CN108636137B - Film composite material loaded with indium zinc sulfide and polyvinylidene fluoride and preparation method thereof - Google Patents
Film composite material loaded with indium zinc sulfide and polyvinylidene fluoride and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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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- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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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
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- B01D2311/00—Details relating to membrane separation process operations and control
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- B01D2311/2611—Irradiation
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- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/2649—Filtration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/2696—Catalytic reactions
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Abstract
The invention discloses a film composite material loaded with indium zinc sulfide and polyvinylidene fluoride and a preparation method thereof, wherein the preparation method comprises the following steps: step 1, preparing aqueous solutions of zinc chloride, indium chloride tetrahydrate and thioacetamide; step 2, dissolving polyvinylpyrrolidone and polyvinylidene fluoride in N, N-dimethylacetamide; and 3, respectively coating the precursor solution obtained in the step 1 and the casting solution obtained in the step 2 on the surfaces of two sides of the carbon felt, and completely reacting at the temperature of 80-160 ℃ to obtain the film composite material loaded with the indium zinc sulfide and the polyvinylidene fluoride. The membrane composite material can continuously carry out catalytic degradation and filtration on sewage; the indium zinc sulfide photocatalyst is loaded to one side of the carbon felt supporting layer, and the PVDF membrane is loaded to the other side of the carbon felt supporting layer, so that the separation of the photocatalysis and membrane separation processes in space is realized, and the two processes cannot influence each other.
Description
Technical Field
The invention belongs to the technical field of photocatalytic or photoelectrocatalytic membrane composite materials, and particularly relates to a membrane composite material loaded with indium zinc sulfide and polyvinylidene fluoride and a preparation method thereof.
Background
Indium zinc sulfide has great potential value in the fields of photocatalysis, charge storage, electrochemical recording, thermoelectric application and the like, and becomes a material of hot research in recent years. Indium zinc sulfide has a proper semiconductor band gap structure, has high photocatalytic activity under visible light, has various synthesis methods, is convenient to prepare, and is widely applied to photocatalytic degradation of refractory organic pollutants by photocatalytic degradation of hydrogen produced by photolysis, photocatalytic reduction of carbon dioxide, selective catalytic oxidation reaction and the like. However, the nano or micron powdered indium zinc sulfide photocatalyst has the problem of difficult separation in sewage treatment.
Polyvinylidene fluoride (PVDF) is one of the most widely used membrane separation materials at present, and has the advantages of strong antioxidant activity, excellent chemical resistance, strong thermal stability, large mechanical strength, good film forming performance, high wear resistance and easy processing. PVDF membranes are commonly used in processes such as ultrafiltration, microfiltration, etc. in water treatment. At present, the sewage treatment by coupling the PVDF membrane with the photocatalysis process mainly has two modes: (1) a supported photocatalytic membrane reactor; (2) suspension type photocatalytic membrane reactor. The supported photocatalytic film is divided into film surface loading and body modification, but the PVDF film surface is smooth, the catalyst is difficult to load on the surface of the PVDF film for a long time, the photocatalytic effect can be obviously reduced by doping the photocatalyst into the PVDF film, and the film structure of the organic PVDF film material can be damaged in the long-term photocatalytic reaction. For a suspended photocatalytic membrane reactor, a PVDF membrane is mainly used for intercepting and separating a catalyst, but catalyst particles can block membrane pores and further form a filter cake layer on the membrane surface, so that severe membrane pollution is generated, and the flux of the PVDF membrane is reduced.
Disclosure of Invention
The invention aims to provide a film composite material loaded with indium zinc sulfide and polyvinylidene fluoride and a preparation method thereof, so as to solve the technical problems. The membrane composite material can continuously carry out catalytic degradation and filtration on sewage; the indium zinc sulfide photocatalyst is loaded to one side of the carbon felt supporting layer, the PVDF membrane is loaded to the other side of the carbon felt supporting layer, the separation of the photocatalysis process and the membrane separation process in space can be realized, the two processes are coupled together, and the two processes cannot mutually influence each other.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a film composite material loaded with indium zinc sulfide and polyvinylidene fluoride comprises the following steps:
and 3, respectively coating the precursor solution obtained in the step 1 and the casting solution obtained in the step 2 on the surfaces of two sides of the carbon felt, and completely reacting at the temperature of 80-160 ℃ to obtain the film composite material loaded with the indium zinc sulfide and the polyvinylidene fluoride.
Further, the step 1 specifically comprises the steps of dissolving zinc chloride, indium chloride tetrahydrate and thioacetamide in deionized water, wherein the molar mass ratio of the zinc chloride to the indium chloride tetrahydrate to the thioacetamide is 1:2: 6; adjusting the pH of the prepared aqueous solution to 2-3.
Further, in the step 2, the mass ratio of the polyvinylpyrrolidone to the polyvinylidene fluoride is 1: 5.
Further, step 2 is specifically to dissolve polyvinylpyrrolidone and polyvinylidene fluoride in N, N-dimethylacetamide under continuous stirring at room temperature, and continue stirring until bubbles are removed.
Further, step 3 also includes pretreatment of the carbon felt, and the specific steps include:
(1) soaking the selected carbon felt in acetone for 30-60 minutes, and washing with deionized water;
(2) soaking the carbon felt treated in the step (1) in absolute ethyl alcohol for 30-60 minutes, and washing with deionized water again;
(3) and (3) drying the carbon felt treated in the step (2) for 4 hours at the temperature of 60 ℃.
Further, in step 3, the precursor solution is coated on the rougher surface of the carbon felt, and the casting solution is coated on the smoother surface of the carbon felt.
Further, step 3 specifically includes:
step 3.1, uniformly spraying the precursor solution on the front surface of the pretreated carbon felt, and reacting for 6-16 hours at the temperature of 80-160 ℃;
step 3.2, washing the surface of the carbon felt treated in the step 3.1 by deionized water, and then drying for 6 hours in vacuum at the temperature of 60 ℃;
3.3, fixing the carbon felt processed in the step 3.2 on a glass plate with the back face upward, and uniformly coating the casting solution on the back face of the carbon felt by using a film scraping knife;
step 3.4, placing the carbon felt treated in the step 3.3 in clear water to obtain a membrane composite material;
wherein, the front of the carbon felt is a rough surface, and the back of the carbon felt is a smooth surface.
A PVDF film coating, a carbon felt layer and an indium zinc sulfide adhesion layer; a carbon felt layer is used as a supporting and conducting layer, and an indium zinc sulfide adhesion layer and a PVDF film coating are respectively adhered to the surfaces of two sides of the carbon felt layer.
Further, indium zinc sulfide is attached to the surface of the rougher side of the carbon felt, and polyvinylidene fluoride is attached to the surface of the smoother side of the carbon felt.
The application of any one of the film composite materials loaded with indium zinc sulfide and polyvinylidene fluoride is applied to treatment of sewage and wastewater.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the composite material of the loaded indium zinc sulfide and the PVDF film uses the carbon felt as the supporting layer, so that the surfaces of two sides of the carbon felt are respectively attached with the indium zinc sulfide and the PVDF film, the separation of the photocatalysis process and the film separation process on the space is realized, the two processes cannot mutually influence, and the two processes are skillfully coupled together to carry out continuous photocatalysis or photoelectrocatalysis reaction. In addition, the carbon felt is used as a conductive layer, has stable structure, good adsorption capacity and good conductivity, and can be used as an electrode for photoelectrocatalysis.
The composite material of the loaded indium zinc sulfide and PVDF membrane can continuously catalyze, degrade and filter sewage, and can treat pollutants in water while ensuring the filtering rate; the photocatalytic degradation and the sewage filtration are carried out simultaneously, so that the integrated sewage treatment can be realized without intervals; indium zinc sulfide and polyvinylidene fluoride are respectively attached to two sides of the carbon felt template, so that the indium zinc sulfide can be prevented from blocking membrane holes, and the filtering rate can be ensured. The membrane composite material is applied to the treatment of sewage and wastewater, and can carry out continuous photocatalytic or photoelectrocatalysis treatment.
Drawings
The invention is described in further detail below with reference to the figures and specific examples.
FIG. 1 is a schematic cross-sectional structural view of a film composite of the present invention supporting indium zinc sulfide and polyvinylidene fluoride;
FIG. 2 is a scanning electron micrograph of the surface of the carbon mat of FIG. 1 on the side loaded with indium zinc sulfide;
FIG. 3 is a scanning electron micrograph of one side of the carbon felt-loaded PVDF film of FIG. 1;
in fig. 1, 1 is a PVDF film coating, 2 is a carbon felt layer, and 3 is an indium zinc sulfide adhesion layer.
Detailed Description
Referring to fig. 1 to 3, a method for preparing a film composite loaded with indium zinc sulfide and polyvinylidene fluoride (PVDF) according to the present invention includes the following steps:
(1) choose for use the carbon felt as membrane combined material's support and conducting layer, the carbon felt size with water treatment membrane subassembly size the same can to carry out the preliminary treatment to the carbon felt of choosing, in the preliminary treatment acetone with absolute ethyl alcohol's quantity can with the carbon felt submergence, specifically include:
firstly, soaking a carbon felt in acetone for 30-60 minutes, and washing the carbon felt for several times by using deionized water;
secondly, soaking the carbon felt in absolute ethyl alcohol for 30-60 minutes, and then washing the carbon felt for several times by using deionized water;
and thirdly, drying the washed carbon felt for 4 hours at the temperature of 60 ℃ to obtain a pretreated carbon felt template for later use.
(2) Preparing a casting solution:
at room temperature, 3g of polyvinylpyrrolidone (k.30) and 15g of polyvinylidene fluoride (PVDF) were dissolved in 100mL of N, N-Dimethylacetamide (DMAC) while continuously stirring, and continuously stirred overnight to remove air bubbles, to obtain a casting solution.
(3) Preparing a precursor solution:
0.1363g of zinc chloride, 0.5865g of indium chloride tetrahydrate and 0.4508g of thioacetamide are dissolved in 10-100 mL of deionized water, and the pH is adjusted to 2-3 by adding hydrochloric acid to obtain a precursor solution.
(4) Synthesis of membrane composite material:
and (3) uniformly spraying the precursor solution prepared in the step (3) on the front surface of the carbon felt pretreated in the step (1) by using a mechanical arm and an art spray pen, then filling the carbon felt into a non-heat-insulation sealed container, and reacting for 6-16 hours at the temperature of 80-160 ℃. And after the reaction is completed, taking out the carbon felt, washing the surface of the carbon felt by deionized water, and then drying the carbon felt for 6 hours in vacuum at the temperature of 60 ℃. And then fixing the carbon felt on a glass plate with the back surface facing upwards, uniformly coating the casting film liquid on the back surface of the carbon felt by using a film scraping knife, and finally placing the carbon felt in clear water to obtain the film composite material loaded with indium zinc sulfide and polyvinylidene fluoride (PVDF). Wherein, the front of the carbon felt is a rough surface, and the back of the carbon felt is a smooth surface.
In the step (4), the casting solution can be coated on the back surface of the carbon felt to obtain a PVDF film coating, and then the precursor solution is sprayed on the front surface of the carbon felt to carry out the catalyst synthesis loading process, so as to obtain the film composite material finally.
Referring to fig. 1, a film composite loaded with indium zinc sulfide and polyvinylidene fluoride prepared by the above preparation method adopts a carbon felt as a supporting and conducting layer, and the indium zinc sulfide and the polyvinylidene fluoride are respectively attached to the surfaces of two sides of the carbon felt; indium zinc sulfide is attached to the surface of the rougher side of the carbon felt, and polyvinylidene fluoride is attached to the surface of the smoother side of the carbon felt. Referring to fig. 2, it can be observed that a layer of indium zinc sulfide is attached to the surface of the carbon felt fiber, and even a surplus of lumps are attached. Referring to fig. 3, it can be observed that the PVDF membrane is attached to the surface of the carbon felt and has a large number of filtration pores.
The application of the prepared film composite material loaded with indium zinc sulfide and polyvinylidene fluoride is applied to treatment of sewage and wastewater.
Example one
A preparation method of a composite material loaded with indium zinc sulfide and a PVDF film comprises the following steps:
(1) selecting a 17cm × 19cm carbon felt as a composite material template for pretreatment:
step one, placing a carbon felt in 200mL of acetone, soaking for 30 minutes, and then washing with deionized water;
secondly, soaking the carbon felt in 200mL of absolute ethyl alcohol for 30 minutes, and then washing the carbon felt clean by using deionized water;
and thirdly, drying the washed carbon felt for 4 hours at the temperature of 60 ℃.
(2) Preparing a casting solution:
at room temperature, 3g polyvinylpyrrolidone (k.30) and 15g PVDF were dissolved in 100mL N, N-Dimethylacetamide (DMAC) with constant stirring and stirring was continued overnight to remove air bubbles.
(3) Preparing a precursor solution:
0.1363g of zinc chloride, 0.5865g of indium chloride tetrahydrate and 0.4508g of thioacetamide were dissolved in 10mL of deionized water to prepare a precursor solution, and hydrochloric acid was added to adjust the pH to 2.
(4) Synthesis of the composite material:
and uniformly spraying the precursor solution on the front surface of the pretreated carbon felt by using a robot mechanical arm and an art spray pen, putting the carbon felt into a non-heat-insulation sealed container, and reacting for 6 hours at the temperature of 80 ℃. After the reaction, the carbon felt was taken out, washed with deionized water on the surface, and vacuum-dried at 60 ℃ for 6 hours. And then fixing the carbon felt on a glass plate with the back surface facing upwards, uniformly coating the casting solution on the back surface of the carbon felt by using a film scraping knife, and finally placing the carbon felt in clear water to obtain the PVDF film coating based on the carbon felt.
Example two
A preparation method of a composite material loaded with indium zinc sulfide and a PVDF film comprises the following steps:
(1) selecting a 17cm × 19cm carbon felt as a composite material template for pretreatment:
step one, placing a carbon felt in 200mL of acetone, soaking for 60 minutes, and then washing with deionized water;
secondly, soaking the carbon felt in 200mL of absolute ethyl alcohol for 60 minutes, and then washing the carbon felt clean by using deionized water;
and thirdly, drying the washed carbon felt for 4 hours at the temperature of 60 ℃.
(2) Preparing a casting solution:
at room temperature, 3g polyvinylpyrrolidone (k.30) and 15g PVDF were dissolved in 100mL N, N-Dimethylacetamide (DMAC) with constant stirring and stirring was continued overnight to remove air bubbles.
(3) Preparing a precursor solution:
0.1363g of zinc chloride, 0.5865g of indium chloride tetrahydrate and 0.4508g of thioacetamide were dissolved in 20mL of deionized water to prepare a precursor solution, and hydrochloric acid was added to adjust the pH to 2.5.
(4) Synthesis of the composite material:
and fixing the carbon felt on a glass plate with the back surface facing upwards, uniformly coating the casting solution on the back surface of the carbon felt by using a film scraping knife, and then putting the carbon felt in clear water to obtain the PVDF film coating based on the carbon felt. And then, uniformly spraying the precursor solution on the front surface of the pretreated carbon felt by using a robot mechanical arm and an art spray pen, putting the carbon felt into a non-heat-insulation sealed container, and reacting for 10 hours at the temperature of 100 ℃. After the reaction, the carbon felt was taken out, washed with deionized water on the surface, and vacuum-dried at 60 ℃ for 6 hours.
EXAMPLE III
A preparation method of a composite material loaded with indium zinc sulfide and a PVDF film comprises the following steps:
(1) selecting a 17cm × 19cm carbon felt as a composite material template for pretreatment:
step one, placing a carbon felt in 200mL of acetone, soaking for 45 minutes, and then washing with deionized water;
secondly, soaking the carbon felt in 200mL of absolute ethyl alcohol for 45 minutes, and then washing the carbon felt clean by using deionized water;
and thirdly, drying the washed carbon felt for 4 hours at the temperature of 60 ℃.
(2) Preparing a casting solution:
at room temperature, 3g polyvinylpyrrolidone (k.30) and 15g PVDF were dissolved in 100mL N, N-Dimethylacetamide (DMAC) with constant stirring and stirring was continued overnight to remove air bubbles.
(3) Preparing a precursor solution:
0.1363g of zinc chloride, 0.5865g of indium chloride tetrahydrate and 0.4508g of thioacetamide were dissolved in 50mL of deionized water to prepare a precursor solution, and hydrochloric acid was added to adjust the pH to 2.5.
(4) Synthesis of the composite material:
and uniformly spraying the precursor solution on the front surface of the pretreated carbon felt by using a robot mechanical arm and an art spray pen, putting the carbon felt into a non-heat-insulation sealed container, and reacting for 16 hours at 120 ℃. After the reaction, the carbon felt was taken out, washed with deionized water on the surface, and vacuum-dried at 60 ℃ for 6 hours. And then fixing the carbon felt on a glass plate with the back surface facing upwards, uniformly coating the casting solution on the back surface of the carbon felt by using a film scraping knife, and finally placing the carbon felt in clear water to obtain the PVDF film coating based on the carbon felt.
Example four
A preparation method of a composite material loaded with indium zinc sulfide and a PVDF film comprises the following steps:
(1) selecting a 17cm × 19cm carbon felt as a composite material template for pretreatment:
step one, placing a carbon felt in 200mL of acetone, soaking for 30 minutes, and then washing with deionized water;
secondly, soaking the carbon felt in 200mL of absolute ethyl alcohol for 30 minutes, and then washing the carbon felt clean by using deionized water;
and thirdly, drying the washed carbon felt for 4 hours at the temperature of 60 ℃.
(2) Preparing a casting solution:
at room temperature, 3g polyvinylpyrrolidone (k.30) and 15g PVDF were dissolved in 100mL N, N-Dimethylacetamide (DMAC) with constant stirring and stirring was continued overnight to remove air bubbles.
(3) Preparing a precursor solution:
0.1363g of zinc chloride, 0.5865g of indium chloride tetrahydrate and 0.4508g of thioacetamide were dissolved in 100mL of deionized water to prepare a precursor solution, and the pH value was adjusted to 3.
(4) Synthesis of the composite material:
and fixing the carbon felt on a glass plate with the back surface facing upwards, uniformly coating the casting solution on the back surface of the carbon felt by using a film scraping knife, and then putting the carbon felt in clear water to obtain the PVDF film coating based on the carbon felt. And then, uniformly spraying the precursor solution on the front surface of the pretreated carbon felt by using a robot mechanical arm and an art spray pen, putting the carbon felt into a non-heat-insulation sealed container, and reacting for 10 hours at 160 ℃. After the reaction, the carbon felt was taken out, washed with deionized water on the surface, and vacuum-dried at 60 ℃ for 6 hours.
Claims (9)
1. A preparation method of a film composite material loaded with indium zinc sulfide and polyvinylidene fluoride is characterized by comprising the following steps:
step 1, preparing aqueous solutions of zinc chloride, indium chloride tetrahydrate and thioacetamide to obtain a precursor solution;
step 2, dissolving polyvinylpyrrolidone and polyvinylidene fluoride in N, N-dimethylacetamide to obtain a membrane casting solution;
step 3, respectively coating the precursor solution obtained in the step 1 and the casting solution obtained in the step 2 on the surfaces of two sides of a carbon felt, and completely reacting at the temperature of 80-160 ℃ to obtain the film composite material loaded with indium zinc sulfide and polyvinylidene fluoride;
the step 3 specifically comprises the following steps:
step 3.1, uniformly spraying the precursor solution on the front surface of the pretreated carbon felt, and reacting for 6-16 hours at the temperature of 80-160 ℃;
step 3.2, washing the surface of the carbon felt treated in the step 3.1 by deionized water, and then drying for 6 hours in vacuum at the temperature of 60 ℃;
3.3, fixing the carbon felt processed in the step 3.2 on a glass plate with the back face upward, and uniformly coating the casting solution on the back face of the carbon felt by using a film scraping knife;
step 3.4, placing the carbon felt treated in the step 3.3 in clear water to obtain a membrane composite material;
wherein, the front of the carbon felt is a rough surface, and the back of the carbon felt is a smooth surface.
2. The preparation method according to claim 1, wherein the step 1 specifically comprises dissolving zinc chloride, indium chloride tetrahydrate and thioacetamide in deionized water, wherein the molar mass ratio of the zinc chloride, the indium chloride tetrahydrate and the thioacetamide is 1:2: 6; adjusting the pH value of the prepared aqueous solution to 2-3.
3. The method according to claim 1, wherein in the step 2, the mass ratio of the polyvinylpyrrolidone to the polyvinylidene fluoride is 1: 5.
4. The method according to claim 1, wherein the step 2 is to dissolve polyvinylpyrrolidone and polyvinylidene fluoride in N, N-dimethylacetamide under continuous stirring at room temperature, and to continue stirring until bubbles are removed.
5. The preparation method of claim 1, wherein the step 3 further comprises pretreatment of the carbon felt, and the specific steps comprise:
(1) soaking the selected carbon felt in acetone for 30-60 minutes, and washing with deionized water;
(2) soaking the carbon felt treated in the step (1) in absolute ethyl alcohol for 30-60 minutes, and washing with deionized water again;
(3) and (3) drying the carbon felt treated in the step (2) for 4 hours at the temperature of 60 ℃.
6. The method according to claim 1, wherein in step 3, the precursor solution is coated on a relatively rough surface of the carbon felt, and the casting solution is coated on a relatively smooth surface of the carbon felt.
7. A film composite supporting indium zinc sulfide and polyvinylidene fluoride prepared by the preparation method according to any one of claims 1 to 6, comprising: a PVDF film coating (1), a carbon felt layer (2) and an indium zinc sulfide adhesion layer (3); the carbon felt layer (2) is used as a supporting and conducting layer, and the indium zinc sulfide adhesion layer (3) and the PVDF film coating (1) are respectively adhered to the surfaces of two sides of the carbon felt layer (2).
8. The indium zinc sulfide and polyvinylidene fluoride-loaded film composite of claim 7, wherein the indium zinc sulfide is attached to the rougher side surface of the carbon felt and the polyvinylidene fluoride is attached to the smoother side surface of the carbon felt.
9. Use of the indium zinc sulfide and polyvinylidene fluoride-loaded membrane composite of claim 7 or 8 in the treatment of wastewater.
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| CN110354904A (en) * | 2019-07-24 | 2019-10-22 | 西安建筑科技大学 | A kind of Polyglycolic acid fibre-indium sulfide zinc compound film electrode and preparation method thereof |
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