CN112808024A - MXene-CNT photo-thermal composite membrane for self-floating removal of organic dye and realization of clean water regeneration and preparation method thereof - Google Patents
MXene-CNT photo-thermal composite membrane for self-floating removal of organic dye and realization of clean water regeneration and preparation method thereof Download PDFInfo
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- CN112808024A CN112808024A CN202110015189.1A CN202110015189A CN112808024A CN 112808024 A CN112808024 A CN 112808024A CN 202110015189 A CN202110015189 A CN 202110015189A CN 112808024 A CN112808024 A CN 112808024A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/021—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/14—Treatment of water, waste water, or sewage by heating by distillation or evaporation using solar energy
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
Abstract
The invention discloses a preparation method of an MXene-CNT photo-thermal composite membrane for self-floating removal of organic dye and realization of clean water regeneration. The preparation method comprises the following steps: 1) preparing MXene nano material by etching with hydrofluoric acid; 2) weighing MXene and CNT powder, respectively mixing with ultrapure water according to the ratio of mg: mL to 1:1, and respectively performing ultrasonic treatment for 10-15min under the condition that the ultrasonic power is 20-25 kHZ; 3) uniformly mixing the two nano materials subjected to ultrasonic treatment respectively or alternatively performing suction filtration on a polyurethane sponge base film soaked for more than 8 hours by using polyvinyl alcohol (PVA) by adopting a vacuum suction filtration pump according to different sequences to prepare a composite film; 4) putting the composite membrane prepared in the step 3) into a vacuum drying oven to be dried for 8-12h at the temperature of 40-50 ℃; the composite membrane has higher removal efficiency and higher regeneration efficiency of clean water on organic dye, has strong structural performance stability, is easy to regenerate, and greatly prolongs the service life of the composite membrane.
Description
Technical Field
The invention relates to the technical field of photo-thermal adsorption materials, in particular to a preparation method of an MXene-CNT photo-thermal composite membrane for self-floating organic dye removal and clean water regeneration.
Background
The current method for removing organic pollutants in water bodies has the defects of contradiction between material selectivity and permeability, short service life, low clean water recovery rate, high energy consumption, difficult concentrated water treatment and the like, so that the large-scale popularization and application of the method are restricted. Therefore, it is important to develop a novel water treatment membrane material and a novel water treatment process for reducing treatment energy consumption and cost and effectively realizing the regeneration and utilization of polluted water while ensuring the efficient removal efficiency of organic pollutants.
Disclosure of Invention
The invention aims to provide a preparation method of an MXene-CNT photo-thermal composite membrane for self-floating removal of organic dyes in a water body and realization of clean water regeneration.
The purpose of the invention is realized by the following technical scheme:
the preparation method of the MXene-CNT photo-thermal composite membrane for self-floating removal of organic dye and realization of clean water regeneration is characterized by comprising the following steps:
1) weighing CNT powder and MXene powder according to a mass ratio of 1:1, mixing with ultrapure water according to a ratio of mg: mL to 1:1, and performing ultrasonic treatment for 10-15min under the condition of 20-25 kHZ; etching MXene powder with 20-30mL of 40-50 wt% hydrofluoric acid solution per gram of Ti3AlC2 powder for 24h, centrifuging, and removing upper layer liquid; repeatedly performing ultrasonic treatment with deoxygenated water, centrifuging, cleaning, precipitating, and drying until pH of the liquid is greater than 6;
2) uniformly mixing the CNT turbid liquid and the MXene turbid liquid which are respectively subjected to ultrasonic dispersion, and performing suction filtration treatment, or alternatively performing suction filtration treatment on the two kinds of ultrasonically dispersed turbid liquids according to different sequences; forming MXene-CNT photo-thermal composite films with three different structures;
3) drying in a vacuum drying oven at 40-50 deg.C for 8-12 hr; the mass of the nano material covered by each square meter of the composite film is 7-10 g.
Further, the basement membrane was placed in 2-5mg mL before suction filtration-1The PVA binder solution is soaked for more than 8 hours.
Further, polyurethane sponge is used as a base film.
The preparation method of the MXene-CNT photo-thermal composite membrane for removing the organic dye and realizing clean water regeneration is characterized in that the microstructure of the composite membrane is influenced by the sequence of CNT and MXene suction filtration, and further the capability of the trace composite membrane in carrying out clean water distillation and the capability of the trace composite membrane in treating pollutants are influenced.
The invention ensures the stability and hydrophilicity of the composite membrane by the following preparation method:
1) commercially purchasing polyurethane sponge, and cleaning with ultrapure water to remove impurities;
2) soaking the cleaned polyurethane sponge in 2mg mL-1The PVA of (2) is in the presence of water for more than 8 hours;
3) using a vacuum suction filtration pump to suction filter the nano material on the polyurethane sponge treated in the step 2);
4) and after the suction filtration is finished, putting the composite membrane into a vacuum drying oven, and drying for 8-12h at 40-50 ℃.
The invention has the following advantages: firstly, the base film used in the invention has low price, the preparation process of the film is simple, and the nano material crushed by ultrasonic is filtered and filtered on the base film soaked with PVA by a vacuum pumping and filtering pump, and is dried for 8-12h under vacuum at 40-50 ℃; the photothermal composite membrane prepared by the invention has better water permeability, can continuously transmit sewage from bottom to top for CNT to adsorb dye molecules, has self-floating property, still floats on the water surface while completely absorbing water, directly contacts with sunlight, and fully exerts the maximum photothermal performance of MXene; after PVA is soaked and placed in an oven for treatment until the PVA is completely dried, the PVA can be placed in water to keep better stability, and the nano material cannot cause secondary pollution to a water body due to falling off; the photo-thermal composite film prepared by the invention has better regeneration performance, can be repeatedly used and prolongs the service life.
Drawings
FIG. 1 shows the density at 350mW cm-2Under the light intensity of the three MXene-CNT photo-thermal composite films and the blank polyurethane sponge, the rhodamine B removal rate is 6 h. Rhodamine B concentration is 20mg L-1The volume of sewage is 50mL, CNT is 5mg, MXene mass is 5 mg.
FIG. 2 at 350mW cm-2The evaporation efficiency of the three MXene-CNT photo-thermal composite membranes and the blank polyurethane sponge on the dye wastewater and the recovery amount of the clean water (6h) under the light intensity. Rhodamine B concentration is 20mg L-1The volume of the sewage is 50mL, the mass of CNT is 5mg, and the mass of MXene is 5 mg.
FIG. 3 is a schematic diagram of the composite membrane after membrane 1, membrane 2 and membrane 3 are sonicated for 2h and the composite membrane is placed in ultrapure water. CNT mass 5mg, MXene mass 5mg, room temperature 25 ℃.
FIG. 4 shows the rhodamine B removal rate and the clean water regeneration efficiency after five times of regeneration of the membrane 1(a), the membrane 2(B) and the membrane 3 (c). The regeneration solution is 0.1M NaCl, the light intensity is 350mW cm-2Rhodamine B concentration ═ 20mg L-1The volume of the sewage is 50 mL.
Detailed Description
The invention is described below with reference to the figures and examples.
Example 1
The preparation method of the photothermal nano material MXene comprises the following steps:
1) weighing 10g of Ti3AlC2Powder is used for later use;
2) 40mL of hydrofluoric acid (40 wt%) was weighed using a measuring cylinder and poured into a beaker;
3) mixing Ti3AlC2Adding the beaker;
4) stirring for 24 hours at room temperature by using a magnetic stirrer, wherein the rotating speed is 200 rpm;
5) centrifuging the solution after reaction, and removing the upper layer liquid;
6) repeatedly performing ultrasonic treatment by using deoxygenated water, and centrifugally cleaning the precipitate until the pH value of the liquid is greater than 6;
7) the precipitate was dried under vacuum at room temperature until use.
Example 2
After the two materials are uniformly mixed, the MXene-CNT photo-thermal composite film is prepared by using a suction filtration method, and the specific preparation method comprises the following steps:
1) preparing a photo-thermal material MXene with the size of 1-5 microns, the titanium atom percentage of 42.57% and the oxygen atom percentage of 15.58% by etching with hydrofluoric acid, and commercially purchasing a Carbon Nano Tube (CNT) with the hydroxyl group mass percentage of 6.4% and the oxygen atom percentage of 3.4%, a polyvinyl alcohol adhesive (PVA) and a polyurethane sponge;
2) a circular polyurethane sponge having a diameter of 4cm was placed in a volume of 2mg mL-1Soaking the PVA in the solution for 8 hours for standby;
3) 5mg of CNT powder and 5mg of MXene powder were weighed out and mixed with ultrapure water in a ratio of 1 mg: 1mL, and then respectively carrying out ultrasonic treatment for 10min, wherein the ultrasonic power is 20 kHZ;
4) uniformly mixing the CNT turbid liquid and the MXene turbid liquid which are respectively and uniformly dispersed in the step 3) by ultrasonic, and uniformly distributing the uniformly mixed turbid liquid on a circular polyurethane sponge sheet which is fully soaked in PVA and has the diameter of 4cm by a suction filtration method;
5) the prepared MXene-CNT composite membrane (membrane 1) was dried in vacuum at 40 ℃ for 12 hours, and charged with 50mL of 20mg L-1In the rhodamine sewage, the concentration is 350mW cm-2The removal rate of the solution was 97.4% and the evaporation rate was 5.971kg · m after 6h of treatment under the light intensity of (1)-2h-1。
The MXene-CNT photo-thermal composite film is prepared by alternately performing suction filtration on the two materials according to different sequences, and the specific preparation method comprises the following steps:
1) preparing a photo-thermal material MXene with the size of 1-5 microns, the titanium atom percentage of 42.57% and the oxygen atom percentage of 15.58% by etching with hydrofluoric acid, and commercially purchasing a Carbon Nano Tube (CNT) with the hydroxyl group mass percentage of 6.4% and the oxygen atom percentage of 3.4%, a polyvinyl alcohol adhesive (PVA) and a polyurethane sponge;
2) a circular polyurethane sponge having a diameter of 4cm was placed in a volume of 2mg mL-1Soaking the PVA in the solution for 8 hours for standby;
3) 5mg of CNT powder and 5mg of MXene powder were weighed out and mixed with ultrapure water in a ratio of 1 mg: 1mL, and then respectively carrying out ultrasonic treatment for 10min, wherein the ultrasonic power is 20 kHZ;
4) uniformly distributing the CNT turbid liquid uniformly dispersed in the ultrasonic mode in the step 3) on a circular polyurethane sponge sheet which is fully soaked in PVA and has the diameter of 4cm by using a suction filtration method, and then repeating the suction filtration step on the MXene turbid liquid uniformly dispersed in the step 3) to prepare a film 2;
5) the prepared MXene-CNT composite membrane (membrane 2) was dried in vacuum at 40 ℃ for 12h, and charged with 50mL of 20mg L-1In the rhodamine sewage, the concentration is 350mW cm-2The removal rate of the solution was 92.27% and the evaporation rate was 4.910kg · m for 6h-2h-1。
Example 4
The MXene-CNT photo-thermal composite film is prepared by alternately performing suction filtration on the two materials according to different sequences, and the specific preparation method comprises the following steps:
1) preparing a photo-thermal material MXene with the size of 1-5 microns, the titanium atom percentage of 42.57% and the oxygen atom percentage of 15.58% by etching with hydrofluoric acid, and commercially purchasing a Carbon Nano Tube (CNT) with the hydroxyl group mass percentage of 6.4% and the oxygen atom percentage of 3.4%, a polyvinyl alcohol adhesive (PVA) and a polyurethane sponge;
2) a circular polyurethane sponge having a diameter of 4cm was placed in a volume of 2mg mL-1Soaking the PVA in the solution for 8 hours for standby;
3) 5mg of CNT powder and 5mg of MXene powder were weighed out and mixed with ultrapure water in a ratio of 1 mg: 1mL, and then respectively carrying out ultrasonic treatment for 10min, wherein the ultrasonic power is 20 kHZ;
4) uniformly distributing MXene suspension uniformly dispersed in the step 3) on a circular polyurethane sponge sheet fully soaked with PVA and having the diameter of 4cm by using a suction filtration method, and then repeating the suction filtration step on the CNT suspension uniformly dispersed in the step 3) to prepare a film 3;
5) the prepared MXene-CNT composite membrane (membrane 3) was vacuum dried at 40 ℃ for 12h, 50mL, 20mg L-1In the rhodamine sewage, the concentration is 350mW cm-2The removal rate of the solution is 96.91 percent and the evaporation rate is 5.839 kg.m after the solution is treated for 6 hours under the light intensity of (1)-2h-1。
Example 5
The composite membranes 1,2 and 3 are prepared according to the schemes in cases 1,2 and 3, the stability of the composite membranes is tested, the composite membranes are placed in ultrapure water to be subjected to ultrasonic treatment for 2 hours respectively, and the absorbance and the photos are recorded, so that the result shows that the absorbance of the ultrapure water is constant all the time, the prepared composite membranes hardly have the phenomenon of nanometer material shedding, and the composite membranes have good stability.
Example 6
The method for detecting the regeneration performance of the three membranes is as follows:
and (3) putting the membrane 1, the membrane 2 and the membrane 3 into a 0.1M NaCl solution, carrying out ultrasonic treatment for 30min, monitoring the rhodamine B removal efficiency and the clean water evaporation rate of the three regenerated membranes, and repeating five times to explore the regeneration performance of the membranes. The results show that after five times of regeneration, the removal efficiency of the membrane 1 on rhodamine B can still reach 96.91%, and the evaporation rate of clean water can reach 5.839kg m-2h-1(ii) a The removal efficiency of the membrane 2 on rhodamine B can still reach 90.37%, and the evaporation rate of clean water can reach 5.573 kg.m-2h-1(ii) a The removal efficiency of the membrane 3 on rhodamine B can still reach 91.51 percent, and the evaporation rate of the clean water can reach 5.042 kg.m-2h-1。
Claims (3)
1. The preparation method of the MXene-CNT photo-thermal composite membrane for self-floating removal of organic dye and realization of clean water regeneration is characterized by comprising the following steps:
1) weighing CNT powder and MXene powder at a mass ratio of 1:1, mixing with ultrapure water at a ratio of mg: mL to 1:1, and subjecting to 20-25kHz for 10-15minCarrying out ultrasonic treatment; MXene powder from per gram of Ti3AlC2Etching the powder for 24 hours by using 20-30mL of 40-50 wt% hydrofluoric acid solution, and carrying out centrifugal treatment to remove upper-layer liquid; repeatedly performing ultrasonic treatment with deoxygenated water, centrifuging, cleaning, precipitating, and drying until pH of the liquid is greater than 6;
2) uniformly mixing the CNT turbid liquid and the MXene turbid liquid which are respectively subjected to ultrasonic dispersion, and performing suction filtration treatment, or alternatively performing suction filtration treatment on the two kinds of ultrasonically dispersed turbid liquids according to different sequences; forming MXene-CNT photo-thermal composite films with three different structures;
3) drying in a vacuum drying oven at 40-50 deg.C for 8-12 hr; the mass of the nano material covered by each square meter of the composite film is 7-10 g.
2. The production method according to claim 1, characterized in that: placing the basement membrane into 2-5mg mL-1The PVA binder solution is soaked for more than 8 hours.
3. The production method according to claim 1, characterized in that: polyurethane sponge is used as a basement membrane.
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| CN113429595A (en) * | 2021-06-25 | 2021-09-24 | 哈尔滨工程大学 | Preparation method of nano-material modified carbon fiber epoxy resin composite material |
| CN117180980A (en) * | 2023-08-29 | 2023-12-08 | 华北电力大学（保定） | Composite nanofiltration membrane for efficiently intercepting ammonium sulfate and ammonium nitrate and simultaneously adsorbing and removing mercury ions and preparation method thereof |
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| CN113429595A (en) * | 2021-06-25 | 2021-09-24 | 哈尔滨工程大学 | Preparation method of nano-material modified carbon fiber epoxy resin composite material |
| CN117180980A (en) * | 2023-08-29 | 2023-12-08 | 华北电力大学（保定） | Composite nanofiltration membrane for efficiently intercepting ammonium sulfate and ammonium nitrate and simultaneously adsorbing and removing mercury ions and preparation method thereof |
| CN117180980B (en) * | 2023-08-29 | 2024-03-08 | 华北电力大学（保定） | Composite nanofiltration membrane for efficiently intercepting ammonium sulfate and ammonium nitrate and simultaneously adsorbing and removing mercury ions and preparation method thereof |
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