CN113731186A - Preparation method of metal nanoparticle/lignocellulose-based functionalized filter membrane for treating wastewater - Google Patents
Preparation method of metal nanoparticle/lignocellulose-based functionalized filter membrane for treating wastewater Download PDFInfo
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Abstract
The invention discloses a preparation method of a metal nanoparticle/lignocellulose-based functionalized filter membrane for treating wastewater. The method has simple process, low cost and environmental protection, and can be applied to actual industrial production; the functionalized filter membrane product has excellent catalytic and antibacterial properties, excellent stability and recoverability, and can be widely used for treating nitrogen-containing organic pollutants and microbial pollutants in wastewater.
Description
Technical Field
The invention belongs to the technical field of biomass material processing and the field of water treatment, and particularly relates to a preparation method of a metal nanoparticle/lignocellulose-based functionalized filter membrane for treating wastewater.
Background
The pollutant sources in the wastewater are wide, and the nitrogen-containing organic compounds and biological pollutants seriously pollute the water environment. In recent years, the content of nitrogen-containing organic substances and microbial pollutants in water environment has increased due to the development of industrial production, the expansion of human social activities and agricultural activities in the production of nitrogen-containing organic substances and the regeneration of microorganisms, and the pollutants are toxic, carcinogenic, mutagenic and the like to human beings and aquatic organisms. In order to improve the current situation of wastewater pollution, various treatment methods such as adsorption, chemical precipitation, extraction, ion exchange, filtration, catalysis and the like can be applied to the treatment of wastewater. Metal nanoparticles have gained wide attention in wastewater treatment because of their high specific surface area, catalytic ability, antibacterial properties and stability. However, in practice, metal nanoparticles have problems of synthesis, aggregation, and difficulty in recovery, thus making them impossible to be applied on a large scale.
The lignocellulose raw material has the advantages of no toxicity, no harm, low cost, reproducibility, sustainability, biodegradability and the like, has wide sources, and can be obtained from different kinds of plants. The main chemical components of the lignocellulose contain various functional groups such as hydroxyl, carboxyl, mercapto, nitrogen, phosphorus, sulfur and the like, and have strong reduction capability, so that the precious metal nanoparticles with high catalytic activity are reduced in situ by taking the lignocellulose as the raw material, and the lignocellulose raw material has a wide application prospect, has a three-dimensional network and a porous structure, can be used for stabilizing and dispersing the metal nanoparticles, reduces the coagulation phenomenon in the using process, and improves the recycling performance.
In the chinese patent application, "graphene-like embedded in metal nanoparticles, and a preparation method and application thereof" (application No. 201910757045.6, published 2021, 3/5/l), organic small molecules are used as a carbon source, placed in a quartz boat, and directly deposited on a metal substrate by using a normal pressure physical meteorological transmission method, so as to obtain the graphene-like embedded in metal nanoparticles. However, the method needs to be carried out in inert gas at the high temperature of 500-650 ℃, has complex preparation process, higher energy consumption and increased cost, and is not suitable for large-scale popularization and application.
Disclosure of Invention
The invention discloses a preparation method of a metal nanoparticle/lignocellulose-based functionalized filter membrane for treating wastewater, which is simple in process, low in cost and environment-friendly.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a metal nanoparticle/lignocellulose-based functionalized filter membrane for treating wastewater takes lignocellulose as a raw material, and metal salt is reduced in situ into metal nanoparticles loaded on the surface of the lignocellulose raw material so as to prepare the functionalized filter membrane.
The in situ reduction is carried out under heat or light.
The lignocellulose is selected from eucalyptus, tung, balsa, sugarcane, and basswood.
The metal salt is silver nitrate, chloroauric acid, nickel nitrate, and copper acetate.
The preparation method of the functionalized filter membrane comprises the following steps:
(1) cutting a lignocellulose raw material into a sheet sample, grinding and polishing the sample, and then washing the sample for multiple times by using deionized water to remove surface impurities;
(2) extracting the flaky sample obtained in the step (1) in a Soxhlet extractor by using a benzene alcohol mixed solution, then washing the flaky sample with deionized water for multiple times, and air-drying the flaky sample overnight to obtain a lignocellulose-based sample;
(3) adding the lignocellulose-based sample in the step (2) into a metal salt solution for vacuum soaking treatment;
(4) and (3) heating or lighting the lignocellulose-based sample containing the metal salt obtained by the treatment in the step (3), ultrasonically washing the lignocellulose-based sample in deionized water after the reaction is finished, then washing the lignocellulose-based sample with ethanol and deionized water for multiple times, removing unreacted impurities, and performing vacuum drying to obtain the metal nanoparticle/lignocellulose-based functional filter membrane.
In the step (1), the diameter of the sheet sample is 1-8cm, and the thickness of the sheet sample is 1-5 mm; in the step (2), the mixed solution of benzene and ethanol with the volume ratio of 2:1 is used as the mixed solution of benzene and ethanol; the metal salt solution in the step (3) is prepared by dissolving the metal salt in deionized water, and the concentration of the metal salt is 1-100 mM.
The temperature of the extraction treatment in the step (2) is 90 ℃, and the time is 24 hours; the heating or light irradiation treatment in the step (4) is carried out at 70-90 deg.C for 0.5-3h, the ultrasonic washing time is 30min, and the vacuum drying time is 8 h.
The metal nano-particle/lignocellulose-based functionalized filter membrane prepared by the preparation method.
The application of the metal nano-particle/lignocellulose-based functionalized filter membrane in the aspect of wastewater treatment.
The application is used for removing nitrogenous organic matters in wastewater and killing microorganisms in the wastewater.
Aiming at the problems existing in the preparation and use of the metal nanoparticles for wastewater treatment at present, the inventor establishes a preparation method of the metal nanoparticles/lignocellulose-based functionalized filter membrane for wastewater treatment, lignocellulose is used as a raw material, and metal salt is reduced in situ into metal nanoparticles to be loaded on the surface of the lignocellulose raw material, so that the functionalized filter membrane is prepared. The method uses the lignocellulose raw material to modify the metal nanoparticles by an in-situ reduction method, overcomes the harmfulness of reducing the metal nanoparticles by a chemical method and the problems of difficult coagulation and recovery of the metal nanoparticles in practical application of wastewater treatment, can realize high-value utilization of the lignocellulose raw material, can maintain high catalytic activity of the metal nanoparticles, and realizes effective removal of nitrogen-containing organic matters in the wastewater and killing of microorganisms in the wastewater. The metal nanoparticle/lignocellulose-based functionalized filter membrane prepared by the invention takes lignocellulose as a carrier and precious metal nanoparticles as modifiers, and pollutants in wastewater can be effectively treated by utilizing the high catalytic performance of the metal nanoparticles and the three-dimensional porous structure of the lignocellulose.
In conclusion, the raw material for preparing the metal nanoparticle/lignocellulose-based functionalized filter membrane is a renewable plant fiber raw material, can be directly obtained from the nature, has rich sources, low cost and can be recycled, thereby meeting the national sustainable development strategy and opening up a new idea for high-value utilization of lignocellulose raw materials; the preparation process is simple and easy to implement, safe and environment-friendly, does not use chemical reagents, saves energy consumption, has low requirements on equipment, and can be applied to actual industrial production; the functionalized filter membrane product has excellent catalytic and antibacterial properties, excellent stability and recoverability, and can be widely used for treating nitrogen-containing organic pollutants and microbial pollutants in wastewater.
Drawings
Fig. 1 is a scanning electron microscope image of a silver nanoparticle/lignocellulose-based functionalized filter membrane obtained in example 1 of the present invention, in which (a) is a scanning electron microscope image of a silver nanoparticle/lignocellulose-based pipeline structure, and (b) is a scanning electron microscope image of silver nanoparticles uniformly dispersed on lignocellulose-based.
Fig. 2 is a dynamic filtration and purification diagram of a silver nanoparticle/lignocellulose-based functionalized filter membrane in a simulation device for bacteria-containing wastewater in example 2 of the present invention, in which (a) is a wastewater dynamic filtration simulation device, (b) is a schematic diagram of escherichia coli in wastewater before filtration, (c) is a schematic diagram of escherichia coli death after filtration by the filter membrane, (d) is a schematic diagram of staphylococcus aureus in wastewater before filtration, and (e) is a schematic diagram of staphylococcus aureus death after filtration.
Fig. 3 is a dynamic filtration catalysis test chart of a gold nanoparticle/lignocellulose-based functionalized filter membrane on a nitrogenous organic matter 4-nitrophenol in a simulation device in embodiment 3 of the invention, wherein (a) is a wastewater dynamic filtration simulation device, and (b) is an ultraviolet monitoring chart before and after 4-nitrophenol wastewater filtration.
FIG. 4 is a diagram of the gold nanoparticle/lignocellulose-based functionalized filter membrane of example 3 of the present invention in a simulation apparatus for dynamic catalytic degradation of a nitrogenous organic compound, 4-nitrophenol.
Detailed Description
The present invention will be described in further detail with reference to examples, wherein the experimental methods used are conventional methods unless otherwise specified, and experimental drugs such as materials and reagents used therein are commercially available without otherwise specified.
Example 1 preparation of silver nanoparticle/lignocellulose-based functionalized filtration membranes
(1) Pretreatment of raw materials: cutting eucalyptus into a sheet sample with the diameter of 8cm and the thickness of 1mm, polishing, and washing with deionized water for multiple times to remove surface impurities.
(2) And (2) extracting the eucalyptus flake sample in the step (1) by using a benzene-alcohol mixed solution (benzene: ethanol is 2:1) in a soxhlet extractor at the temperature of 90 ℃ for 24h, washing the eucalyptus flake sample with deionized water for multiple times, and air-drying the eucalyptus flake sample overnight to obtain the eucalyptus sample.
(3) And (3) adding the eucalyptus sample obtained in the step (2) into a 50mM silver nitrate solution for vacuum soaking treatment.
(4) And (3) heating the eucalyptus sample containing the metal salt in the step (3), wherein the temperature is 90 ℃, the treatment time is 3 hours, after the reaction is finished, ultrasonically washing the eucalyptus in deionized water for 30min, then washing the eucalyptus with ethanol and deionized water for multiple times, removing unreacted impurities, and performing vacuum drying for 8 hours to obtain the silver nanoparticle/lignocellulose-based filter membrane.
Example 2 preparation of silver nanoparticle/lignocellulose-based functionalized filtration membranes
(1) Pretreatment of raw materials: cutting sugarcane into a sheet sample with the diameter of 3cm and the thickness of 3mm, polishing, and washing with deionized water for multiple times to remove surface impurities.
(2) And (2) extracting the sugarcane flaky sample in the step (1) by using a benzene-alcohol mixed solution (benzene: ethanol is 2:1) in a soxhlet extractor at the temperature of 90 ℃ for 24h, washing the sugarcane flaky sample with deionized water for multiple times, and air-drying the sugarcane flaky sample overnight to obtain the sugarcane sample.
(3) And (3) adding the sugarcane sample in the step (2) into a 10mM silver nitrate solution for vacuum soaking treatment.
(4) And (3) heating the sugarcane sample containing the metal salt in the step (3), wherein the temperature is 70 ℃, the treatment time is 0.5h, ultrasonically washing the sugarcane in deionized water for 30min after the reaction is finished, then washing the sugarcane with ethanol and deionized water for multiple times, removing unreacted impurities, and performing vacuum drying for 8h to obtain the silver nanoparticle/lignocellulose-based filter membrane.
Example 3 preparation of gold nanoparticle/lignocellulose-based functionalized filtration Membrane
(1) Pretreatment of raw materials: cutting and processing the tung wood into a sheet sample with the diameter of 4cm and the thickness of 2mm, polishing, and then washing with deionized water for multiple times to remove surface impurities.
(2) And (2) extracting the tung wood sheet sample in the step (1) by using a benzene-alcohol mixed solution (benzene: ethanol is 2:1) in a soxhlet extractor at the temperature of 90 ℃ for 24h, washing the tung wood sheet sample with deionized water for multiple times, and air-drying the tung wood sheet sample overnight to obtain the tung wood sample.
(3) And (3) adding the tung wood sample in the step (2) into a chloroauric acid solution with the concentration of 2mM for vacuum soaking treatment.
(4) And (3) carrying out illumination treatment on the tung wood sample containing the metal salt in the step (3), wherein the illumination treatment time is 3h, ultrasonically washing the tung wood in deionized water for 30min after the reaction is finished, then washing the tung wood with ethanol and deionized water for multiple times, removing unreacted impurities, and carrying out vacuum drying for 8h to obtain the gold nanoparticle/lignocellulose-based filter membrane.
Example 4 preparation of gold nanoparticle/lignocellulose-based functionalized filtration Membrane
(1) Pretreatment of raw materials: cutting sugarcane into a sheet sample with the diameter of 2cm and the thickness of 4mm, polishing, and washing with deionized water for multiple times to remove surface impurities.
(2) And (2) extracting the sugarcane flaky sample in the step (1) by using a benzene-alcohol mixed solution (benzene: ethanol is 2:1) in a soxhlet extractor at the temperature of 90 ℃ for 24h, washing the sugarcane flaky sample with deionized water for multiple times, and air-drying the sugarcane flaky sample overnight to obtain the sugarcane sample.
(3) And (3) adding the sugarcane sample in the step (2) into a chloroauric acid solution with the concentration of 1mM for vacuum soaking treatment.
(4) And (3) carrying out illumination treatment on the sugarcane sample containing the metal salt in the step (3), wherein the illumination time is 0.5h, ultrasonically washing the sugarcane in deionized water for 30min after the reaction is finished, then washing the sugarcane with ethanol and deionized water for multiple times, removing unreacted impurities, and carrying out vacuum drying for 8h to obtain the gold nanoparticle/lignocellulose-based filter membrane.
Example 5 preparation of gold nanoparticle/lignocellulose-based functionalized filtration Membrane
(1) Pretreatment of raw materials: cutting Barsha wood into a sheet sample with the diameter of 5cm and the thickness of 4mm, polishing, and washing with deionized water for multiple times to remove surface impurities.
(2) And (2) extracting the balsa sheet sample in the step (1) in a soxhlet extractor by using a benzene-alcohol mixed solution (benzene: ethanol is 2:1), washing the balsa sheet sample for multiple times by using deionized water at the temperature of 90 ℃ for 24 hours, and air-drying the balsa sheet sample overnight to obtain the balsa sample.
(3) Adding the balsawood sample in the step (2) into a nickel nitrate solution with the concentration of 100mM for vacuum soaking treatment.
(4) And (3) carrying out illumination treatment on the Barbarea sample containing the metal salt in the step (3), wherein the illumination time is 1h, ultrasonically washing the Barbarea in deionized water for 30min after the reaction is finished, then washing the Barbarea with ethanol and deionized water for multiple times, removing unreacted impurities, and carrying out vacuum drying for 8h to obtain the nickel nanoparticle/lignocellulose-based filter membrane.
Application example 1 high resolution scanning electron microscopy analysis of functionalized filters
As shown in fig. 1, in example 1, after the cross section and the surface of the metal nanoparticle/lignocellulose-based functionalized filter membrane are subjected to gold spraying treatment, scanning is performed on an electron microscope, and the metal nanoparticles are uniformly dispersed on the surface of the lignocellulose raw material pipeline. The uniform distribution and the three-dimensional pipeline structure of the metal nanoparticles are beneficial to effective contact of pollutants in the wastewater and the metal nanoparticles. Application example 2 Performance test of purification and Sterilization with functionalized Filter Membrane
As shown in figure 2, the silver nanoparticle/lignocellulose-based functionalized filter membrane of example 2 is used to construct a dynamic wastewater treatment device to treat wastewater containing Escherichia coli and Staphylococcus aureus. After being filtered by the filter membrane, the physiological structure of bacteria is destroyed, which shows that the silver nanoparticle/lignocellulose-based functionalized filter membrane can effectively kill microorganisms in wastewater.
Application example 3 Performance test of catalytic reduction of 4-nitrophenol with functionalized filter membranes
Under the condition of room temperature, a dynamic wastewater treatment device is constructed by utilizing the gold nanoparticles/lignocellulose-based functionalized filter membrane in the embodiment 3 for catalytic reduction of 4-nitrophenol, and wastewater simulation is carried out by using 4-nitrophenol (0.2mmol/L) and NaBH4(50mmol/L), and the concentration change of 4-nitrophenol before and after filtration is monitored by an ultraviolet-visible spectrophotometer. As shown in FIG. 3, 400nm and 287nm are characteristic absorption peaks of 4-nitrophenol and 4-aminophenol, respectively, and after treatment, the characteristic peak of 4-nitrophenol disappears and the characteristic peak of 4-aminophenol appears. The experimental result shows that the gold nanoparticle/lignocellulose-based functionalized filter membrane has excellent catalytic performance.
Application example 4 example 3 Recycling Performance testing of functionalized Filter membranes
At room temperature, 4-nitrophenol (0.2mmol/L) and NaBH4(50mmol/L) mixed solution is simulated wastewater, and the recycling performance of the filter membrane is monitored by using an ultraviolet-visible spectrophotometer. After each time of wastewater treatment, the filter membrane is washed for multiple times by using ethanol and deionized water in sequence, and then recycled for the next time after air drying. As shown in FIG. 4, after 8 times of recycling, the catalytic degradation efficiency of 4-nitrophenol is still as high as 85%. Experimental results show that the functionalized filter membrane prepared by the invention has excellent recycling performance.
Claims (10)
1. A preparation method of a metal nanoparticle/lignocellulose-based functionalized filter membrane for treating wastewater is characterized in that lignocellulose is used as a raw material, and metal salt is reduced in situ into metal nanoparticles to be loaded on the surface of the lignocellulose raw material, so that the functionalized filter membrane is prepared.
2. The method of claim 1, wherein the functionalized filter membrane is prepared by: the in-situ reduction is carried out under heating or illumination.
3. The method of claim 1, wherein the functionalized filter membrane is prepared by: the lignocellulose base is selected from eucalyptus, tung, balsa, sugarcane, and basswood.
4. The method of claim 1, wherein the functionalized filter membrane is prepared by: the metal salt is silver nitrate, chloroauric acid, nickel nitrate and copper acetate.
5. The process for the preparation of a functionalized filter membrane according to claim 1, characterized in that it is carried out according to the following steps:
(1) cutting a lignocellulose raw material into a sheet sample, grinding and polishing the sample, and then washing the sample for multiple times by using deionized water to remove surface impurities;
(2) extracting the flaky sample obtained in the step (1) in a Soxhlet extractor by using a benzene alcohol mixed solution, then washing the flaky sample with deionized water for multiple times, and air-drying the flaky sample overnight to obtain a lignocellulose-based sample;
(3) adding the lignocellulose-based sample in the step (2) into a metal salt solution for vacuum soaking treatment;
(4) and (3) heating or lighting the lignocellulose-based sample containing the metal salt obtained by the treatment in the step (3), ultrasonically washing the lignocellulose-based sample in deionized water after the reaction is finished, then washing the lignocellulose-based sample with ethanol and deionized water for multiple times, removing unreacted impurities, and performing vacuum drying to obtain the metal nanoparticle/lignocellulose-based functional filter membrane.
6. The method for preparing a functionalized filter membrane according to claim 1, wherein in step (1), the sheet sample has a diameter of 1-8cm and a thickness of 1-5 mm; in the step (2), the mixed solution of benzene and ethanol with the volume ratio of 2:1 is used as the mixed solution of benzene and ethanol; the metal salt solution in the step (3) is prepared by dissolving the metal salt in deionized water, and the concentration of the metal salt is 1-100 mM.
7. The process for preparing a functionalized filter membrane according to claim 1, wherein the temperature of the extraction treatment in step (2) is 90 ℃ and the time is 24 hours; the heating or light irradiation treatment in the step (4) is carried out at 70-90 deg.C for 0.5-3h, the ultrasonic washing time is 30min, and the vacuum drying time is 8 h.
8. The metal nanoparticle/lignocellulose-based functionalized filter membrane obtained by the preparation method of any one of claims 1 to 7.
9. Use of the metal nanoparticle/lignocellulose-based functionalized filtration membrane according to claim 8 for wastewater treatment.
10. The use of claim 9 for removing nitrogenous organic compounds from wastewater and for killing microorganisms in wastewater.
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| CN116328733A (en) * | 2023-03-10 | 2023-06-27 | 广西民族大学 | Cationic sugarcane loaded nano silver composite material and preparation method and application thereof |
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