CN113426430B - Intelligent oil-water separation material and preparation method and application thereof - Google Patents
Intelligent oil-water separation material and preparation method and application thereof Download PDFInfo
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- CN113426430B CN113426430B CN202110869122.4A CN202110869122A CN113426430B CN 113426430 B CN113426430 B CN 113426430B CN 202110869122 A CN202110869122 A CN 202110869122A CN 113426430 B CN113426430 B CN 113426430B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000000926 separation method Methods 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003513 alkali Substances 0.000 claims abstract description 22
- 238000001179 sorption measurement Methods 0.000 claims abstract description 20
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000011065 in-situ storage Methods 0.000 claims abstract description 11
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 8
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 7
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- 238000002474 experimental method Methods 0.000 description 12
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- 229940043267 rhodamine b Drugs 0.000 description 7
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- XMEVHPAGJVLHIG-FMZCEJRJSA-N chembl454950 Chemical compound [Cl-].C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H]([NH+](C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O XMEVHPAGJVLHIG-FMZCEJRJSA-N 0.000 description 5
- 239000000356 contaminant Substances 0.000 description 5
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 5
- 229960004989 tetracycline hydrochloride Drugs 0.000 description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 4
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
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- RCTGMCJBQGBLKT-PAMTUDGESA-N scarlet red Chemical compound CC1=CC=CC=C1\N=N\C(C=C1C)=CC=C1\N=N\C1=C(O)C=CC2=CC=CC=C12 RCTGMCJBQGBLKT-PAMTUDGESA-N 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
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- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28042—Shaped bodies; Monolithic structures
- B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses an intelligent oil-water separation material, and a preparation method and application thereof. The intelligent oil-water separation material is prepared by growing BiOBr crystals in situ on melamine sponge MS by using a stirring mode, further modifying perfluoro caprylic acid, and taking 3-aminopropyl trimethoxy silane as an adhesive. The preparation method is simple, complex equipment and excessive energy consumption are not needed, and the synthesized material has super-hydrophobic-super-lipophilic property, pH responsiveness and excellent mechanical stability, has strong adsorption capacity on various oils and organic solvents, and has high oil-water separation efficiency. The material treated by alkali can be converted into super-hydrophilic-underwater super-oleophobic material, and can efficiently photo-catalytically degrade various water-soluble pollutants.
Description
Technical Field
The invention relates to an intelligent oil-water separation material prepared by an in-situ synthesis method and a multifunctional application thereof, in particular to a general method for preparing the intelligent oil-water separation material by in-situ growing crystals and a substrate material on a sponge and carrying out surface modification, and belongs to the technical field of materials.
Background
The frequent occurrence of petroleum leakage accidents and the increase of industrial wastewater containing organic pollutants cause serious water pollution, and cause great threat to sustainable development of human beings. Therefore, it is of profound interest to develop an efficient and environmentally friendly process for the treatment and recovery of oil contaminants. Many traditional oil-water separation methods, such as a chemical method, an in-situ combustion method, a biological repair method, a membrane separation method and the like, still have the problems of complicated treatment, low efficiency, high cost, secondary pollution and the like. In addition, the industrial wastewater contains complex components, various oils and fats, and water-soluble dyes. Therefore, it is necessary and important in industrial applications to design a multifunctional material that can simultaneously remove various contaminants in water.
Compared with the traditional oil-water separation material, the super-wettability material has the advantages of energy conservation, simple operation, high separation efficiency, wide application range and the like, and is widely applied in the oil-water separation field in recent years. The super-hydrophobic-super-oleophylic material and the super-hydrophilic-underwater super-oleophylic material belong to super-wettability materials, can be used for coping with different types of oil-water pollutants, belong to oil removal materials, can completely repel water and allow oil phases to freely permeate, and therefore efficient oil-water separation is achieved. The super-hydrophilic-underwater super-oleophobic material belongs to a water removal material, can be fully infiltrated by water, further repels an oil phase, and realizes efficient oil-water separation. However, most "water removal" materials are not capable of removing a significant amount of water-soluble contaminants from wastewater and do not meet practical water purification requirements. Photocatalytic technology degrades pollutants by inducing redox reactions is an effective way to solve the water pollution problem.
"Smart" oil-water separation materials are capable of switching between hydrophobic and hydrophilic in response to an external stimulus (e.g., temperature, pH, electric field, light, etc.), and have attracted great attention. These responsive materials are more suitable for the construction of highly controllable simplified separation devices which are suitable for handling complex situations while reducing energy consumption, and pH responsive materials have been most widely studied due to their rapid response compared to other stimuli responsive oil-water separation materials. Therefore, it would be highly desirable to develop a multifunctional oil-water separation material with switchable surface wettability.
Disclosure of Invention
The invention aims to provide a preparation method of an intelligent oil-water separation material, which has the advantages of simple synthesis process, wide application range, good stability and strong durability. The intelligent oil-water separation material has switchable super-wettability, extremely high oil absorption performance, extremely strong oil-water separation capability, ultra-strong mechanical stability, photocatalytic pollutant degradation performance and relatively good recycling capability.
The technical scheme adopted by the invention is as follows: the intelligent oil-water separation material is prepared by growing BiOBr crystals in situ on Melamine Sponge (MS) in a stirring manner, further modifying perfluorooctanoic acid (PFOA), and taking 3-aminopropyl trimethoxy silane (KH-540) as an adhesive.
The preparation method of the intelligent oil-water separation material comprises the following steps:
1) Adding bismuth nitrate pentahydrate into a mixed solution of deionized water and glycerol, carrying out ultrasonic treatment for 10min, and stirring at room temperature until the solution is clear and transparent to obtain a solution A; dissolving potassium bromide in deionized water, and stirring until the potassium bromide is completely dissolved to obtain a solution B;
2) Immersing melamine sponge MS in the solution B to enable the sponge to fully absorb the solution B, then dropwise adding the rest of the solution B into the solution A, transferring the sponge adsorbed with the solution B into the solution A, stirring for 1h, and aging for 3h at room temperature; after the reaction is finished, taking out the sponge, washing with water and ethanol, and drying to obtain a BiOBr crystal grown in situ on the melamine sponge MS to synthesize a BiOBr@MS;
3) And dissolving perfluorooctanoic acid (PFOA) and 3-aminopropyl trimethoxysilane (KH-540) in absolute ethyl alcohol, activating under stirring to obtain a modification solution, soaking BiOBr@MS in the modification solution, taking out, and drying to obtain a target product S-BiOBr@MS.
Further, in the above preparation method, in step 1), the volume ratio of the deionized water to the glycerol=1:2 is the mixed solution of deionized water and glycerol.
Further, in the above preparation method, in the step 1), the bismuth nitrate concentration in the solution A is 33.3 mmol.L -1 。
Further, in the above preparation method, in the step 1), the concentration of potassium bromide in the solution B is 33.3 mmol.L -1 。
Further, in the above preparation method, in step 1), bismuth nitrate and potassium bromide=1:1 in molar ratio.
Further, in the above preparation method, in step 3), the activation is that the activation is performed at 60 ℃ for 1 hour.
Further, in the above-mentioned production method, in the step 3), the concentration of perfluorooctanoic acid in the modification liquid is 0.08 mol.L -1 The concentration of 3-aminopropyl trimethoxysilane was 0.042 mol.L -1 。
Further, in the preparation method and the step 3), the soaking is performed at 60 ℃ for 4 hours.
The application of the intelligent oil-water separation material in adsorbing oil provided by the invention comprises the following steps: and (3) adding an intelligent oil-water separation material into the oil-water mixture for adsorption.
The application of the intelligent oil-water separation material in oil-water separation provided by the invention comprises the following steps: filtering the oil-water mixture by an intelligent oil-water separation material or an intelligent oil-water separation material treated by alkali, and carrying out gravity separation and pump separation.
The invention provides an application of an intelligent oil-water separation material in photocatalytic degradation of organic pollutants in wastewater.
Further, the method comprises the following steps: and adding an intelligent oil-water separation material or an intelligent oil-water separation material treated by alkali into the wastewater containing the organic pollutants to perform photocatalytic degradation.
Further, the organic contaminants are rhodamine B, methylene blue, and tetracycline hydrochloride.
The beneficial effects of the invention are as follows:
1. according to the invention, melamine sponge is used as a substrate material, biOBr crystals are grown in situ on the sponge, so that the surface roughness of the substrate material is improved, the photocatalytic degradation capability is introduced, the overall surface energy of the material is reduced after perfluoro caprylic acid modification, and 3-aminopropyl trimethoxy silane is used as a stable adhesive, so that the mechanical stability of the material is enhanced, and a multifunctional intelligent oil-water separation material is constructed, and the multifunctional intelligent oil-water separation material can be widely used for collecting floating oil, oil-water separation, photocatalytic degradation pollutants and other industries.
2. The preparation method provided by the invention is simple, low in production cost, free from complex equipment and harsh experimental conditions, high in adsorption efficiency of the synthesized material on oils and organic solvents, and capable of solving the problems of crude oil leakage, oil spill collection and the like under the low-cost condition.
3. The intelligent oil-water separation material prepared by the invention has super-hydrophobic and super-oleophilic properties, the wettability of the material after alkali treatment can be switched, the material has super-hydrophilic and underwater super-oleophobic properties, both materials can be used for oil-water separation, and the separation efficiency is extremely high.
4. The intelligent oil-water separation material prepared by the invention has excellent mechanical stability and strong recycling capability, and can be applied to various extreme conditions.
5. After alkali treatment, the intelligent oil-water separation material prepared by the invention can be used for photocatalytic degradation of various water-soluble pollutants, and has higher degradation efficiency.
Drawings
FIG. 1 is a scanning electron micrograph of MS, biOBr@MS and S-BiOBr@MS; wherein, (a 1-a 3) are original MS sponge SEM images; (b 1-b 3) are BiOBr@MS material SEM images; (c 1-c 3) are SEM pictures of S-BiOBr@MS material.
FIG. 2 is a graph of the wettability of a sponge with varying degrees of modification; wherein (a) is MS; (b) is BiOBr@MS; (c) is MS modified with perfluorooctanoic acid; (d) Is S-BiOBr@MS (embedded as specific contact angle values); (e) is a photograph of the S-BiOBr@MS material immersed under water.
FIG. 3 is a photograph of various droplets on an S-BiOBr@MS; wherein, (a) is a photograph of a water droplet on an S-BiOBr@MS; (b) is a photograph of a plurality of liquid droplets on an S-BiOBr@MS; (c) Is a photograph of a water droplet at ph=13 and ph=7 on S-biobr@ms; (d) Is a photograph of an alkali treated S-BiOBr@MS oil droplet under water.
FIG. 4 is a photograph of S-BiOBr@MS selective adsorption of oils of different densities in an oil-water mixture; wherein (a-c) is a selective adsorption process of the material to the light oil; (d-f) is a selective adsorption process of heavy oil by the material.
FIG. 5 is a graph of saturated adsorption capacity and adsorption-desorption cycles of S-BiOBr@MS material for different oils and organic solvents; wherein (a) is a histogram of saturated adsorption capacities of the material for different oils and organic solvents; (b) Is a graph of adsorption-desorption cycle of materials on different oils and organic solvents.
FIG. 6 is a diagram of a specific application device for oil-water separation of S-BiOBr@MS material; wherein, (a 1-a 2) is S-BiOBr@MS material used for gravity separation (heavy oil/water) of oil-water mixture; (b) Is S-BiOBr@MS material used for pump separation (light oil/water) of oil-water mixture; (c 1-c 2) is an alkali treated S-BiOBr@MS material for gravity separation (light oil/water) of an oil-water mixture; (d) Is an alkali treated S-BiOBr@MS material used for pump separation (heavy oil/water) of oil-water mixtures.
FIG. 7 is a graph of the mechanical stability test of the S-BiOBr@MS material; wherein, (a) mechanical wear test; (b) a stretching experiment; (c) a torsion experiment; (d) a compression experiment; (e) Water impact test.
FIG. 8 is a graph of photocatalytic degradation of three contaminants by alkali treated S-BiOCl@MS; wherein, (a 1) and (a 2) are photos of equipment before and after the photocatalytic degradation of rhodamine B; (a 3) is the photodegradation curve of the material for rhodamine B; (b1) (b 2) is a photograph of the equipment before and after photocatalytic degradation of methylene blue; (b 3) is the photodegradation curve of the material for methylene blue; (c1) (c 2) is a photograph of equipment before and after photocatalytic degradation of tetracycline hydrochloride; (c 3) is a photodegradation graph of the material against tetracycline hydrochloride.
FIG. 9 is a schematic illustration of the preparation of S-BiOBr@MS material by in situ synthesis and its multifunctional applications.
Detailed Description
Example 1 Intelligent oil-Water separation Material S-BiOBr@MS
The preparation method comprises the following steps:
1) 0.0485g of bismuth nitrate pentahydrate is weighed and added into a mixed solution of 10mL of deionized water and 20mL of glycerol, the solution is subjected to ultrasonic treatment for 10min, and the solution is further stirred at room temperature until the solution is clear and transparent, so as to obtain solution A.
0.0119g of potassium bromide is weighed and dissolved in 30mL of deionized water, and stirred until the potassium bromide is completely dissolved, so as to obtain a solution B.
2) A melamine sponge MS of 1cm by 1cm was immersed in the solution B, allowing the sponge to fully absorb the solution B.
Then, the remaining solution B was added dropwise to the solution A with a dropper while stirring, while transferring the saturated MS having adsorbed the solution B to the solution A, stirring for 1 hour, and then aging for 3 hours at room temperature. After the reaction is finished, the sponge is taken out, washed once by water and washed once by ethanol, and then the sponge is dried for 12 hours at 60 ℃ to realize the in-situ growth of BiOBr on MS, so that BiOBr@MS is synthesized.
3) 1g of perfluorooctanoic acid and 225 mu L of 3-aminopropyl trimethoxysilane were dissolved in 30mL of ethanol and activated at 60℃for 1 hour to obtain a modified solution. A piece of BiOBr@MS was immersed in the modification solution at 60℃for 4h. And taking out the sponge after the reaction is finished, and drying at 60 ℃ overnight to prepare the S-BiOBr@MS with the surface wettability of superhydrophobic-superoleophilic.
(II) detection
1. Microscopic morphologies of MS, biOBr@MS and S-BiOBr@MS were observed using a Scanning Electron Microscope (SEM).
As shown in FIG. 1, (a 1-a 3), (b 1-b 3) and (c 1-c 3) are respectively the microcosmic morphology of MS, biOBr@MS and S-BiOBr@MS material structures, and the original framework structure of the MS is maintained by observing two-step modification by a low-power SEM (scale of 500 μm), so that the mild reaction condition is proved to not damage the pore structure of the MS. In FIG. 1, (a 2) and (a 3) are the local morphologies of MS (scale bars of 50 μm and 10 μm, respectively), and it was found that the unmodified MS skeleton had a smooth surface. As shown in (b 2) and (b 3) of FIG. 1, the MS skeleton forms a layer of uniform protrusions, so that the surface is obviously roughened. In fig. 1, (c 2) and (c 3) clearly show that the surface protrusions of the sponge skeleton modified by PFOA and KH-540 are more obvious, and the distribution is still uniform.
2. The wettability of the intelligent oil-water separation material is observed and characterized by utilizing the penetration condition of liquid drops and the contact angle, the contact angle is measured by using a KRUSS optical contact angle measuring instrument DSA100, and the surface wettability is characterized.
As shown in fig. 2, (a) to (d) are sponge wettability comparisons of different modification degrees (water drops are dyed with methylene blue, ph=7), and e is a photograph of S-biobr@ms material immersed in water. The MS itself is hydrophilic, and water drops instantaneously penetrate into the sponge after contacting the surface of the MS (a in fig. 2). After in-situ growth of BiOBr on sponge, biOBr@MS still shows extremely strong hydrophilicity, because the BiOBr crystal surface has a large number of hydroxyl groups, hydrogen bonds are easily formed with water molecules, and water drops are instantaneously flattened after contacting the surface (b in FIG. 2). When MS is directly modified by PFOA, the surface energy of the material is reduced, the material has certain hydrophobicity, the water drop is hemispherical, and the contact angle is 137 degrees (c in figure 2). The wettability of the S-BiOBr@MS material is shown as d in fig. 2, and a water drop is spherical but not diffuse on the surface of the material, has a contact angle of 157 degrees and is superhydrophobic. When the S-BiOBr@MS material is completely immersed in water, a layer of air film can be generated at the interface of the sponge and water due to the superhydrophobicity of the material, and the air film covers the whole material, so that the water phase cannot enter the interior of the material (e in fig. 2).
As shown in fig. 3 a, the water droplets with ph=7 stand on the surface of the S-bio bor@ms material in a complete sphere shape. As shown in fig. 3 b, the various droplets (milk, nectar, water, coffee, green tea) also do not penetrate into the S-bio bor@ms material, maintaining a complete sphere. As shown in fig. 3 c, the water droplets at ph=13 gradually penetrate into the S-biobr@ms material, while the water droplets at ph=7 remain repelled. In fig. 3 d shows that the alkali treated S-bio bor@ms material is immersed in water and the oil droplets are repelled outside the material, the underwater oil contact angle can reach 151 °. These results show that the prepared S-BiOBr@MS material has pH response capability and can be intelligently switched from super-hydrophobic-super-oleophilic to super-hydrophilic-underwater super-oleophobic wettability.
3. The performance of the oil absorbing material can be evaluated by using the adsorption amount, which can be measured by the following procedure. S-BiOBr@MS samples were weighed, then placed into different types of oils and organic solvents for adsorption testing, then the samples were removed, the surface oils and organic solvents were wiped off with filter paper, and then the oil absorbing samples were weighed again. The adsorption capacity (Q) is calculated by the following equation:
Q＝(m t -m 0 )/m 0 wherein m is 0 And m t The weights of the samples before and after adsorption, respectively.
Example 2 application of Intelligent oil-water separation material S-BiOBr@MS in separation of oil-water mixture
1. In order to examine the practical application of the intelligent oil-water separation material for collecting spilled oil, the condition that oil is separated from an oil-water mixture under natural conditions is simulated. The selective adsorption experiments were performed using n-hexane (light oil, sudan III staining) and chloroform (heavy oil, sudan iv staining), respectively, mixed with water, and the results are shown in fig. 4.
As shown in fig. 4 (a) - (c), n-hexane has a relatively low density, and above the aqueous phase, n-hexane is rapidly absorbed into the sponge when the material is in contact therewith, thereby effecting a static separation of n-hexane from water.
In contrast, as shown in fig. 4 (d) to (f), chloroform is sunk below the water phase due to its high density, and when the material is in contact with chloroform, the chloroform is rapidly sucked into the interior by the material, thereby realizing static separation of the chloroform from the water. The oil absorbed in the material is collected in a simple extrusion mode, so that the separation of the oil and the water is realized, and no red pollutant is observed in the water, which indicates that the material has strong oil absorption capacity, high separation efficiency and no secondary pollution.
2. The saturated adsorption capacities of the S-BiOBr@MS material for two oils (soybean oil, engine oil) and organic solvents (dichloromethane, nitrobenzene, chloroform, toluene, meta-xylene, n-hexane) were examined. The results are shown in FIG. 5. As can be seen from FIG. 5 a, the saturated adsorption capacity of the S-BiOBr@MS material for different oils and organic solvents is up to 14.98-37.10 times of the self-mass, and the S-BiOBr@MS material has higher adsorption capacity.
3. The number of times of recycling of the S-BiOBr@MS material was examined. After saturated adsorption of different kinds of oils or organic solvents by the material, lightly extruding the material, discharging a large amount of adsorbed oils or organic solvents, then washing and drying the material by absolute ethyl alcohol to realize controllable desorption, and then carrying out an adsorption experiment again to carry out a recycling test. As a result, as shown in FIG. 5 b, the saturated adsorption amount was maintained substantially stable as the number of cycles was increased, and the recovered material was reused for 18 cycles in adsorption-desorption, and the separation efficiency was slightly lowered but still greater than 97%.
4. The continuous oil-water separation capability of the S-BiOBr@MS material is examined. The separation process is shown in fig. 6, in which the S-bio-ir ms material is inserted into a funnel in fig. 6 a1 to a2, the heavy oil/water (chloroform/water) mixture is poured into the funnel, the organic phase flows down due to the super-hydrophobic-super-lipophilic nature of the S-bio-ir ms material, and the aqueous phase is trapped in the funnel. In fig. 6 b, one end of the peristaltic pump tube was plugged into the S-biobr@ms material and this end was placed in a light oil/water (n-hexane/water) mixture, and the organic phase was gradually transferred all the way into the beaker at the other end of the tube under peristaltic pump drive. In fig. 6 c 1-c 2 the alkali treated S-bio-b@ms material (S-bio-b@ms was immersed in an aqueous sodium hydroxide solution at ph=13 for 4h at room temperature) was plugged into the funnel, the light oil/water mixture was poured into the funnel, the aqueous phase flowed down due to the super-hydrophilic-underwater super-oleophobic of the alkali treated S-bio-b@ms material, and the organic phase was trapped in the funnel. In fig. 6 d, one end of the peristaltic pump tube was plugged into the alkali treated S-bio-ir ms material and this end was placed in the heavy oil/water mixture, and the aqueous phase was gradually transferred all the way to the beaker at the other end of the tube under peristaltic pump drive. After the separation, the aqueous phase and the organic phase have no residue on each other.
Example 3 investigation of mechanical stability of Intelligent oil-Water separation Material S-BiOBr@MS
1. The mechanical stability of the S-BiOBr@MS material was examined. As shown in fig. 7 a, a wear experiment was performed on S-bio ir ms material; as shown in fig. 7 b, a tensile experiment was performed on S-bio ir ms material; as shown in fig. 7 c, a torsion experiment was performed on the S-bio ir ms material; as shown in fig. 7 d, a pressing experiment was performed on S-bio ir ms material; as shown in FIG. 7 e, a water impact experiment was performed on the S-BiOBr@MS material. Each experiment is repeated for a plurality of times, the contact angle of the S-BiOBr@MS material can still be kept above 150 degrees, and the oil-water separation efficiency can still be kept above 90 percent.
Example 4 application of Intelligent oil-water separation material S-BiOBr@MS in catalytic degradation of water-soluble pollutants
1. The photocatalytic degradation capability of the S-BiOBr@MS material on water-soluble pollutants is examined.
And (3) placing the S-BiOBr@MS in a sodium hydroxide aqueous solution with pH=13, soaking for 4 hours at room temperature, and drying to obtain the alkali-treated S-BiOBr@MS material. The S-BiOBr@MS material subjected to alkali treatment has super-hydrophilic and super-oleophobic properties. The results are shown in FIG. 8, wherein a1, b1 and c1 in FIG. 8 are the devices for the photocatalytic degradation experiment, and a2, b2 and c2 in FIG. 8 are the color changes of the solution after the reaction.
As a1 to a2 in FIG. 8, a block of 1X 1cm is taken 3 The sized S-biobr@ms material was placed in a reaction cell containing 50ml of 10ppm rhodamine B aqueous solution at ph=7. The reaction tank system is placed in a dark place and stirred for 30min to reach self-absorption-desorption balance of the material to rhodamine B. After 30min, the reaction cell was placed under irradiation of a 500W xenon lamp (simulated sunlight). And 4mL of reaction solution is taken every 30min of irradiation, and the content of rhodamine B in the solution is measured by using an ultraviolet-visible light diffuse reflection spectrometer. As shown in a3 of FIG. 8, the degradation efficiency of the alkali-treated S-BiOBr@MS material on rhodamine B reaches more than 98% after the illumination is carried out for 3 hours, and the solution becomes colorless and transparent after the reaction is finished.
The photocatalytic degradation capability of the S-BiOBr@MS material subjected to alkali treatment on methylene blue is also considered, and specific experimental operations are the same as those described above, as shown in b 1-b 2 in FIG. 8. As shown in b3 of FIG. 8, the degradation efficiency of the alkali-treated S-BiOBr@MS material on methylene blue reaches more than 97% after the irradiation for 6 hours, and the solution becomes colorless and transparent after the reaction is finished.
The photocatalytic degradation capability of the S-BiOBr@MS material subjected to alkali treatment on tetracycline hydrochloride is also considered, and specific experimental operations are the same as those described above, as shown in fig. 8, namely c 1-c 2. As shown in the graph C3 of FIG. 8, the degradation efficiency of the alkali-treated S-BiOBr@MS material on tetracycline hydrochloride reaches over 66% after illumination for 2 hours, and the solution becomes colorless and transparent after the reaction is finished.
Claims (5)
1. The preparation method of the intelligent oil-water separation material is characterized by comprising the following steps of:
1) Adding bismuth nitrate pentahydrate into a mixed solution of deionized water and glycerol, carrying out ultrasonic treatment for 10min, and stirring at room temperature until the solution is clear and transparent to obtain a solution A; dissolving potassium bromide in deionized water, and stirring until the potassium bromide is completely dissolved to obtain a solution B; the volume ratio of the deionized water to the glycerol=1:2; bismuth nitrate to potassium bromide=1:1 in molar ratio;
2) Immersing melamine sponge MS in the solution B to enable the sponge to fully absorb the solution B, then dropwise adding the rest of the solution B into the solution A, transferring the sponge adsorbed with the solution B into the solution A, stirring for 1h, and aging for 3h at room temperature; after the reaction is finished, taking out the sponge, washing with water and ethanol, and drying to obtain a BiOBr crystal grown in situ on the melamine sponge MS to synthesize a BiOBr@MS;
3) Dissolving perfluoro caprylic acid and 3-aminopropyl trimethoxy silane in absolute ethyl alcohol, stirring, activating for 1h at 60 ℃ to obtain a modification liquid, putting BiOBr@MS into the modification liquid, soaking for 4h at 60 ℃, taking out, and drying to obtain a target product S-BiOBr@MS.
2. The use of the intelligent oil-water separation material prepared according to the method of claim 1 for adsorbing oil, characterized in that the method comprises the following steps: and (3) adding an intelligent oil-water separation material into the oil-water mixture for adsorption.
3. The application of the intelligent oil-water separation material prepared by the method according to claim 1 in oil-water separation is characterized in that the method comprises the following steps: filtering the oil-water mixture by an intelligent oil-water separation material or an intelligent oil-water separation material treated by alkali, and carrying out gravity separation and pump separation.
4. The use of an intelligent oil-water separation material prepared according to the method of claim 1 in photocatalytic degradation of organic pollutants in wastewater.
5. The use according to claim 4, characterized in that the method is as follows: and adding an intelligent oil-water separation material or an intelligent oil-water separation material treated by alkali into the wastewater containing the organic pollutants to perform photocatalytic degradation.
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