CN115650378A - MgFe-LDH/AC composite electrode material, and preparation method and application of capacitor electrode - Google Patents
MgFe-LDH/AC composite electrode material, and preparation method and application of capacitor electrode Download PDFInfo
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- 239000007772 electrode material Substances 0.000 title claims abstract description 74
- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 239000003990 capacitor Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 95
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000001035 drying Methods 0.000 claims abstract description 43
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- 239000002244 precipitate Substances 0.000 claims abstract description 20
- 239000002002 slurry Substances 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 12
- 239000006229 carbon black Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 159000000003 magnesium salts Chemical class 0.000 claims abstract description 5
- 238000007873 sieving Methods 0.000 claims abstract description 5
- 150000002505 iron Chemical class 0.000 claims abstract description 4
- 239000000758 substrate Substances 0.000 claims abstract description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 11
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 11
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 244000144972 livestock Species 0.000 claims description 9
- 238000011068 loading method Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000007790 scraping Methods 0.000 claims description 4
- 238000000975 co-precipitation Methods 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 34
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 34
- 239000011574 phosphorus Substances 0.000 abstract description 34
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 10
- 238000004140 cleaning Methods 0.000 abstract description 6
- 238000002242 deionisation method Methods 0.000 abstract description 4
- -1 Polytetrafluoroethylene Polymers 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 239000011259 mixed solution Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 17
- 150000002500 ions Chemical class 0.000 description 15
- 238000001179 sorption measurement Methods 0.000 description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 10
- 229910052802 copper Inorganic materials 0.000 description 10
- 239000010949 copper Substances 0.000 description 10
- 238000000926 separation method Methods 0.000 description 9
- 244000144977 poultry Species 0.000 description 8
- 230000005684 electric field Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 238000005342 ion exchange Methods 0.000 description 5
- 150000001450 anions Chemical class 0.000 description 4
- 239000011267 electrode slurry Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910000000 metal hydroxide Inorganic materials 0.000 description 3
- 150000004692 metal hydroxides Chemical class 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 235000015097 nutrients Nutrition 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention belongs to the technical field of water treatment, and discloses an MgFe-LDH/AC composite electrode material, a capacitor electrode preparation method and application, wherein the MgFe-LDH/AC composite electrode material, the capacitor electrode preparation method and the application of the MgFe-LDH/AC composite capacitor electrode in a CDI device are included, and the MgFe-LDH/AC composite electrode material and the capacitor electrode preparation method are divided into two steps: 1, preparing MgFe-LDH/AC composite electrode material: putting magnesium salt and iron salt into deionized water for dissolving, then adding activated carbon for uniformly mixing, adjusting the pH value of the solution to 13, and cleaning, drying, grinding and sieving the obtained precipitate to obtain the required electrode material; preparing an MgFe-LDH/AC composite capacitance electrode: taking a titanium mesh as a substrate, uniformly mixing an electrode material with Polytetrafluoroethylene (PTFE), carbon black and N-methylpyrrolidone (NMP), then blade-coating the mixture on the titanium mesh, and then drying to prepare the capacitance electrode. The prepared electrode is used as a cathode and an anode of a Capacitive Deionization (CDI) device for recovering phosphorus resources in biogas slurry and removing heavy metals.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a MgFe-LDH/AC composite electrode material, a preparation method of a capacitor electrode and application of the capacitor electrode.
Background
The livestock and poultry biogas slurry contains high-concentration nitrogen, phosphorus, potassium and other nutrient elements, and has a high resource utilization value, but because the feed additive fed by livestock and poultry contains heavy metals, the heavy metal ions are discharged out of the body along with the metabolic activity of the livestock and poultry and enter the biogas slurry. The traditional phosphorus recovery method can not simultaneously realize separation and concentration of nutrient substances such as phosphorus and the like in the livestock and poultry biogas slurry and removal of heavy metal ions.
The Capacitive Deionization (CDI) technology is a novel water treatment technology, and the principle thereof is that charged ions in inlet water move to electrodes with opposite electric properties under the action of an electric field force, and the technology can realize the separation of phosphate ions with negative electricity and heavy metal ions with positive electricity. However, the concentration of chloride ions in the livestock and poultry biogas slurry is far higher than that of phosphate ions, the concentration of ammonium ions is far higher than that of heavy metal ions, and the selective adsorption capacity of Activated Carbon (AC) electrodes commonly used in CDI on ions is weak, so that a high-selectivity electrode material is needed to promote the selective adsorption of CDI on ions in inlet water, and therefore MgFe-LDH (layered hydroxide) and AC are adopted to prepare the capacitor electrode in a composite mode to promote the selective adsorption capacity of the electrode material on ions.
Disclosure of Invention
The invention aims to provide an MgFe-LDH/AC composite electrode material, a capacitor electrode preparation method and application, and aims to solve the problems in the background technology.
In order to achieve the above purpose, the invention provides the following technical scheme: the MgFe-LDH/AC composite electrode material, the capacitor electrode preparation method and the application thereof comprise the MgFe-LDH/AC composite electrode material, the capacitor electrode preparation method and the application of the MgFe-LDH/AC composite capacitor electrode in a CDI device, and the MgFe-LDH/AC composite electrode material and the capacitor electrode preparation method are divided into two steps:
step 1: preparing an MgFe-LDH/AC composite electrode material: putting magnesium salt and ferric salt into deionized water for dissolving, then adding activated carbon for uniformly mixing, preparing an electrode material by adopting a coprecipitation method by adjusting the pH value of the solution to 13, washing the obtained precipitate with a large amount of deionized water until the precipitate is neutral, drying the obtained precipitate, grinding the precipitate, and sieving the ground precipitate with a 100-mesh sieve;
step 2: preparing an MgFe-LDH/AC composite capacitance electrode: and taking a titanium mesh as a substrate, uniformly mixing an electrode material with PTFE, carbon black and NMP, then blade-coating the electrode material on the titanium mesh, and drying to prepare the capacitor electrode.
Preferably, mgCl2 and FeCl3 are respectively adopted as the magnesium salt and the iron salt in the step 1;
in the step 1, 5g of activated carbon is taken, and MgCl2 and FeCl3 are put into 200mL of deionized water according to the molar ratio of metal elements to atoms of 2, the mass ratio of the metal elements to the activated carbon (0.15 to 0.6) of 1.
Preferably, the precipitate obtained in the step 1 is dried in a constant temperature drying oven at 80-120 ℃ for 12-24h.
Preferably, in the step 2, the 100-mesh titanium mesh is sequentially ultrasonically cleaned by acetone, hydrochloric acid, ethanol and deionized water and then dried for later use.
Preferably, the area of the titanium mesh in the step 2 is 4 x 4cm 2 。
Preferably, in the step 2, the MgFe-LDH/AC composite electrode material, the carbon black and the PTFE are fully and uniformly mixed in a mortar according to a mass ratio of 8 2 And obtaining the CDI electrode.
Preferably, the MgFe-LDH/AC composite capacitance electrode is applied to a CDI device and comprises the following steps:
and (3) taking the MgFe-LDH/AC composite capacitor electrode in the step (2) as a cathode and an anode of a CDI device for treating the livestock and poultry biogas slurry, wherein the CDI capacitor device operates in a circulation mode, the water flow direction is downward inlet and upward outlet, 0.4-1.4V voltage is applied to two ends of the capacitor device, the inflow flow rate of the capacitor device is 27.5mL/min, and the operation is 90min.
The invention has the following beneficial effects:
1. compared with the existing biogas slurry recovery technology, the invention can realize the separation and concentration of nutrient substances such as phosphorus and the like and the removal of heavy metal ions in the livestock and poultry biogas slurry through a capacitive deionization technology (CDI), namely anions such as phosphate ions and the like are enriched in the anode of the CDI, and heavy metal ions are deposited in the cathode of the CDI, so that a phosphorus product with high added value is obtained, the risk caused by the heavy metal in the livestock and poultry biogas slurry is favorably controlled, and the method is a biogas slurry treatment mode with great potential.
2. The capacitive deionization technology adopted by the invention can release the adsorbed ions by short-circuiting or reverse connection of the electrodes after the electrodes are adsorbed and saturated, and the electrodes are regenerated.
3. The invention selects MgCl2 and FeCl3 to prepare the layered double hydroxide, and the selected metal elements have low biological toxicity.
4. The MgFe-LDH and the activated carbon are compounded, so that the conductivity of the layered double hydroxide can be improved, the specific surface area of the composite material can be increased, and the adsorption capacity can be improved.
Drawings
FIG. 1 is a scanning electron microscope photograph of MgFe-LDH/AC in accordance with a preferred embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
(1) Taking 5g of activated carbon, putting MgCl2 and FeCl3 into 200mL of deionized water according to the molar ratio of metal elements as 2 to 1 and the mass ratio of the metal elements to the activated carbon as 0.15-0.6 to 1 to obtain a mixture of a metal ion solution and the activated carbon, and fully stirring for 1h;
the proportion and the quality of the active carbon, the deionized water, the MgCl2 and the FeCl3 are controlled, and the stirring time is controlled according to the current mixing proportion, so that the obtained mixed solution is more in line with the standard and the requirement;
(2) Dropwise adding a 10wt% NaOH solution into the mixed solution obtained in the step (1) to adjust the pH value to about 13, washing the obtained precipitate with a large amount of deionized water to be neutral, drying the obtained precipitate in a constant-temperature drying oven at 80 ℃ for 24 hours, grinding the dried electrode material, and sieving with a 100-mesh sieve;
the pH of the mixed solution of step (1) was adjusted to a prescribed range by dropwise addition of a 10wt% NaOH solution so that the formed MgFe-LDH was supported on the AC surface, and then washed to neutrality to remove impurities. Strictly controlling the drying environment and time of the obtained precipitate so as to achieve better drying effect, and then grinding the dried electrode material until the electrode material can pass through a 100-mesh sieve, wherein FIG. 1 is a scanning electron microscope image of MgFe-LDH/AC of a preferred embodiment, and FIG. 1 shows a lamellar structure of the MgFe-LDH material, which can be used as a CDI electrode material;
(3) 100 mesh titanium mesh (4X 4 cm) 2 ) Ultrasonically cleaning the mixture by using acetone, hydrochloric acid, ethanol and deionized water in sequence and then drying the mixture for later use;
the titanium mesh is sequentially cleaned by acetone, hydrochloric acid, ethanol and deionized water in an ultrasonic manner and then dried, so that the surface of the titanium mesh is cleaned for use;
(4) Fully grinding the composite electrode material obtained in the step (2), carbon black and PTFE in a mortar according to a mass ratio of 8;
the MgFe-LDH/AC composite electrode material, carbon black and PTFE are fully and uniformly mixed according to the mass ratio of 8;
(5) Uniformly scraping the electrode slurry which is uniformly ground on a cleaned titanium mesh by using a scraper, and drying the electrode slurry for 24 hours in a constant-temperature drying oven at the temperature of 80 ℃, wherein the loading capacity of the electrode material is 6 mg/cm 2 ；
The drying effect is better by controlling the drying environment and time during drying. The loading capacity of the electrode material is clearly indicated, so that when slurry of the electrode material is coated in a blade mode, the slurry does not appear to be too thick or too thin, and a qualified CDI electrode is obtained;
(6) Taking the electrode obtained in the step (5) as a cathode and an anode of a CDI device, and adsorbing phosphorus in the mixed solution of 500mg/L nitrogen and 20mg/L phosphorus;
by using the MgFe-LDH/AC composite electrode obtained in the step (5) as the cathode and the anode of the CDI device, when in use, because the MgFe-LDH is a two-dimensional (2D) ion layered compound consisting of positively charged metal hydroxide layers and exchangeable anions filled between the layers, phosphorus in a mixed solution (a mixed solution of 500mg/L nitrogen-20 mg/L phosphorus) can be separated and adsorbed by adsorption and ion exchange under the action of an electric field when power is supplied.
(7) Adjusting the initial pH of the inflow solution to be 6, operating the CDI capacitor device in a circulation mode, wherein the water flow direction is downward inlet and upward outlet, applying 1V voltage to two ends of the capacitor device, and operating the capacitor device for 90min at the inflow flow rate of 27.5 mL/min;
the CDI capacitor device runs in a circulation mode, and flows in a water flow mode in a mode of feeding water from bottom to top, so that the separation effect is better. 1V voltage is applied to two ends of the capacitor device, and under the action of an electric field, phosphorus resources in water are recovered in an adsorption and ion exchange mode. Controlling the flow rate of the inflow water to be 27.5mL/min and the running time to be 90min, so that the water can obtain enough residence time in the capacitor device, and the separation effect is better;
(8) And the mass ratio of the metal elements to the activated carbon is (0.15-0.6): 1, and the removal rate of phosphorus for the cathode and the anode of the CDI device is about 39-52%. When the mass ratio of the metal elements to the activated carbon is 0.3.
By adjusting the mass ratio of the metal elements to the activated carbon, the electrode of the prepared CDI device has better adsorption and removal effects on phosphorus. Experiments show that when the mass ratio of the metal element to the activated carbon is (0.15 to 0.6): 1, the removal rate of the CDI device to phosphorus is about 39-52%, and when the mass ratio of the metal element to the activated carbon is 0.3.
Example 2:
(1) Taking 5g of activated carbon, putting MgCl2 and FeCl3 into 200mL of deionized water according to the molar ratio of metal elements to the activated carbon of 0.3;
the proportion and the quality of the active carbon, the deionized water, the MgCl2 and the FeCl3 are controlled, and the stirring time is controlled according to the current mixing proportion, so that the obtained mixed solution is more in line with the standard and the requirement;
(2) Dripping a 10wt% NaOH solution into the mixed solution obtained in the step (1) dropwise until the pH value is adjusted to about 13, washing the obtained precipitate with a large amount of deionized water until the precipitate is neutral, drying the obtained precipitate in a constant-temperature drying oven at 80 ℃ for 24 hours, grinding the dried electrode material, and screening the ground electrode material with a 100-mesh screen;
the pH of the mixed solution of step (1) was adjusted to a prescribed range by dropwise addition of a 10wt% NaOH solution so that the formed MgFe-LDH was supported on the AC surface, and then washed to neutrality to remove impurities. Strictly controlling the drying environment and time of the obtained precipitate so as to ensure that the drying effect is better, and then grinding the dried electrode material until the electrode material can pass through a 100-mesh sieve;
(3) 100 mesh titanium mesh (4X 4 cm) 2 ) Ultrasonically cleaning the mixture by using acetone, hydrochloric acid, ethanol and deionized water in sequence, and drying the mixture for later use;
the method comprises the following steps of ultrasonically cleaning a titanium mesh with acetone, hydrochloric acid, ethanol and deionized water in sequence, and then drying to clean the surface of the titanium mesh for later use;
(4) Fully grinding the composite electrode material obtained in the step (2), carbon black and PTFE in a mortar according to the mass ratio of 8;
fully and uniformly mixing the MgFe-LDH/AC composite electrode material, carbon black and PTFE according to a mass ratio of 8;
(5) Will grind uniformlyUniformly scraping the electrode slurry on the cleaned titanium mesh by using a scraper, and drying for 24 hours in a constant-temperature drying oven at 80 ℃, wherein the loading capacity of the electrode material is 6 mg/cm 2 ；
The drying effect is better by controlling the drying environment and time during drying. The loading capacity of the electrode material is clearly indicated, so that the electrode material slurry does not appear too thick or too thin when being subjected to blade coating, and a qualified CDI electrode is obtained;
(6) Taking the electrode obtained in the step (5) as a cathode and an anode of a CDI device, and adsorbing phosphorus in the mixed solution of 500mg/L nitrogen and 20mg/L phosphorus;
by using the MgFe-LDH/AC composite electrode obtained in the step (5) as the cathode and the anode of the CDI device, when in use, because the MgFe-LDH is a two-dimensional (2D) ion layered compound consisting of positively charged metal hydroxide layers and exchangeable anions filled between the layers, phosphorus in a mixed solution (a mixed solution of 500mg/L nitrogen-20 mg/L phosphorus) can be separated and adsorbed by adsorption and ion exchange under the action of an electric field when power is supplied.
(7) Adjusting the initial pH of the water inflow solution to be 6, operating the CDI capacitance device in a circulation mode, wherein the water flow direction is downward, upward and downward, applying voltages of 0.4 to 1.4V to two ends of the capacitance device respectively, and operating the capacitance device for 90min at the water inflow flow rate of 27.5 mL/min;
the CDI capacitor device runs in a circulation mode, and flows in a water flow mode in a mode of going in and out from bottom to top, so that the separation effect is better. Applying 0.4-1.4V voltage to two ends of the capacitor device, testing how different recovery and removal effects of phosphorus resources in water are under the action of electric fields formed by different voltages, controlling the water inflow flow rate to be 27.5mL/min and the running time to be 90min, so that the water can obtain enough residence time in the capacitor device, and the separation effect is better;
(8) When different voltages are applied to the CDI device, the removal rate of phosphorus is about 41-52%. When the voltage applied to the CDI device is 1.0V, the phosphorus can achieve a better adsorption effect, and the removal rate of the phosphorus reaches about 52 percent.
Experiments show that when a voltage in the range of 0.4 to 1.4V is applied to a CDI device, the removal rate of phosphorus in an influent solution with the initial pH of 6 is about 41 to 52 percent, and when the voltage is applied to the CDI device at 1.0V, the phosphorus can achieve a better adsorption effect, and the removal rate of the phosphorus reaches about 52 percent.
Example 3:
(1) Taking 5g of activated carbon, putting MgCl2 and FeCl3 into 200mL of deionized water according to the molar ratio of metal elements to the activated carbon of 0.3;
the proportion and the quality of the active carbon, the deionized water, the MgCl2 and the FeCl3 are controlled, and the stirring time is controlled according to the current mixing proportion, so that the obtained mixed solution is more in line with the standard and the requirement;
(2) Dropwise adding a 10wt% NaOH solution into the mixed solution obtained in the step (1) to adjust the pH value to about 13, washing the obtained precipitate with a large amount of deionized water to be neutral, drying the obtained precipitate in a constant-temperature drying oven at 80 ℃ for 24 hours, grinding the dried electrode material, and sieving with a 100-mesh sieve;
the pH of the mixed solution of step (1) was adjusted to a prescribed range by dropwise addition of a 10wt% NaOH solution so that the formed MgFe-LDH was supported on the AC surface, and then washed to neutrality to remove impurities. Strictly controlling the drying environment and time of the obtained precipitate so as to ensure that the drying effect is better, and then grinding the dried electrode material until the electrode material can pass through a 100-mesh sieve;
(3) 100 mesh titanium mesh (4X 4 cm) 2 ) Ultrasonically cleaning the mixture by using acetone, hydrochloric acid, ethanol and deionized water in sequence, and drying the mixture for later use;
the method comprises the following steps of ultrasonically cleaning a titanium mesh with acetone, hydrochloric acid, ethanol and deionized water in sequence, and then drying to clean the surface of the titanium mesh for later use;
(4) Fully grinding the composite electrode material obtained in the step (2), carbon black and PTFE in a mortar according to a mass ratio of 8;
the MgFe-LDH/AC composite electrode material, carbon black and PTFE are fully and uniformly mixed according to the mass ratio of 8;
(5) Uniformly scraping and coating the uniformly ground electrode slurry on the cleaned titanium mesh by using a scraper, and drying for 24 hours in a constant-temperature drying oven at the temperature of 80 ℃, wherein the loading capacity of the electrode material is 6 mg/cm 2 ；
The drying effect is better by controlling the drying environment and time during drying. The loading capacity of the electrode material is clearly indicated, so that the electrode material slurry does not appear too thick or too thin when being subjected to blade coating, and a qualified CDI electrode is obtained;
(6) Treating the mixed solution of 500mg/L nitrogen-20 mg/L phosphorus-2 mg/L copper by using the electrode obtained in the step (5) as a cathode and an anode of a CDI device;
by using the MgFe-LDH/AC composite electrode obtained in the step (5) as a cathode and an anode of a CDI device, when in use, because the MgFe-LDH is a two-dimensional (2D) ion layered compound consisting of a positively charged metal hydroxide layer and exchangeable anions filled between layers, phosphorus and copper in a mixed solution (a mixed solution of 500mg/L nitrogen-20 mg/L phosphorus-2 mg/L copper) can be separated and adsorbed by adsorption and ion exchange under the action of an electric field when being electrified;
(7) Adjusting the initial pH of the water inflow solution to be 4-10 respectively, adopting a circulation mode for a CDI capacitance device, enabling the water flow direction to be downward, upward and downward, applying 1V voltage to two ends of the capacitance device, enabling the water inflow flow rate of the capacitance device to be 27.5mL/min, and operating for 90min;
the effect of removing phosphorus and copper in the water inflow solutions with different pH values of the CDI capacitance device is determined by adjusting the initial pH values of the water inflow solutions to be 4-10 respectively. The CDI capacitor device runs in a circulation mode, and flows in a water flow mode in a mode of feeding water from bottom to top, so that the separation effect is better. 1V voltage is applied to two ends of the capacitor device, and under the action of an electric field, phosphorus and heavy metal ions in water are adsorbed in adsorption and ion exchange modes. Controlling the flow rate of the inflow water to be 27.5mL/min and the running time to be 90min, so that the water can obtain enough residence time in the capacitor device, and the separation effect is better;
(8) Under the condition that the initial pH value is 4 to 10, the removal rate of phosphorus is about 29 to 61 percent, the removal rate of copper is about 84 to 98 percent, when the pH value is 6, phosphorus and copper can achieve a good removal effect, the removal rate of phosphorus reaches about 61 percent, and the removal rate of copper reaches about 96 percent.
Experiments show that when a voltage of 1V is applied to two ends of the capacitor device, the initial pH of the water inlet solution is adjusted in the range of 4 to 10 respectively, the removal rate of phosphorus is about 29-61%, the removal rate of copper is about 84-98%, when the initial pH of the water inlet solution is adjusted to 6, the phosphorus and the copper can achieve a good removal effect, the removal rate of phosphorus reaches about 61%, and the removal rate of copper reaches about 96%.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The MgFe-LDH/AC composite electrode material, the capacitor electrode preparation method and the application of the MgFe-LDH/AC composite capacitor electrode in a CDI device are characterized in that: the preparation method of the MgFe-LDH/AC composite electrode material and the capacitor electrode comprises the following two steps:
step 1: preparing an MgFe-LDH/AC composite electrode material: dissolving magnesium salt and iron salt in deionized water, adding activated carbon, mixing uniformly, adjusting the pH value of the solution to 13, preparing an electrode material by adopting a coprecipitation method, washing the obtained precipitate with a large amount of deionized water, washing to be neutral, drying the obtained precipitate, grinding, and sieving by using a 100-mesh sieve;
step 2: preparing an MgFe-LDH/AC composite capacitance electrode: and taking a titanium mesh as a substrate, uniformly mixing an electrode material with PTFE, carbon black and NMP, then blade-coating the electrode material on the titanium mesh, and drying to prepare the capacitor electrode.
2. The MgFe-LDH/AC composite electrode material, the capacitance electrode preparation method and the application of the MgFe-LDH/AC composite electrode material as claimed in claim 1, wherein the MgFe-LDH/AC composite electrode material comprises the following steps: the magnesium salt and the iron salt in the step 1 adopt MgCl2 and FeCl3 respectively;
in the step 1, 5g of activated carbon is taken, and MgCl2 and FeCl3 are put into 200mL of deionized water according to the molar ratio of metal elements to atoms of 2:1 and the mass ratio of the metal elements to the activated carbon (0.15 to 0.6): 1.
3. The MgFe-LDH/AC composite electrode material, the capacitance electrode preparation method and the application of the MgFe-LDH/AC composite electrode material as claimed in claim 1, wherein the MgFe-LDH/AC composite electrode material comprises the following steps: and (3) drying the precipitate obtained in the step (1) in a constant-temperature drying oven at the temperature of 80-120 ℃ for 12-24h.
4. The MgFe-LDH/AC composite electrode material, the capacitance electrode preparation method and the application of the MgFe-LDH/AC composite electrode material as claimed in claim 1, wherein the MgFe-LDH/AC composite electrode material comprises the following steps: and in the step 2, the titanium mesh with 100 meshes is ultrasonically cleaned and dried by acetone, hydrochloric acid, ethanol and deionized water in sequence for later use.
5. The MgFe-LDH/AC composite electrode material, the capacitance electrode preparation method and the application of the MgFe-LDH/AC composite electrode material as claimed in claim 1, wherein the MgFe-LDH/AC composite electrode material comprises the following steps: the area of the titanium mesh in the step 2 is 4 multiplied by 4cm 2 。
6. The MgFe-LDH/AC composite electrode material, the capacitance electrode preparation method and the application of the MgFe-LDH/AC composite electrode material as claimed in claim 1, wherein the MgFe-LDH/AC composite electrode material comprises the following steps: in the step 2, mgFe-LDH/AC composite electrode material, carbon black and PTFE are mixed1, sufficiently and uniformly mixing in a mortar, and adding 1.5mL of NMP into each gram of the mixture to dissolve into paste; uniformly scraping the uniformly mixed electrode material slurry on a cleaned titanium mesh by using a scraper, and drying the titanium mesh in a constant-temperature drying oven at 80-120 ℃ for 12-24h, wherein the loading capacity of the electrode material is 6 mg/cm 2 And obtaining the CDI electrode.
7. The MgFe-LDH/AC composite electrode material, the capacitor electrode preparation method and the application of claim 1 are characterized in that: the application of the MgFe-LDH/AC composite capacitance electrode in a CDI device comprises the following steps:
and the MgFe-LDH/AC composite capacitance electrode in the step 2 is used as a cathode and an anode of the CDI device and is used for treating the livestock biogas slurry.
8. The MgFe-LDH/AC composite electrode material, the capacitance electrode preparation method and the application of the MgFe-LDH/AC composite electrode material as claimed in claim 7, wherein the MgFe-LDH/AC composite electrode material comprises the following steps: the CDI capacitor device runs in a circulation mode, the water flow direction is downward inlet and upward outlet, 0.4-1.4V voltage is applied to two ends of the capacitor device, the water inlet flow rate of the capacitor device is 27.5mL/min, and the operation is 90min.
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