CN112808024B - 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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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 =1:1, and respectively carrying out 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 membrane soaked for more than 8 hours by using polyvinyl alcohol (PVA) by using a vacuum suction filtration pump according to different sequences to prepare a composite membrane; 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 the CNT powder and MXene powder with ultrapure water according to a ratio of mg: mL =1:1, and performing ultrasonic treatment for 10-15min under the condition of 20-25 kHZ; etching MXene powder for 24 hours by using 20-30mL of 40-50wt% hydrofluoric acid solution per gram of Ti3AlC2 powder, and centrifuging to remove upper liquid; repeatedly performing ultrasonic treatment with deoxygenated water, centrifuging, cleaning precipitate until pH of the liquid is greater than 6, and drying;
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 7-10g.
Further, the basement membrane was placed in 2-5mg mL before suction filtration -1 The 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 -1 The PVA of (2) is in the presence of water for more than 8 hours;
3) Using a vacuum suction 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 photo-thermal 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, can still float on the water surface while completely absorbing water, is directly contacted with sunlight, and fully exerts the maximum photo-thermal 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 -2 Under light intensity ofThe removal rate of three MXene-CNT photo-thermal composite films and blank polyurethane sponge to rhodamine B (6 h). Rhodamine B concentration =20mg L -1 Sewage volume 50ml, cnt =5mg, mxene mass =5mg.
FIG. 2 at 350mW cm -2 The 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 (6 h) under the light intensity. Rhodamine B concentration =20mg L -1 Sewage volume 50ml, cnt mass =5mg, mxene mass =5mg.
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. The mass of CNT was 5mg, the mass of MXene was 5mg, and the temperature was 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, and the light intensity is 350mW cm -2 Rhodamine B concentration =20mg L -1 The volume of the sewage is 50mL.
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 Ti 3 AlC 2 Powder 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 Ti 3 AlC 2 Adding the beaker;
4) Stirring for 24 hours at room temperature by using a magnetic stirrer, wherein the rotating speed is 200rpm;
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 -1 Soaking the PVA in the solution for 8 hours for standby;
3) 5mg of CNT powder and 5mg of MXene powder were weighed and mixed with ultrapure water in a ratio of 1mg:1mL, and then respectively carrying out ultrasonic treatment for 10min, wherein the ultrasonic power is 20kHZ;
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 vacuum-dried at 40 ℃ for 12 hours, and 50mL of 2mg L -1 In the rhodamine sewage, the concentration is 350mW cm -2 The removal rate of the solution is 97.4 percent, the evaporation rate is 5.971kg m after the solution is treated for 6 hours under the light intensity of (1) -2 h -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 -1 Soaking 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 1mg:1mL, and then respectively carrying out ultrasonic treatment for 10min, wherein the ultrasonic power is 20kHZ;
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 MXene-CNT composite membrane (membrane 2) thus prepared was vacuum-dried at 40 ℃ for 12 hours, and then charged into 50mL of a container (20 mg/L) -1 In the rhodamine wastewater, the concentration is 350mW cm -2 The removal rate is 92.27% and the evaporation rate is 4.910kg m after 6h of treatment under the optical power of (1) -2 h -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 mu m, the titanium atom percentage of 42.57% and the oxygen atom percentage of 15.58% by hydrofluoric acid etching, and commercially purchasing a Carbon Nano Tube (CNT), a polyvinyl alcohol adhesive (PVA) and a polyurethane sponge with the hydroxyl group mass percentage of 6.4% and the oxygen atom percentage of 3.4%;
2) A circular polyurethane sponge having a diameter of 4cm was placed in a volume of 2mg mL -1 Soaking 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 1mg:1mL, and then respectively carrying out ultrasonic treatment for 10min, wherein the ultrasonic power is 20kHZ;
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 MXene-CNT composite membrane (membrane 3) thus prepared was vacuum-dried at 40 ℃ for 12 hours, and then charged into 50mL of a container (20 mg/L) -1 In the rhodamine sewage, the concentration is 350mW cm -2 The removal rate is 96.91 percent and the evaporation rate is 5.839 kg.m after the treatment for 6 hours under the light intensity of (1) -2 h -1 。
Example 5
The composite films 1,2 and 3 are prepared according to the scheme of 1,2,3, the stability of the composite films is tested, the composite films are placed into ultrapure water to be subjected to ultrasonic treatment for 2 hours respectively, the absorbance and the photos are recorded, and the results show that the absorbance of the ultrapure water is constant all the time, the prepared composite films hardly have the phenomenon of nanometer material falling, and the composite films 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 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 the steps five times to explore the regeneration performance of the membranes. The result shows 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 5.839 kg-m -2 h -1 (ii) a The removal efficiency of the membrane 2 to rhodamine B can still reach 90.37 percent, and the evaporation rate of clean water can reach 5.573 kg.m -2 h -1 (ii) a The removal efficiency of the membrane 3 on rhodamine B can still reach 91.51 percent, and the evaporation rate of clean water can reach 5.042 kg.m -2 h -1 。
Claims (1)
1. Preparation method of MXene-CNT photo-thermal composite membrane for self-floating removal of organic dye and realization of clean water regeneration, and preparation method thereof
Is characterized in that:
1) Weighing CNT powder and MXene powder according to a mass ratio of 1:1, mixing the CNT powder and MXene powder with ultrapure water according to a ratio of mg: mL =1:1, and performing ultrasonic treatment for 10-15min under the condition of 20-25 kHZ; MXene powder from per gram of Ti 3 AlC 2 Etching the powder with 20-30mL of hydrofluoric acid solution with the concentration of 40-50wt% to 24h, carrying out centrifugal treatment, 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 to form an MXene-CNT photo-thermal composite film;
3) Placing in a vacuum drying oven, and drying at 40-50 deg.C for 8-12h; the mass of the nano material covered by each square meter of the composite film is 7-10 g;
polyurethane sponge is used as a basement membrane, and the basement membrane is placed in 2-5mg mL -1 The PVA binder solution (A) is soaked in the PVA binder solution (A) for more than 8 h.
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| CN113293655B (en) * | 2021-05-27 | 2022-08-02 | 电子科技大学 | Preparation method of MXene composite film with controllable thickness and novel structure |
| CN113429595B (en) * | 2021-06-25 | 2022-05-10 | 哈尔滨工程大学 | Preparation method of nano-material modified carbon fiber epoxy resin composite material |
| 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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