CN111777068A - Novel chloride ion removing material Ti3C2TxPreparation method and application of/Ag - Google Patents
Novel chloride ion removing material Ti3C2TxPreparation method and application of/Ag Download PDFInfo
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 43
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims description 5
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000008367 deionised water Substances 0.000 claims abstract description 31
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 31
- 229910021607 Silver chloride Inorganic materials 0.000 claims abstract description 25
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000084 colloidal system Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims abstract description 5
- 238000005530 etching Methods 0.000 claims abstract description 3
- 239000011259 mixed solution Substances 0.000 claims description 57
- 239000000243 solution Substances 0.000 claims description 36
- 238000005303 weighing Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 11
- 238000010612 desalination reaction Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000002242 deionisation method Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 101710134784 Agnoprotein Proteins 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims 1
- 238000011033 desalting Methods 0.000 abstract description 14
- 230000035484 reaction time Effects 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000009830 intercalation Methods 0.000 abstract description 7
- 239000002105 nanoparticle Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 230000002687 intercalation Effects 0.000 abstract description 5
- 230000001276 controlling effect Effects 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 4
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 238000011068 loading method Methods 0.000 abstract description 3
- 239000007800 oxidant agent Substances 0.000 abstract description 3
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 description 8
- 230000007246 mechanism Effects 0.000 description 7
- 238000010168 coupling process Methods 0.000 description 6
- 238000005859 coupling reaction Methods 0.000 description 6
- 239000013535 sea water Substances 0.000 description 6
- 230000008878 coupling Effects 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- -1 chlorine ions Chemical class 0.000 description 3
- 238000006298 dechlorination reaction Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000003011 anion exchange membrane Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical group 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 239000005447 environmental material Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
Abstract
Novel chloride ion removing material Ti3C2TxPreparation method and application of Ag. Etching bulk Ti3AlC2Obtaining Ti of lamellar layer3C2Tx-MXene; ultrasonic stripping of Ti3C2Tx-MXene solution, supernatant to get Ti with less lamella3C2Tx-MXene solution; taking a certain amount of AgNO3Dissolving in deionized water, and adding a certain amount of hydrochloric acid under an ultrasonic condition to obtain an AgCl colloidal solution; the Ag obtained above is addedCl colloid is added into a few Ti sheets3C2TxOscillating MXene solution for a certain time under the conditions of constant temperature and constant rotating speed; vacuum filtering and separating the reacted mixture, washing with deionized water several times, and naturally drying at room temperature to obtain Ti3C2Txa/Ag film. By using in-situ self-reduction technology, AgCl colloid as oxidant and Ti3C2TxMXene is a reducing agent, the loading capacity and the particle size of Ag are regulated and controlled by controlling the reaction time, and the synthetic method is simple and easy to implement; battery effect (conversion reaction) and Ti based on Ag nanoparticles3C2TxPseudo-capacitance behavior (ion intercalation) of (A) to prepare synthetic Ti3C2TxThe Ag film has excellent chloride ion removing capacity and good desalting performance.
Description
Technical Field
The invention belongs to the technical field of synthesis of environmental materials, and particularly relates to a novel chloride ion removing material Ti3C2TxA preparation method of/Ag and application thereof in capacitive deionization and desalination.
Background
With the continuous development of industry and agriculture and the increase of population, the problem of water resource shortage is increasingly highlighted. The seawater resource on the earth is rich, and if the seawater is desalinated, sufficient water resource can be provided for human beings. Seawater mainly contains a large amount of salt, and NaCl is a main component of seawater. At present, the seawater desalination technologies mainly comprise thermal evaporation, electrodialysis, multi-stage flash evaporation, reverse osmosis, electrochemical oxidation and the like, but the technologies have the defects of high energy consumption, heavy pollution, high cost and the like at different degrees, and the large-scale application of the technologies is hindered.
The Capacitive Deionization (CDI) technology, as a novel seawater desalination technology, has the characteristics of high energy efficiency, high cycle performance, simplicity and convenience in operation and the like, and attracts the attention of a large number of researchers in the world. At present, capacitive deionization and sodium removal electrodes (cathodes) are widely researched, but dechlorination electrodes (anodes) are less researched, so that further development of the electrodes is limited. The dechlorination electrode researched at present mainly comprises redox polymer, conducting polymer, MXene, Bi/BiOCl, VOCl and the like, and the materials have the defects of poor stability, low desalting capacity, low desalting rate and the like. Therefore, development of a novel chloride ion removal electrode having high desalination capacity, high desalination rate, and good cycle performance is demanded.
Disclosure of Invention
Aiming at the defects in the prior art, the invention mainly aims to provide a novel chloride ion removal material Ti3C2TxA preparation method of Ag.
It is a second object of the present invention to provide a novel chloride ion-removing material Ti3C2Tx/Ag。
The third object of the present invention is to provide the above-mentioned novel chloride ion removing material Ti3C2TxUse of/Ag.
In order to achieve the above purpose, the solution of the invention is as follows:
the technical scheme of the method is as follows:
novel material Ti for removing chloride ions3C2TxThe preparation method of/Ag is characterized in that: etching bulk Ti3AlC2Obtaining Ti of lamellar layer3C2Tx-MXene; ultrasonic stripping of Ti3C2Tx-MXene solution, supernatant to get Ti with less lamella3C2Tx-MXene solution; taking a certain amount of AgNO3Dissolving in deionized water, and adding a certain amount of hydrochloric acid under an ultrasonic condition to obtain an AgCl colloidal solution; adding the AgCl colloid into a few Ti sheets3C2TxOscillating MXene solution for a certain time under the conditions of constant temperature and constant rotating speed; vacuum filtering and separating the reacted mixture, washing with deionized water several times, and naturally drying at room temperature to obtain Ti3C2Txa/Ag film. The invention uses the in-situ self-reduction technology, uses AgCl colloid as an oxidant and uses Ti3C2TxMXene is a reducing agent, the loading capacity and the particle size of Ag are regulated and controlled by controlling the reaction time, and the synthetic method is simple and easy to implement; battery effect (conversion reaction) and Ti based on Ag nanoparticles3C2TxPseudo-capacitance behavior (ion intercalation) of (A) to prepare synthetic Ti3C2Txthe/Ag film shows excellent chloride ion removing capacity and has desalting performance of high capacity, high speed and high cycle performance under the condition of low energy consumption.
Novel material Ti for removing chloride ions3C2TxThe preparation method of/Ag comprises the following steps:
(1) weighing LiF, adding the LiF into a hydrochloric acid solution to obtain a first mixed solution, and heating in a water bath;
(2) adding Ti into the first mixed solution3AlC2Obtaining a second mixed solution, and continuing heating in a water bath;
(3) washing the obtained second mixed solution with anhydrous ethanol and deionized water for several times, and drying to obtain lamellar Ti3C2TxPowder;
(4) taking a certain amount of the obtained sheet Ti3C2TxDispersing the powder into deionized water, ultrasonically stripping and centrifuging to obtain a supernatant as a third mixed solution;
(5) measuring a third mixed solution with a certain volume, drying in an oven, weighing the obtained solid mass, and determining Ti in the third mixed solution3C2TxThe concentration of (c);
(6) according to the third mixed solution Ti3C2TxThe low-sheet Ti with specific concentration and specific volume is prepared3C2TxThe solution is a fourth mixed solution;
(7) weighing AgNO3Dissolving the solid in deionized water, and dropwise adding a hydrochloric acid solution under an ultrasonic state to form AgCl colloid as a fifth mixed solution;
(8) adding the fifth mixed solution into the fourth mixed solution to obtain a sixth mixed solution; in the step (8), an in-situ redox reaction occurs, wherein the fifth mixed solution AgCl colloid is equivalent to the oxidant, and the fourth mixed solution has few Ti layers3C2TxCorresponding to a reducing agent, thereby adding Ag+Reducing to Ag nano particles loaded to Ti3C2TxThe above.
(9) Putting the sixth mixed solution into a constant-temperature shaking table, and oscillating for a certain time to obtain a seventh mixed solution;
(10) vacuum-filtering and separating the seventh mixed solution, washing with deionized water, and naturally drying at room temperature to obtain Ti3C2Txa/Ag film.
Preferably, in the step (1), the addition amount of the LiF is 1g, the hydrochloric acid solution is obtained by mixing 5mL of deionized water and 15mL of 36% -38% concentrated hydrochloric acid, the temperature of water bath heating is 40 ℃, and the time is 30 min.
Preferably, in step (2), Ti3AlC2The amount of (1) was 1g, the temperature of the water bath heating was 40 ℃ and the time was 24 hours.
Preferably, in the step (3), the washing condition is that the solution is washed until the pH value is more than 5, and the drying condition is that the vacuum drying is carried out at 60 ℃ and the drying time is 12 h.
Preferably, in step (4), Ti is weighed3C2TxThe amount of the powder is 1g, the amount of the measured deionized water is 250mL, the ultrasonic condition is ultrasonic for 1h under Ar atmosphere, and the centrifugal condition is 3500rpm for 60 min.
Preferably, in the step (5), the third mixed solution Ti3C2TxThe concentration of (b) is about 2-4 mg/mL.
Preferably, in step (6), a specific few sheets of Ti are formulated3C2TxThe concentration of the solution was 2mg/mL and the volume was 15 mL.
Preferably, in step (7), AgNO is weighed3The mass of the solid is 25.39mg, the volume of the measured deionized water is 5mL, and the concentration and the volume of the hydrochloric acid solution are 1mol/L and 138 mu L respectively.
Preferably, in the step (9), the conditions of the constant temperature shaking table are 25 ℃, 150rpm and 0-24 h of oscillation time.
The technical scheme of the product is as follows:
the novel chloride ion removal material Ti obtained by the preparation method3C2Tx/Ag。
The application technical scheme is as follows:
the above-mentioned novel chloride ion-removing material Ti3C2Txthe/Ag is used as an anode for capacitive deionization and is used in capacitive deionization and desalination.
Due to the adoption of the scheme, the invention has the beneficial effects that:
firstly, dechlorination is carried out by conversion reaction of Ag and AgCl, the battery effect (conversion reaction) of Ag can be exerted, higher desalination capacity is realized, and meanwhile, the Ag also has the characteristics of high reaction rate, stable potential, corrosion resistance and antibiosis.
Second, with Ti3C2TxAs a carrier loaded by Ag nano-particles, the Ag nano-particles can effectively exert the advantages of a two-dimensional lamellar structure, uniformly disperse the Ag nano-particles and simultaneously facilitate the chlorine ions to be diffused into the crystal lattices of Ag for carrying out redox reaction. Further, Ti3C2TxAnd the ion-exchange membrane also has the characteristic of pseudo capacitance (ion intercalation), and can capture chlorine ions through intercalation, thereby increasing the removal capacity and rate of the chlorine ions.
Thirdly, Ag and Ti3C2TxCoupled together, can effectively exert the functions of battery (Ag) and pseudocapacitance (Ti)3C2Tx) The synergistic effect of (A) and (B) realizes the desalting performance with high capacity, high speed and high cyclicity.
And fourthly, regulating and controlling the size of the Ag nano particles by regulating and controlling the reaction time.
In summary, the present invention is achieved by combining Ag and Ti3C2TxCoupling is carried out, the advantages of battery effect (conversion reaction) and pseudocapacitance effect (ion intercalation) are fully exerted, and the defects of large and thick particles of Ag and Ti in the circulation process are overcome3C2TxDeficiency of low desalting capacity, Ti3C2Txthe/Ag compound forms a three-dimensional electron transport network, and electrons are in Ti3C2TxAnd the transmission is carried out between the sheet layers, so that the problem of poor conductivity of AgCl is solved. Thus, a novel chloride ion removal material Ti based on a battery-pseudocapacitive coupling mechanism3C2Txthe/Ag has desalting performance of high speed, high capacity and high cyclicity.
Drawings
FIG. 1 shows a novel chloride ion-removing material Ti according to the present invention3C2TxXRD patterns of/Ag at different reaction times.
FIG. 2 shows a novel chloride ion removing material Ti of the present invention3C2TxTEM images of/Ag at different reaction times.
FIG. 3 shows a novel chloride ion removing material Ti according to the present invention3C2TxOptical diagram of surface water contact angle of Ag at different reaction time.
FIG. 4 shows a novel chloride ion removing material Ti of the present invention3C2TxChloride desalination capacity plot of/Ag at different current densities.
FIG. 5 shows a novel chloride ion removing material Ti according to the present invention3C2TxDesalting energy consumption and chloride ion removal rate of/Ag.
FIG. 6 shows a novel chloride ion removing material Ti according to the present invention3C2TxCycle performance plot of/Ag.
FIG. 7 shows a novel chloride ion removing material Ti according to the present invention3C2TxDesalting mechanism diagram of/Ag.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
the novel chloride ion removal material Ti based on the battery-pseudocapacitive coupling mechanism of the embodiment3C2TxThe preparation method of the/Ag comprises the following steps:
(1) weighing 1g of LiF, adding the LiF into a hydrochloric acid solution (5mL of deionized water is mixed with 15mL of 36% -38% concentrated hydrochloric acid) to obtain a first mixed solution, and heating the first mixed solution in a water bath at 40 ℃ for 30 min;
(2) adding Ti into the first mixed solution3AlC2Obtaining a second mixed solution, and continuing heating in a water bath for 24 hours at the temperature of 40 ℃;
(3) washing the obtained second mixed solution with anhydrous ethanol and deionized water for several times until the pH of the solution is more than 5, and vacuum drying at 60 deg.C to obtain lamellar Ti3C2TxPowder;
(4) collecting 1g of the aboveResulting lamellar Ti3C2TxDispersing the powder into 250mL of deionized water, ultrasonically stripping for 1h under Ar atmosphere, and centrifuging for 60min at 3500rpm to obtain a supernatant which is a third mixed solution;
(5) measuring 5mL of third mixed solution, drying at 60 ℃ in vacuum, weighing to obtain the mass of solid, and determining Ti in the third mixed solution3C2TxThe concentration of (c);
(6) according to the third mixed solution Ti3C2TxThe concentration of (A) is 2mg/mL and 15mL of Ti with few sheets3C2TxThe solution is a fourth mixed solution;
(7) weighing 25.39mg AgNO3The solid was dissolved in 5mL of deionized water and 138 was added dropwise under sonication
Mu L of 1mol/L hydrochloric acid solution, and the formed AgCl colloid is a fifth mixed solution;
(8) adding the fifth mixed solution into the fourth mixed solution to obtain a sixth mixed solution;
(9) placing the sixth mixed solution into a constant-temperature shaking table, and oscillating for 3 hours at the rotation speed of 150rpm at the temperature of 25 ℃ to obtain a seventh mixed solution;
(10) vacuum-filtering and separating the seventh mixed solution, washing with deionized water, and naturally drying at room temperature to obtain Ti3C2Txa/Ag-3 film.
Example 2:
the novel chloride ion removal material Ti based on the battery-pseudocapacitive coupling mechanism of the embodiment3C2TxThe preparation method of the/Ag comprises the following steps:
(1) preparing 2mg/mL and 15mL of few-lamellar Ti3C2TxA solution;
(2) weighing 25.39mg AgNO3Dissolving the solid in 5mL of deionized water, and dropwise adding 138 mu L of 1mol/L hydrochloric acid solution under an ultrasonic state to form AgCl colloid;
(3) adding the AgCl colloid into a few Ti sheets3C2TxIn solution, then obtainPlacing the obtained mixed solution into a constant-temperature shaking table, and oscillating for 6h at the rotation speed of 150rpm and at the temperature of 25 ℃;
(4) vacuum filtering and separating the reacted mixed solution, washing with deionized water, and naturally drying at room temperature to obtain Ti3C2TxAg-6 film.
Example 3:
the novel chloride ion removal material Ti based on the battery-pseudocapacitive coupling mechanism of the embodiment3C2TxThe preparation method of the/Ag comprises the following steps:
(1) preparing 2mg/mL and 15mL of few-lamellar Ti3C2TxA solution;
(2) weighing 25.39mg AgNO3Dissolving the solid in 5mL of deionized water, and dropwise adding 138 mu L of 1mol/L hydrochloric acid solution under an ultrasonic state to form AgCl colloid;
(3) adding the AgCl colloid into a few Ti sheets3C2TxPutting the obtained mixed solution into a constant-temperature shaking table, and oscillating for 9 hours at the rotating speed of 150rpm and at the temperature of 25 ℃;
(4) vacuum filtering and separating the reacted mixed solution, washing with deionized water, and naturally drying at room temperature to obtain Ti3C2TxAg-9 film.
Example 4:
the novel chloride ion removal material Ti based on the battery-pseudocapacitive coupling mechanism of the embodiment3C2TxThe preparation method of the/Ag comprises the following steps:
(1) preparing 2mg/mL and 15mL of few-lamellar Ti3C2TxA solution;
(2) weighing 25.39mg AgNO3Dissolving the solid in 5mL of deionized water, and dropwise adding 138 mu L of 1mol/L hydrochloric acid solution under an ultrasonic state to form AgCl colloid;
(3) adding the AgCl colloid into a few Ti sheets3C2TxAdding the mixture into the solution, and placing the mixture into a constant temperature shaking table at 25 deg.C and 15 deg.COscillating for 12 hours at the rotating speed of 0 rpm;
(4) vacuum filtering and separating the reacted mixed solution, washing with deionized water, and naturally drying at room temperature to obtain Ti3C2TxAg-12 film.
< experiment >
The following experiments were carried out with the products of the above examples, respectively.
< experiment 1>
The purpose of this experiment was to characterize the novel chloride ion removing material Ti3C2The composition, morphology and hydrophilicity of Ag.
As shown in fig. 1, diffraction peaks at 38.14 °, 44.24 °, 64.48 ° and 77.38 ° of the four samples respectively correspond to diffraction peaks (111), (200), (220) and (311) of an Ag standard card with a body-centered cubic structure, which indicates that the simple substance of Ag exists in all the samples. In addition to Ti3C2Tx/Ag-3、Ti3C2TxIn the two samples of/Ag-6, there were two diffraction peaks at 32.18 ℃ and 46.18 ℃ corresponding to the (200) and (220) diffraction peaks in the AgCl standard card, respectively, indicating that the reaction did not proceed to completion at 3h and 6h, and that AgCl remained. This is mainly due to the lower solubility of AgCl in water, releasing Ag+The lower content limits the reaction rate of the whole oxidation-reduction process.
As shown in FIG. 2, in all the samples, Ti3C2TxThere is a significant lamellar structure. At Ti3C2TxIn the/Ag-3 sample, Ti3C2TxNano Ag particles with the average particle size of about 20nm are uniformly distributed on the sheet layer. At Ti3C2TxIn the Ag-6 sample, the Ag particles are significantly larger, and the average particle size is about 40 nm. As the reaction time increased to 9 hours, significant aggregation of Ag particles had occurred, and when the reaction time reached 12 hours, large-sized polycrystalline Ag particles, having a size of about 800nm, had been formed.
As shown in FIG. 3, all four samples were hydrophilic and the contact angles of the samples gradually decreased with increasing reaction time, indicating the samplesThe hydrophilicity becomes better and better. The reason is that along with the increase of the reaction time, the loading capacity of Ag is continuously increased, the content of AgCl is continuously reduced, so that the hydrophilicity of the sample is continuously enhanced, and after 9 hours, AgCl basically and completely reacts to generate an Ag simple substance, so that Ti3C2TxAg-9 and Ti3C2TxThe contact angles of the two samples,/Ag-12, did not change much.
< experiment 2>
The purpose of this experiment was to explore a novel chloride ion removing material Ti3C2TxDesalting performance, desalting rate and energy consumption of/Ag.
As shown in FIG. 4, Ti was added at current densities of 20, 30 and 50mA/g3C2TxThe Ag-3 samples all show the highest chloride ion removal capacity, and reach 374.7mg-Cl-/(g-Ti3C2TxAg-3), equal to about 308.7mg-NaCl/g-electrodes, is about sample Ti3C2Tx/Ag-12(100.5mg-Cl-/(g-Ti3C2TxAg-12)) 3.7 times.
As shown in FIG. 5, Ti3C2TxThe chloride removal rate of the/Ag-3 sample was 1.54mg-Cl-/(g-Ti3C2TxAg-3)/min. Albeit Ti3C2TxThe desalting capacity of the/Ag-6 sample is far lower than that of Ti3C2TxAg-3, but the removal rate of chloride ions can reach 2.95mg-Cl-/(g-Ti3C2TxAg-6)/min is Ti3C2TxAlmost 2 times that of the/Ag-3 sample. At a current density of 50mA/g, Ti3C2TxAg-3 and Ti3C2TxThe desalting energy consumption of the/Ag-6 sample is 0.36kWh/kg-Cl-Left and right.
< experiment 3>
The purpose of this experiment was to explore a novel chloride ion removing material Ti3C2TxThe cyclic stability and desalting mechanism of/Ag-3 are shown.
As shown in FIG. 6, the current density is high at 100mA/gAt the temperature, after 25 times of circulation, the capacity is not obviously greatly attenuated, which shows that Ti3C2Txthe/Ag-3 sample has higher cycling stability.
As shown in fig. 7, the desalination mechanism is mainly divided into the following three parts: (i) na (Na)+And Cl-Passing through a Cation Exchange Membrane (CEM) and an Anion Exchange Membrane (AEM), respectively; (ii) na (Na)+Diffusion to Ti3C2TxElectrode surface, then storing in Ti by intercalation3C2TxIn a lamellar structure; (iii) cl-Diffusion to Ti3C2TxThe Ag/Ag electrode surface is further diffused into the crystal lattice of Ag from the surface to generate AgCl through conversion reaction with Ag, thereby storing Cl-And also a portion of Cl-Is stored in Ti by intercalation3C2TxIn a lamellar structure.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.
Claims (10)
1. Novel material Ti for removing chloride ions3C2TxThe preparation method of/Ag is characterized in that: etching bulk Ti3AlC2Obtaining Ti of lamellar layer3C2Tx-MXene; ultrasonic stripping of Ti3C2Tx-MXene solution, supernatant to get Ti with less lamella3C2Tx-MXene solution; taking a certain amount of AgNO3Dissolving in deionized water, and adding a certain amount of hydrochloric acid under an ultrasonic condition to obtain an AgCl colloidal solution; adding the AgCl colloid into a few Ti sheets3C2Tx-MXeneOscillating for a certain time in the solution under the conditions of constant temperature and constant rotating speed; vacuum filtering and separating the reacted mixture, washing with deionized water several times, and naturally drying at room temperature to obtain Ti3C2Txa/Ag film.
2. The novel chloride ion removing material Ti as claimed in claim 13C2TxThe preparation method of/Ag comprises the following steps:
(1) weighing LiF, adding the LiF into a hydrochloric acid solution to obtain a first mixed solution, and heating in a water bath;
(2) adding Ti into the first mixed solution3AlC2Obtaining a second mixed solution, and continuing heating in a water bath;
(3) washing the obtained second mixed solution with anhydrous ethanol and deionized water for several times, and drying to obtain lamellar Ti3C2TxPowder;
(4) taking a certain amount of the obtained sheet Ti3C2TxDispersing the powder into deionized water, ultrasonically stripping and centrifuging to obtain a supernatant as a third mixed solution;
(5) measuring a third mixed solution with a certain volume, drying in an oven, weighing the obtained solid mass, and determining Ti in the third mixed solution3C2TxThe concentration of (c);
(6) according to the third mixed solution Ti3C2TxThe low-sheet Ti with specific concentration and specific volume is prepared3C2TxThe solution is a fourth mixed solution;
(7) weighing AgNO3Dissolving the solid in deionized water, and dropwise adding a hydrochloric acid solution under an ultrasonic state to form AgCl colloid as a fifth mixed solution;
(8) adding the fifth mixed solution into the fourth mixed solution to obtain a sixth mixed solution;
(9) putting the sixth mixed solution into a constant-temperature shaking table, and oscillating for a certain time to obtain a seventh mixed solution;
(10) vacuum-pumping the seventh mixed solutionFiltering and separating, washing with deionized water, and naturally drying at room temperature to obtain Ti3C2Txa/Ag film.
3. The novel chloride ion removing material Ti as claimed in claim 23C2TxThe preparation method of/Ag is characterized in that: in the step (1), the addition amount of the LiF is 1g, the hydrochloric acid solution is obtained by mixing 5mL of deionized water and 15mL of 36% -38% concentrated hydrochloric acid, the water bath heating temperature is 40 ℃, and the time is 30 min.
4. The novel chloride ion removing material Ti as claimed in claim 23C2TxThe preparation method of/Ag is characterized in that: in the step (2), Ti3AlC2The amount of (1) was 1g, the temperature of the water bath heating was 40 ℃ and the time was 24 hours.
5. The novel chloride ion removing material Ti as claimed in claim 13C2TxThe preparation method of/Ag is characterized in that: in the step (3), the washing condition is that the pH value of the solution is greater than 5, the drying condition is that the solution is dried in vacuum at the temperature of 60 ℃, and the drying time is 12 hours;
in the step (4), weighed Ti3C2TxThe amount of the powder is 1g, the amount of the measured deionized water is 250mL, the ultrasonic condition is ultrasonic for 1h in Ar atmosphere, and the centrifugal condition is 3500rpm centrifugal for 60 min;
in the step (5), the third mixed solution Ti3C2TxThe concentration of (b) is about 2-4 mg/mL.
6. The novel chloride ion removing material Ti as claimed in claim 13C2TxThe preparation method of/Ag is characterized in that: in the step (6), the specific few-layer Ti is prepared3C2TxThe concentration of the solution was 2mg/mL and the volume was 15 mL.
7. The novel of claim 1Material Ti for removing chloride ion3C2TxThe preparation method of/Ag is characterized in that: in step (7), AgNO is weighed3The mass of the solid is 25.39mg, the volume of the measured deionized water is 5mL, and the concentration and the volume of the hydrochloric acid solution are 1mol/L and 138 mu L respectively.
8. The novel chloride ion removing material Ti as claimed in claim 13C2TxThe preparation method of/Ag is characterized in that: in the step (9), the conditions set by the constant temperature shaking table are 25 ℃, 150rpm and 0-24 h of oscillation time.
9. Novel material Ti for removing chloride ions3C2TxAg, characterized in that: obtained by the process according to any one of claims 1 to 8.
10. The novel chloride ion removing material Ti as claimed in claim 93C2TxThe application of/Ag in capacitive deionization and desalination.
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