 description 2
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- 150000001768 cations Chemical class 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4691—Capacitive deionisation
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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
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- 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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Abstract
The invention relates to the technical field of electrode materials, in particular to a molybdenum disulfide/porous carbon sphere composite material for capacitive desalination and a preparation method thereof. The molybdenum disulfide/porous carbon sphere composite material for capacitance desalination, which has the advantages of developed pore structure, rich adsorption sites and excellent hydrophilicity and conductivity, is prepared by adopting an in-situ growth strategy through an ultrasonic spray pyrolysis method, has the characteristics of simple process, continuous operation, suitability for large-scale production, high specific surface area, gao Jiekong volume, good conductivity and wettability, provides rich ion adsorption sites, shortens the diffusion path of ions and electrons, and effectively improves the desalination performance of the capacitance desalination electrode.
Description
Technical Field
The invention relates to the technical field of electrode materials, in particular to a molybdenum disulfide/porous carbon sphere composite material for capacitive desalination and a preparation method thereof.
Background
Over-exploitation of fresh water resources due to rapid industrialization and population growth has forced people to turn to process using non-conventional water sources to meet the increasing demands. In order to solve the problem of lack of fresh water resources, nanofiltration, reverse osmosis, multistage flash evaporation, electrodialysis and other technologies have been applied to desalination of sea water and brackish water. However, the methods have the problems of high energy consumption, complex process, secondary pollution and the like. The Capacitive Deionization (CDI) technology is a novel desalination technology, and has the characteristics of high water recovery rate, low energy consumption, environmental friendliness and the like, so that the technology becomes a sea water desalination technology with great application prospect. The removal of salt ions in solution is achieved by applying an external electric field to the CDI device, adsorbing the salt ions at the electrical double layer at the interface of the electrode and the salt solution.
The electrode material is a decisive factor for influencing the CDI desalination performance, and the porous carbon material has developed pore structure, large specific surface area and good chemical stability, so that the electrode material becomes an ideal CDI electrode material. Currently, porous carbon materials also face the inevitable oxidation side reactions and homoion rejection effects of low charge storage capacity when used as CDI electrode materials, resulting in limited desalination capacity.
In order to improve the desalination performance of CDI, researchers have turned their eyes towards intercalated pseudocapacitive materials. Pseudocapacitive materials are capable of storing salt ions within the material by intercalation or faradaic reactions, which have higher specific capacities and lower self-discharge effects. Pseudocapacitive materials generally have a higher desalination capacity than conventional carbon materials. Meanwhile, cations or anions are adsorbed between layers of the material to form intercalation compounds, so that the homoion rejection effect is effectively relieved, an expensive ion selective membrane is avoided, and the charge utilization efficiency is improved. The valence state of molybdenum atoms in the two-dimensional layered molybdenum disulfide can be converted from +2 valence to +6 valence, and meanwhile, the S-Mo-S layered structure can provide a larger specific surface area and more exposed active sites, so that the two-dimensional layered molybdenum disulfide has higher pseudocapacitance energy storage capacity. However, the poor conductivity and sheet stacking of molybdenum disulfide limit the improvement in desalination capacity.
Disclosure of Invention
The invention provides a molybdenum disulfide/porous carbon sphere composite material for capacitance desalination and a preparation method thereof, which overcome the defects of the prior art, and can effectively solve the problems of low desalination capacity, poor conductivity of molybdenum disulfide and sheet stacking of the existing single carbon material.
One of the technical schemes of the invention is realized by the following measures: the preparation method of the molybdenum disulfide/porous carbon sphere composite material for the capacitance desalination is carried out according to the following steps:
step 1, performing liquid phase oxidation treatment on raw coal by mixed acid, collecting supernatant, dialyzing the supernatant to neutrality, and performing evaporation concentration and freeze drying to obtain coal-based graphene quantum dots;
step 2, adding the coal-based graphene quantum dots, sodium molybdate dihydrate and thiourea into deionized water, and performing ultrasonic treatment and stirring to obtain a precursor solution;
and step 3, performing ultrasonic spray pyrolysis on the precursor solution to obtain a pyrolysis product, washing the pyrolysis product to be neutral, and performing freeze drying to obtain the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination.
The following are further optimizations and/or improvements to one of the above-described inventive solutions:
in the step 1, the mixed acid is a mixed solution of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 3:1.
In the step 2, 1.00g of coal-based graphene quantum dots, 1.45g to 1.94g of sodium molybdate dihydrate and 2.28g to 3.04g of thiourea are added to every 100ml of deionized water.
In the step 3, the ultrasonic spray pyrolysis parameters are as follows: the pushing speed of the injection pump is 0.18mL/min to 0.22mL/min, the ultrasonic frequency is 1.7MHz to 2.4MHz, the carrier gas flow rate is 0.45L/min to 0.50L/min, and the pyrolysis temperature is 780 ℃ to 820 ℃.
The second technical scheme of the invention is realized by the following measures: a molybdenum disulfide/porous carbon sphere composite material for capacitive desalination, which is prepared by the preparation method according to one of the technical schemes.
Compared with the prior art, the invention has the following beneficial effects:
firstly, the molybdenum disulfide/porous carbon sphere composite material for capacitance desalination has simple process, can continuously operate, and is suitable for large-scale production.
Secondly, the molybdenum disulfide/porous carbon sphere composite material for capacitance desalination can realize the regulation and control of molybdenum disulfide content and pore structure by changing the component proportion of the spray precursor solution, and endows the molybdenum disulfide/porous carbon sphere composite material for capacitance desalination with rich adsorption sites, developed pore structure and good wettability.
Third, the capacitance desalination electrode obtained by taking the molybdenum disulfide/porous carbon sphere composite material for capacitance desalination as raw material is prepared by using NaCl and CaCl as the raw materials 2 、MgCl 2 And KCl solution, has excellent desalting performance and wide desalting application range.
In a word, the molybdenum disulfide/porous carbon sphere composite material for capacitance desalination, which has the advantages of developed pore structure, rich adsorption sites and excellent hydrophilicity and conductivity, is prepared by adopting an in-situ growth strategy through an ultrasonic spray pyrolysis method, has the characteristics of simple process, continuous operation, suitability for large-scale production, high specific surface area, gao Jiekong volume, good conductivity and wettability, provides rich ion adsorption sites, shortens the diffusion path of ions and electrons, and effectively improves the desalination performance of the capacitance desalination electrode.
Drawings
FIG. 1 is an X-ray powder diffraction pattern of a molybdenum disulfide/porous carbon sphere composite material for capacitive desalination prepared in example 9 of the present invention;
FIG. 2 is an X-ray photoelectron spectrum of the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination prepared in example 9 of the present invention;
FIG. 3 is a scanning electron microscope image of the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination prepared in example 9 of the present invention;
FIG. 4 is a transmission electron microscope image of the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination prepared in example 9 of the present invention;
FIG. 5 is a graph showing pore size distribution of a molybdenum disulfide/porous carbon sphere composite material for capacitive desalination prepared in example 9 of the present invention;
FIG. 6 is a graph showing the water contact angle of the capacitive desalting electrode prepared in example 11 of the present invention;
FIG. 7 is a graph showing the change in desalting capacity and the maximum desalting rate of Gong Quxian in a 500mg/L NaCl solution for a capacitive desalting electrode prepared in example 11 of the present invention;
FIG. 8 shows a capacitive desalting electrode prepared in example 11 of the invention at 5mM KCl, caCl 2 And MgCl 2 A desalination capacity change curve in solution;
wherein, moS in figures 1, 5 and 7 2 and/CS represents molybdenum disulfide/porous carbon sphere composite material for capacitive desalination.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments can be determined according to the technical scheme and practical situations of the present invention. The various chemical reagents and chemical supplies mentioned in the invention are all commonly known and used in the prior art unless specified otherwise; the percentages in the invention are mass percentages unless specified otherwise; if the solution in the invention is not specially described, the solvent is water, for example, the hydrochloric acid solution is hydrochloric acid aqueous solution; the room temperature and the room temperature in the present invention generally refer to temperatures ranging from 15 ℃ to 25 ℃, and are generally defined as 25 ℃.
The invention is further described below with reference to examples:
example 1: the preparation method of the molybdenum disulfide/porous carbon sphere composite material for the capacitance desalination is carried out according to the following method:
step 1, performing liquid phase oxidation treatment on raw coal by mixed acid, collecting supernatant, dialyzing the supernatant to neutrality, and performing evaporation concentration and freeze drying to obtain coal-based graphene quantum dots;
step 2, adding the coal-based graphene quantum dots, sodium molybdate dihydrate and thiourea into deionized water, and performing ultrasonic treatment and stirring to obtain a precursor solution;
and step 3, performing ultrasonic spray pyrolysis on the precursor solution to obtain a pyrolysis product, washing the pyrolysis product to be neutral, and performing freeze drying to obtain the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination.
Example 2: in the step 1, the mixed acid is a mixed solution of concentrated sulfuric acid and concentrated nitric acid with the volume ratio of 3:1.
Example 3: as an optimization of the above step, in step 2, 1.00g of coal-based graphene quantum dots, 1.45g to 1.94g of sodium molybdate dihydrate, and 2.28g to 3.04g of thiourea were added to every 100ml of deionized water.
Example 4: as an optimization of the above steps, in step 3, the ultrasonic spray pyrolysis parameters are: the pushing speed of the injection pump is 0.18mL/min to 0.22mL/min, the ultrasonic frequency is 1.7MHz to 2.4MHz, the carrier gas flow rate is 0.45L/min to 0.50L/min, and the pyrolysis temperature is 780 ℃ to 820 ℃.
Example 5: the molybdenum disulfide/porous carbon sphere composite material for the capacitance desalination is prepared by the preparation method.
Example 6:
the preparation method of the molybdenum disulfide/porous carbon sphere composite material for the capacitance desalination is carried out according to the following method:
step 1, carrying out liquid phase oxidation treatment on 30g of raw coal by using 540ml of mixed solution (3:1, V/V) of concentrated sulfuric acid and concentrated nitric acid, collecting supernatant, dialyzing the supernatant to be neutral, and carrying out evaporation concentration and freeze drying to obtain the coal-based graphene quantum dot;
step 2, adding 1.00g of coal-based graphene quantum dots, 1.45g of sodium molybdate dihydrate and 2.28g of thiourea into 100ml of deionized water, and sequentially carrying out ultrasonic treatment for 20min and stirring for 2.0h to obtain a precursor solution;
step 3, injecting the precursor solution into an ultrasonic atomizer, and using N as the raw material 2 Is carrier gas and passes through ultrasonic waveSpray pyrolysis is carried out to obtain a pyrolysis product, the pyrolysis product is washed to be neutral, and then the molybdenum disulfide/porous carbon sphere composite material for capacitance desalination is obtained after freeze drying; wherein, ultrasonic spray pyrolysis parameters are: the pushing speed of the injection pump is 0.18mL/min, the ultrasonic frequency is 1.7MHz, the carrier gas flow rate is 0.45L/min, and the pyrolysis temperature is 780 ℃.
Example 7:
the preparation method of the molybdenum disulfide/porous carbon sphere composite material for the capacitance desalination is carried out according to the following method:
step 1, carrying out liquid phase oxidation treatment on 30g of raw coal by using 540ml of mixed solution (3:1, V/V) of concentrated sulfuric acid and concentrated nitric acid, collecting supernatant, dialyzing the supernatant to be neutral, and carrying out evaporation concentration and freeze drying to obtain the coal-based graphene quantum dot;
step 2, adding 1.00g of coal-based graphene quantum dots, 1.94g of sodium molybdate dihydrate and 3.04g of thiourea into 100ml of deionized water, and sequentially carrying out ultrasonic treatment for 30min and stirring for 2.5h to obtain a precursor solution;
step 3, injecting the precursor solution into an ultrasonic atomizer, and using N as the raw material 2 The molybdenum disulfide/porous carbon sphere composite material for the capacitance desalination is obtained by using the carrier gas, carrying out ultrasonic spray pyrolysis to obtain a pyrolysis product, washing the pyrolysis product to be neutral, and then carrying out freeze drying; wherein, ultrasonic spray pyrolysis parameters are: the pushing speed of the injection pump is 0.22mL/min, the ultrasonic frequency is 2.4MHz, the carrier gas flow rate is 0.50L/min, and the pyrolysis temperature is 820 ℃.
Example 8:
the preparation method of the molybdenum disulfide/porous carbon sphere composite material for the capacitance desalination is carried out according to the following method:
step 1, carrying out liquid phase oxidation treatment on 30g of raw coal by using 540ml of mixed solution (3:1, V/V) of concentrated sulfuric acid and concentrated nitric acid, collecting supernatant, dialyzing the supernatant to be neutral, and carrying out evaporation concentration and freeze drying to obtain the coal-based graphene quantum dot;
step 2, adding 1.00g of coal-based graphene quantum dots, 1.45g of sodium molybdate dihydrate and 2.28g of thiourea into 100ml of deionized water, and sequentially carrying out ultrasonic treatment for 20min and stirring for 2.0h to obtain a precursor solution;
step 3, injecting the precursor solution into an ultrasonic atomizer, and using N as the raw material 2 The molybdenum disulfide/porous carbon sphere composite material for the capacitance desalination is obtained by using the carrier gas, carrying out ultrasonic spray pyrolysis to obtain a pyrolysis product, washing the pyrolysis product to be neutral, and then carrying out freeze drying; wherein, ultrasonic spray pyrolysis parameters are: the pushing speed of the injection pump is 0.20mL/min, the ultrasonic frequency is 2.0MHz, the carrier gas flow rate is 0.47L/min, and the pyrolysis temperature is 800 ℃.
Example 9:
the preparation method of the molybdenum disulfide/porous carbon sphere composite material for the capacitance desalination is carried out according to the following method:
step 1, carrying out liquid phase oxidation treatment on 30g of raw coal by using 540ml of mixed solution (3:1, V/V) of concentrated sulfuric acid and concentrated nitric acid, collecting supernatant, dialyzing the supernatant by using a dialysis bag with a molecular weight cutoff of 7000Da, concentrating by using a rotary evaporator after dialyzing to be neutral, and freeze-drying the concentrated solution to obtain the coal-based graphene quantum dots;
step 2, adding 1.00g of coal-based graphene quantum dots, 1.45g of sodium molybdate dihydrate and 2.28g of thiourea into 100ml of deionized water, performing ultrasonic dispersion for 20min, and continuously stirring at room temperature for 2.0h to obtain a precursor solution;
step 3, continuously injecting the precursor solution into an ultrasonic atomizer with ultrasonic frequency of 1.7MHz at a push injection speed of 0.20mL/min, and continuously injecting the precursor solution into the ultrasonic atomizer at N of 0.45L/min 2 And sending the aerosol formed by ultrasonic atomization into a tubular furnace with the temperature of 800 ℃ as carrier gas for pyrolysis to obtain a pyrolysis product, washing the pyrolysis product to be neutral by deionized water, and then obtaining the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination after freeze drying.
Example 10: the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination of example 9 of the present invention was tested, and its X-ray powder diffraction and X-ray photoelectron spectra are shown in fig. 1 and 2, respectively, and analysis in fig. 1 and 2 shows that the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination was successfully prepared through the above steps. In the pyrolysis process, the liquid drops serve as microreactors to generate molybdenum disulfide in situ, meanwhile, the generation of a large amount of gas causes pressure difference between the inside and the outside of the liquid drops, so that the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination breaks and forms developed pore structures (shown in fig. 3 and 4), and the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination with the openings contains abundant micropore and mesoporous structures (shown in fig. 5), can provide more surface active sites, and shortens the transmission paths of ions and electrons.
Example 11: the molybdenum disulfide/porous carbon sphere composite material for capacitance desalination obtained in the embodiment 9 of the invention, acetylene black and polytetrafluoroethylene are mixed according to the mass ratio of 8:1:1, ethanol is added dropwise, the mixture is ground into paste, the paste is coated on graphite paper, the paste is dried at 80 ℃ for 10 hours, a capacitance desalination electrode is obtained, and a desalination test is carried out on the capacitance desalination electrode. As shown in fig. 6, the obtained porous carbon sphere electrode had good wettability with a water contact angle of 56.3 °. At a voltage of 1.2V, the desalination capacity and the maximum desalination rate of 500mg/L NaCl solution are 29.56mg/g and 3.71mg/g/min, respectively (as shown in FIG. 7, a is a desalination capacity change curve chart in FIG. 7, and b is a maximum desalination rate Lagong curve chart); and at 5mM CaCl 2 、MgCl 2 And KCl solutions with desalting capacities of 38.85mg/g, 33.18mg/g and 27.05mg/g, respectively (as shown in FIG. 8).
In summary, the molybdenum disulfide/porous carbon sphere composite material for capacitance desalination, which has the advantages of developed pore structure, rich adsorption sites, excellent hydrophilicity and conductivity, is prepared by adopting an in-situ growth strategy through an ultrasonic spray pyrolysis method, has the characteristics of simple process, continuous operation, suitability for large-scale production, high specific surface area, gao Jiekong volume, good conductivity and wettability, provides rich ion adsorption sites, shortens the diffusion path of ions and electrons, and effectively improves the desalination performance of the capacitance desalination electrode.
The technical characteristics form the embodiment of the invention, have stronger adaptability and implementation effect, and can increase or decrease unnecessary technical characteristics according to actual needs so as to meet the requirements of different situations.
Claims (5)
1. The preparation method of the molybdenum disulfide/porous carbon sphere composite material for the capacitive desalination is characterized by comprising the following steps of:
step 1, performing liquid phase oxidation treatment on raw coal by mixed acid, collecting supernatant, dialyzing the supernatant to neutrality, and performing evaporation concentration and freeze drying to obtain coal-based graphene quantum dots;
step 2, adding the coal-based graphene quantum dots, sodium molybdate dihydrate and thiourea into deionized water, and performing ultrasonic treatment and stirring to obtain a precursor solution;
and step 3, performing ultrasonic spray pyrolysis on the precursor solution to obtain a pyrolysis product, washing the pyrolysis product to be neutral, and performing freeze drying to obtain the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination.
2. The method for preparing the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination according to claim 1, wherein in the step 1, the mixed acid is a mixed solution of concentrated sulfuric acid and concentrated nitric acid in a volume ratio of 3:1.
3. The method for preparing the molybdenum disulfide/porous carbon sphere composite material for capacitive desalination according to claim 1 or 2, characterized in that in step 2, 1.00g of coal-based graphene quantum dots, 1.45g to 1.94g of sodium molybdate dihydrate and 2.28g to 3.04g of thiourea are added to every 100ml of deionized water.
4. A method for preparing a molybdenum disulfide/porous carbon sphere composite material for capacitive desalination according to any one of claims 1 to 3, characterized in that in step 3, the ultrasonic spray pyrolysis parameters are: the pushing speed of the injection pump is 0.18mL/min to 0.22mL/min, the ultrasonic frequency is 1.7MHz to 2.4MHz, the carrier gas flow rate is 0.45L/min to 0.50L/min, and the pyrolysis temperature is 780 ℃ to 820 ℃.
5. A molybdenum disulfide/porous carbon sphere composite material for capacitive desalination obtained by the production method according to any one of claims 1 to 4.
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