CN113929220A - Preparation method of composite material of mesoporous quantum photocatalytic material and biological bacteria based on limited-area oxygenation technology - Google Patents
Preparation method of composite material of mesoporous quantum photocatalytic material and biological bacteria based on limited-area oxygenation technology Download PDFInfo
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- 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
- 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
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Microbiology (AREA)
- Dispersion Chemistry (AREA)
- Biodiversity & Conservation Biology (AREA)
- Health & Medical Sciences (AREA)
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Abstract
The invention provides a preparation method of a composite material of a mesoporous quantum photocatalytic material and biological bacteria based on a limited-area oxygenation technology, which comprises the steps of preparing the mesoporous quantum photocatalytic material and a microorganism-mesoporous quantum photocatalyst, and preparing a microorganism-mesoporous quantum photocatalytic biological filler and a microorganism-mesoporous quantum photocatalytic microorganism generator by using the microorganism-mesoporous quantum photocatalyst. The composite material of the porous photocatalysis and biological bacteria is prepared by proportioning the photocatalysis material, the porous material and the microbial material according to a certain proportion, and the microorganism-mesoporous quantum photocatalyst, the microorganism-mesoporous quantum photocatalytic biological filler and the microorganism-mesoporous quantum photocatalytic microbial generator in the composite material have the limited-area oxygen increasing function, so that the advantages of the porous photocatalysis technology and the biological bacteria technology combined with green sewage treatment such as black and odorous water, blue algae sewage and domestic sewage are fully exerted, the application scene is expanded, and the service life is prolonged.
Description
Technical Field
The invention relates to the technical field of environmental management materials, in particular to a preparation method of a composite material of a mesoporous quantum photocatalytic material and biological bacteria based on a limited-area oxygenation technology.
Background
In recent years, with the rapid development of economy in China, the process of urbanization and industrialization is accelerated, and the discharge amount of urban sewage is continuously increased. However, at present, urban water body protection infrastructure is imperfect, water pollution control and treatment measures are seriously lagged, a large amount of pollutants enter a river, and some urban water bodies, especially water bodies in middle and small cities, directly become main discharge places of industrial, agricultural and domestic wastewater. The concentration of pollutants such as Chemical Oxygen Demand (COD), nitrogen and phosphorus in the water body greatly exceeds the standard, so that the eutrophication of the water body is caused, and seasonal or perennial black and odorous water is frequently seen. The urban black and odorous water body brings extremely poor sensory experience to the masses, becomes the prominent water environment problem at present, and seriously influences the good development of cities in China.
The photocatalytic technology is to utilize semiconductor material to absorb solar energy to perform chemical oxidation-reduction reaction, so as to decompose organic matters into water and carbon dioxide. The technology is used for carrying out in-situ treatment on the sewage by utilizing solar energy, and has the advantages of small engineering quantity, low treatment cost, greenness and safety. The core of the technology is physical/chemical adsorption and photocatalysis, graphene has strong adsorption capacity and can effectively capture various organic pollutants, heavy metal ions, harmful gases and the like in a water body, and titanium dioxide thoroughly decomposes the captured organic pollutants into water and carbon dioxide through photocatalysis to realize sewage treatment. At present, graphene on the market is expensive according to the requirement of purity, the price of the graphene is between dozens of yuan per gram and hundreds of yuan per gram, and the sewage treatment usually needs tons of raw materials, which is obviously not favorable for the commercial application of the graphene photocatalytic material in the aspect of water body treatment.
The research of water pollution treatment by combining zeolite powder with various microorganisms is increased year by year, and the effect is obvious compared with the effect of performing biodegradation by singly using microbial thalli or performing sewage and wastewater treatment by singly using the ion exchange performance and the adsorption performance of the zeolite powder. In these studies, zeolite powder is mostly used as a support carrier, and due to the advantages of its physicochemical properties, it can promote the enrichment and growth of microorganisms on its surface, further expanding the effects of both microorganisms and zeolite powder. In addition, the surface enriched microorganism can regenerate the zeolite powder to a certain extent due to various metabolic activities, so that the reutilization rate and the service life of the zeolite powder are improved. However, at present, there is no report on the preparation of a porous photocatalytic synergistic biological bacteria composite material by proportioning a photocatalytic material, a porous material and a microbial material according to a certain proportion, the expansion of an application scene and the improvement of a service life.
Disclosure of Invention
The invention provides a preparation method of a mesoporous quantum photocatalytic material and biological bacteria synergistic composite material based on a limited-area oxygenation technology, aiming at the technical problems that a photocatalytic material, a porous material and a microbial material are not proportioned according to a certain proportion to prepare a porous photocatalytic synergistic biological bacteria composite material, the application scene is expanded and the service life is prolonged in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a composite material of a mesoporous quantum photocatalytic material and biological bacteria based on a limited-area oxygenation technology comprises the following steps:
physically stirring, grinding and compounding the porous material with a certain specific surface area and the photocatalytic material according to a set proportion to prepare the mesoporous quantum photocatalytic material;
compounding quantitative biological bacteria and a mesoporous quantum photocatalytic material to prepare a mesoporous quantum photocatalytic material composite biological bacteria material with a biodegradation function, namely a microorganism-mesoporous quantum photocatalyst;
loading a microorganism-mesoporous quantum photocatalyst on the surface of a fiber substrate to prepare a microorganism-mesoporous quantum photocatalytic biological filler with photocatalytic activity;
extruding and pouring the microorganism-mesoporous quantum photocatalyst to prepare a microorganism-mesoporous quantum photocatalytic microorganism generator with a honeycomb structure;
the microorganism-mesoporous quantum photocatalyst, the microorganism-mesoporous quantum photocatalytic biological filler and the microorganism-mesoporous quantum photocatalytic microorganism generator have a limited-area oxygen increasing function, the limited-area oxygen increasing function means that due to the rich mesoporous structure of the mesoporous quantum photocatalytic material, the light irradiation depth can be increased, light is reflected and refracted for multiple times in a pore channel, so that the porous material can absorb a light source of 200-1200 nm, the use efficiency of incident sunlight is higher than 10%, the mesoporous quantum photocatalytic material generates electron hole pairs under illumination, and the dissolved oxygen concentration of 1-2 m around the material can be increased by 0.1-10 mg/L through oxygen generated by water splitting.
Compared with the prior art, the preparation method of the composite material of the mesoporous quantum photocatalytic material and the biological bacteria based on the limited-area oxygenation technology, provided by the invention, is characterized in that the photocatalytic material, the porous material and the microbial material are proportioned according to a certain proportion to prepare the composite material of the porous photocatalytic synergistic biological bacteria, and a microorganism-mesoporous quantum photocatalyst, a microorganism-mesoporous quantum photocatalytic biological filler and a microorganism-mesoporous quantum photocatalytic microbial generator in the composite material have the limited-area oxygenation function, so that the advantages of combining the porous photocatalytic technology and the biological bacteria technology and treating sewage in a green way are fully exerted. Specifically, the porous photocatalysis technology can adsorb a large amount of organic matters in water through a mesoporous structure and then decompose the organic matters through photocatalysis, biological bacteria adsorbed on the surface of a mesoporous quantum photocatalysis material can also mineralize in situ to quickly decompose the organic matters on the surface of the porous material, so that the photocatalysis efficiency is improved, the photocatalysis technology supplements oxygen for the biological bacteria, the activity and the reproductive capacity of the biological bacteria are improved, the biological bacteria cooperate with the photocatalysis to accelerate the decomposition rate, the biological bacteria cooperate with the photocatalysis to promote the in-situ treatment effect of the water, no chemical reagent is added in the whole sewage treatment process, and the energy of the nature is really utilized to purify the water; in addition, the mesoporous quantum photocatalytic material is cooperated with the composite material of the biological bacteria to carry out water pollution treatment, manual dredging and sewage interception are not needed, in-situ and green scientific treatment is realized, the engineering quantity is small, the method is economic and environment-friendly, and the method is suitable for treating black and odorous water, blue algae sewage, domestic sewage and the like, so that the application scene is expanded and the service life is prolonged.
Further, the porous material is at least one selected from zeolite powder, molecular sieves, activated carbon, porous alumina, mesoporous silica, mesoporous carbon, mesoporous silicon, carbon black, attapulgite, bentonite, diatomite, three-dimensional graphene, metal organic framework materials, covalent organic framework materials, and two-dimensional metal carbides or nitrides.
Further, the specific surface area of the porous material is not less than 150m2A pore diameter of 0.1 to 10nm and a pore volume of not less than 0.1cm3The porous material has surface hydrophilicity, and the contact angle is not more than 30 degrees.
Further, the photocatalytic material is at least one selected from titanium oxide, zinc oxide, tungsten oxide, carbon nitride, a silver halide photocatalytic material, silver phosphate, indium oxide, strontium titanate, bismuth vanadate, zinc sulfide, copper sulfide, and cuprous oxide.
Further, the physical stirring and grinding compounding of the porous material with a certain specific surface area and the photocatalytic material according to a set proportion means that the porous material and the photocatalytic material are mixed in a ball milling mode, a sand milling mode or an air flow milling mode and a high-speed shearing mode, and the porous material and the photocatalytic material are compounded in a physical adsorption mode and an electrostatic adsorption mode.
Further, the mass ratio of the porous material to the photocatalytic material is 1-1000: 1-1000, and the size of the photocatalytic material is 1-10 nm after physical stirring and grinding treatment.
Furthermore, the mesoporous quantum photocatalytic material is formed by a micron porous framework-mesoporous photocatalytic material and is provided with a micron pore-nanometer mesoporous two-stage fractal junctionThe specific surface area of the mesoporous quantum photocatalytic material is not less than 50m2A pore diameter of 0.1 to 3nm and a pore volume of not less than 0.1cm3The light absorption waveband is 200-1200 nm.
Further, the biological bacteria comprise aerobic biological bacteria and facultative biological bacteria, the aerobic biological bacteria adopt bacillus or/and nitrobacteria, and the facultative biological bacteria adopt denitrifying bacteria or/and nitrifying and denitrifying composite bacteria.
Further, the mass ratio of the biological bacteria to the mesoporous quantum photocatalytic material is 1-100: 1-100 ℃, the pH value of the use environment of the biological bacteria is controlled to be 6-9, the water temperature is controlled to be 5-35 ℃, the composite mode of the biological bacteria and the mesoporous quantum photocatalytic material is mechanical mixing and electrostatic adsorption, the electrostatic adsorption refers to adsorption of the mesoporous quantum photocatalytic material on the biological bacteria in a solvent, the adsorption time is not less than 0.1h, the temperature of the solvent is not less than 5 ℃, and the pH value of the solvent is not less than 1.
Furthermore, the mode of loading the microorganism-mesoporous quantum photocatalyst on the surface of the fiber base material is an impregnation method or a spraying method, the loading amount of the microorganism-mesoporous quantum photocatalyst on the surface of the fiber base material is 0.1-10 g/g, and the fiber is selected from at least one of polyester cotton, nylon, terylene, polypropylene fiber and acrylic fiber.
Drawings
FIG. 1 is a schematic flow chart of a preparation method of a mesoporous quantum photocatalytic material synergistic biological bacteria composite material based on a limited-area oxygenation technology.
Fig. 2 is a scanning electron microscope image of the graphene composite titanium oxide provided by the present invention.
FIG. 3 is a graph of the degradation effect of the graphene composite titanium oxide in the photocatalytic test provided by the invention.
FIG. 4 is a stability test of the degradation effect of the graphene composite titanium oxide in the photocatalytic test provided by the present invention.
FIG. 5 is a schematic view of water pollution treatment of the composite material prepared by the preparation method of the composite material of the mesoporous quantum photocatalytic material cooperating with the biological bacteria based on the limited-area oxygenation technology.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further explained below by combining the specific drawings.
Referring to fig. 1, the present invention provides a method for preparing a composite material of a mesoporous quantum photocatalytic material cooperating with biological bacteria based on a limited-area oxygenation technology, the method comprising:
physically stirring, grinding and compounding the porous material with a certain specific surface area and the photocatalytic material according to a set proportion to prepare the mesoporous quantum photocatalytic material;
compounding quantitative biological bacteria and a mesoporous quantum photocatalytic material to prepare a mesoporous quantum photocatalytic material composite biological bacteria material with a biodegradation function, namely a microorganism-mesoporous quantum photocatalyst;
loading a microorganism-mesoporous quantum photocatalyst on the surface of a fiber substrate to prepare a microorganism-mesoporous quantum photocatalytic biological filler with photocatalytic activity;
extruding and pouring the microorganism-mesoporous quantum photocatalyst to prepare a microorganism-mesoporous quantum photocatalytic microorganism generator with a honeycomb structure;
the microorganism-mesoporous quantum photocatalyst, the microorganism-mesoporous quantum photocatalytic biological filler and the microorganism-mesoporous quantum photocatalytic microorganism generator have a limited-area oxygen increasing function, the limited-area oxygen increasing function means that due to the rich mesoporous structure of the mesoporous quantum photocatalytic material, the light irradiation depth can be increased, light is reflected and refracted for multiple times in a pore channel, so that the porous material can absorb a light source of 200-1200 nm, the use efficiency of incident sunlight is higher than 10%, the mesoporous quantum photocatalytic material generates electron hole pairs under illumination, and the dissolved oxygen concentration of 1-2 m around the material can be increased by 0.1-10 mg/L through oxygen generated by water splitting.
Compared with the prior art, the preparation method of the composite material of the mesoporous quantum photocatalytic material and the biological bacteria based on the limited-area oxygenation technology, provided by the invention, is characterized in that the photocatalytic material, the porous material and the microbial material are proportioned according to a certain proportion to prepare the composite material of the porous photocatalytic synergistic biological bacteria, and a microorganism-mesoporous quantum photocatalyst, a microorganism-mesoporous quantum photocatalytic biological filler and a microorganism-mesoporous quantum photocatalytic microbial generator in the composite material have the limited-area oxygenation function, so that the advantages of combining the porous photocatalytic technology and the biological bacteria technology and treating sewage in a green way are fully exerted. Specifically, the porous photocatalysis technology can adsorb a large amount of organic matters in water through a mesoporous structure and then decompose the organic matters through photocatalysis, biological bacteria adsorbed on the surface of a mesoporous quantum photocatalysis material can also mineralize in situ to quickly decompose the organic matters on the surface of the porous material, so that the photocatalysis efficiency is improved, the photocatalysis technology supplements oxygen for the biological bacteria, the activity and the reproductive capacity of the biological bacteria are improved, the biological bacteria cooperate with the photocatalysis to accelerate the decomposition rate, the biological bacteria cooperate with the photocatalysis to promote the in-situ treatment effect of the water, no chemical reagent is added in the whole sewage treatment process, and the energy of the nature is really utilized to purify the water; in addition, the mesoporous quantum photocatalytic material is cooperated with the composite material of the biological bacteria to carry out water pollution treatment, manual dredging and sewage interception are not needed, in-situ and green scientific treatment is realized, the engineering quantity is small, the method is economic and environment-friendly, and the method is suitable for treating black and odorous water, blue algae sewage, domestic sewage and the like, so that the application scene is expanded and the service life is prolonged.
As a specific example, the porous material is at least one selected from zeolite powder, molecular sieve, activated carbon, porous alumina, mesoporous silica, mesoporous carbon, mesoporous silicon, carbon black, attapulgite, bentonite, diatomaceous earth, three-dimensional graphene, metal organic framework material, covalent organic framework material, and two-dimensional metal carbide or nitride.
As a specific example, the specific surface area of the porous material is not less than 150m2A pore diameter of 0.1 to 10nm and a pore volume of not less than 0.1cm3The porous material has surface hydrophilicity, and the contact angle is not more than 30 degrees, so that the amount of organic pollutants adsorbed by the porous material can be increased, and the decomposition of organic matters is accelerated.
In a specific embodiment, the photocatalytic material is at least one selected from the group consisting of titanium oxide, zinc oxide, tungsten oxide, carbon nitride, silver halide-based photocatalytic materials, silver phosphate, indium oxide, strontium titanate, bismuth vanadate, zinc sulfide, copper sulfide, and cuprous oxide.
As a specific example, the physical stirring and grinding compounding of the porous material with a certain specific surface area and the photocatalytic material according to a set ratio refers to mixing the porous material and the photocatalytic material by ball milling, sand milling or air flow milling and high-speed shearing, and compounding the porous material and the photocatalytic material by physical adsorption and electrostatic force adsorption.
As a specific embodiment, the mass ratio of the porous material to the photocatalytic material is 1-1000: 1-1000, and after physical stirring and grinding treatment, the size of the photocatalytic material is 1-10 nm, so that the photocatalytic material can uniformly coat the surface of the porous material, and a two-stage fractal structure of micron pores and nanometer mesopores is formed.
As a specific embodiment, the mesoporous quantum photocatalytic material is composed of a microporous framework-mesoporous photocatalytic material, and has a two-stage fractal structure of microporous and mesoporous, and the specific surface area of the mesoporous quantum photocatalytic material is not less than 50m2A pore diameter of 0.1 to 3nm and a pore volume of not less than 0.1cm3The light absorption waveband is 200-1200 nm, so that ultraviolet light, visible light and near infrared light can be fully absorbed, and the decomposition reaction of the photocatalytic organic matter is promoted.
As a specific example, the biological bacteria include aerobic biological bacteria and facultative biological bacteria, the aerobic biological bacteria are bacillus or/and nitrifying bacteria, and the facultative biological bacteria are denitrifying bacteria or/and nitrifying and denitrifying composite bacteria.
In a specific embodiment, the mass ratio of the biological bacteria to the mesoporous quantum photocatalytic material is 1-100: 1-100 ℃, the pH value of the use environment of the biological bacteria is controlled to be 6-9, the water temperature is controlled to be 5-35 ℃, the composite mode of the biological bacteria and the mesoporous quantum photocatalytic material is mechanical mixing and electrostatic adsorption, the electrostatic adsorption refers to adsorption of the mesoporous quantum photocatalytic material on the biological bacteria in a solvent, the adsorption time is not less than 0.1h, the temperature of the solvent is not less than 5 ℃, and the pH value of the solvent is not less than 1, so that the propagation of the biological bacteria can be promoted, and the loading of the biological bacteria on the surface of the mesoporous quantum photocatalytic material is accelerated.
In a specific embodiment, the microorganism-mesoporous quantum photocatalyst is loaded on the surface of the fiber substrate by an immersion method or a spraying method, the loading amount of the microorganism-mesoporous quantum photocatalyst on the surface of the fiber substrate is 0.1-10 g/g, and the fiber is at least one selected from polyester cotton, nylon, terylene, polypropylene and acrylic.
As a specific example, the honeycomb size of the honeycomb structure in the microorganism-mesoporous quantum photocatalytic microorganism generator is (1-200) × (1-200) mm3The pore diameter of the honeycomb is 1-10 mm, so that the capture performance of the microorganism-mesoporous quantum photocatalytic microorganism generator on organic pollutants can be improved.
In order to better understand the preparation method of the composite material of the mesoporous quantum photocatalytic material and the biological bacteria based on the limited-area oxygenation technology, the following description is given by combining specific examples:
example 1: preparation of active carbon composite titanium oxide mesoporous quantum photocatalytic material
Activated carbon powder (specific surface area 1000 m) with particle size of 200 meshes2/g)10g of the suspension is put into ethanol and stirred for 1 hour at the temperature of 25 ℃ to obtain suspension A;
mixing 10ml of tetrabutyl titanate with the suspension A, and stirring for 1h at 25 ℃ to obtain a suspension B;
adding 10ml of deionized water into the suspension B, and grinding for 1h by using a ball mill to obtain slurry C;
carrying out suction filtration on the slurry C to obtain a filter cake, and repeatedly washing the filter cake for 3 times by using deionized water;
and (3) placing the washed filter cake in a muffle furnace, and annealing at 400 ℃ for 2h to obtain powder D, namely the activated carbon composite titanium oxide mesoporous quantum photocatalytic material.
Example 2: preparation of graphene composite titanium oxide mesoporous quantum photocatalytic material (graphene-titanium oxide)
Graphene (with a specific surface area of 200 m) with a particle size of 1-3 μm2/g)1g is put in ethanol at 25 DEG CStirring for 1h to obtain a suspension A;
mixing 50ml of tetrabutyl titanate with the suspension A, and stirring for 1h at 25 ℃ to obtain a suspension B;
adding 10ml of deionized water into the suspension B, and grinding for 1h by using a ball mill to obtain slurry C;
carrying out suction filtration on the slurry C to obtain a filter cake, and repeatedly washing the filter cake for 3 times by using deionized water;
and (3) placing the filter cake after washing in a muffle furnace, and annealing at 400 ℃ for 2h to obtain powder D, namely the graphene composite titanium oxide mesoporous quantum photocatalytic material, as shown in figure 1.
Example 3: preparation of Attapulgite composite titanium oxide mesoporous Quantum photocatalytic Material (Attapulgite-titanium oxide)
Attapulgite with the particle size of 200 meshes (the specific surface area is 150 m)2/g)1g of the suspension is put into ethanol and stirred for 1 hour at the temperature of 25 ℃ to obtain suspension A;
mixing 50ml of tetrabutyl titanate with the suspension A, and stirring for 1h at 25 ℃ to obtain a suspension B;
adding 10ml of deionized water into the suspension B, and grinding for 5 hours by adopting a ball mill to obtain slurry C;
carrying out suction filtration on the slurry C to obtain a filter cake, and repeatedly washing the filter cake for 3 times by using deionized water;
and (3) placing the washed filter cake in a muffle furnace, and annealing at 400 ℃ for 2h to obtain powder D, namely the attapulgite composite titanium oxide mesoporous quantum photocatalytic material.
Example 4: preparation of graphene-titanium oxide-composite biological bacteria material
Weighing 2g of composite biological bacteria (containing nitrifying aerobic bacteria, bacillus and facultative denitrifying bacteria) and 1g of glucose, placing the weighed composite biological bacteria and the 1g of glucose into a 250mL conical flask, uniformly mixing the weighed composite biological bacteria and the glucose in a shaking table at 15 ℃, culturing, controlling the pH value of an aqueous solution to be 7, and keeping the culture time for 12 hours to obtain composite biological bacteria liquid A;
uniformly mixing 10g of graphene composite titanium oxide mesoporous quantum photocatalytic material and composite biological bacterium liquid A in a shaking table at 15 ℃ for adsorption cultivation, controlling the pH value of an aqueous solution to be 7, keeping the cultivation time for 12h, and obtaining graphene-titanium oxide-composite biological bacterium material mixed liquid B in a dark environment;
and centrifuging the mixed solution B to obtain a filter cake, and performing low-temperature freeze drying to obtain the graphene-titanium oxide-composite biological bacteria material.
Example 5: preparation of graphene titanium oxide mesoporous quantum photocatalytic biological filler
Preparing graphene-titanium oxide-composite biological bacteria material dispersion liquid according to a mass ratio of 1: 5: 100, mixing a graphene-titanium oxide-composite biological bacterium material, sodium polyacrylate and deionized water, performing ultrasonic treatment for 300min, and stirring for 2h to obtain a graphene-titanium oxide mesoporous quantum photocatalytic material dispersion liquid A;
the fiber material adopts non-woven fabrics/artificial aquatic weeds to prepare the photocatalytic non-woven fabrics/artificial aquatic weeds, firstly, the non-woven fabrics/artificial aquatic weeds are cleaned and dried according to the GB/T8629-2001 standard, and the bath ratio is 1: 20, soaking for 6min, placing the soaked sample on a small padder, and soaking for two times and rolling for two times; and then treating the sample in an automatic shaping drying machine at 150 ℃ for 2min, and finally drying in an electrothermal blowing drying oven at 90 ℃ to obtain the photocatalytic non-woven fabric/artificial waterweed, namely the graphene titanium oxide mesoporous quantum photocatalytic biological filler.
Example 6: preparation of microbial generator by adopting graphene-titanium oxide-composite biological bacteria material
Weighing 200g of composite biological bacteria (containing nitrifying aerobic bacteria, bacillus and facultative denitrifying bacteria) and 10g of glucose, placing the weighed composite biological bacteria and the 10g of glucose into a 250mL conical flask, uniformly mixing the weighed composite biological bacteria and the 10g of glucose in a shaking table at 15 ℃, culturing, controlling the pH value of an aqueous solution to be 7, and keeping the culture time for 12 hours to obtain composite biological bacteria liquid A;
uniformly mixing 1000g of graphene composite titanium oxide mesoporous quantum photocatalytic material and composite biological bacterium liquid A in a shaking table at 15 ℃ for adsorption cultivation, controlling the pH value of an aqueous solution to be 7, keeping the cultivation time for 12h, and obtaining graphene-titanium oxide-composite biological bacterium material mixed liquid B in a dark environment;
centrifuging the mixed solution B to obtain a filter cake, and performing low-temperature freeze drying to obtain a graphene-titanium oxide-composite biological bacteria material;
manufacturing a cylindrical microbial generator mold with the aperture of 1cm, the distance of 1cm, the diameter of 10cm and the height of 10cm, wherein the mold is made of stainless steel;
mixing the graphene-titanium oxide-composite biological bacteria material with polyacrylate according to the weight ratio of 5: 1 to obtain slurry, then filling the slurry into a cylindrical microbial generator mould, drying for 12 hours at the temperature of 50 ℃, naturally cooling and demoulding to obtain the graphene-titanium oxide-composite biological bacteria microbial generator.
Example 7: graphene-titanium oxide photocatalytic dye degradation activity
Preparing 50ml of 20ppm rhodamine B solution, weighing the graphene-titanium oxide photocatalyst prepared in the embodiment 2, placing the graphene-titanium oxide photocatalyst and the graphene-titanium oxide photocatalyst in a beaker, and fully stirring;
carrying out adsorption balance treatment for 60min, then opening a 30W xenon lamp and placing the xenon lamp at a position 15cm above a beaker, wherein a xenon lamp light source is provided with a 420nm filter plate and serves as a visible light source, and sampling is carried out at intervals of 10 min;
centrifuging all samples to obtain supernatant, testing the ultraviolet and visible light absorption spectrum of the supernatant, and finally obtaining visible light degradation data, as shown in fig. 2 and 3.
Example 8: degrading activity of blue algae water body by using graphene-titanium oxide-composite biological bacteria fiber material
Preparation of the test: 1.5m31000L of blue algae water is poured into the bucket, and the bucket is placed outdoors to be fully illuminated;
putting 500g of the graphene-titanium oxide synergistic microbial fibers prepared in the example 5 into a barrel, uniformly stirring, and treating for 7 days;
the water quality change of the blue algae is tested to obtain ammonia nitrogen, total phosphorus, Chemical Oxygen Demand (COD) and permanganate index, and the specific numerical values are shown in the following table 1.
TABLE 1
Example 9: treatment of black and odorous water body by graphene-titanium oxide-composite biological bacterium microbial generator
Preparation of the test: 1.5m3Filling 1000L of black and odorous water into the barrel, and placing the barrel in the barrelFully illuminating outdoors;
putting the 4 graphene-titanium oxide-composite biological bacteria microbial generators prepared in the example 6 into a barrel, and uniformly stirring for 7 days;
the water quality change of the black and odorous water body is tested to obtain ammonia nitrogen, total phosphorus, Chemical Oxygen Demand (COD) and permanganate index, and specific numerical values are shown in the following table 2.
TABLE 2
As can be seen from the data in tables 1 and 2, the graphene-titanium oxide-composite biological bacteria fiber material and the graphene-titanium oxide-composite biological bacteria microbial generator have significant effects in treating algae and black and odorous water bodies, and preferably have significant changes in the index values of ammonia nitrogen and chemical oxygen demand COD.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (10)
1. A preparation method of a composite material of a mesoporous quantum photocatalytic material and biological bacteria based on a limited-area oxygenation technology is characterized by comprising the following steps:
physically stirring, grinding and compounding the porous material with a certain specific surface area and the photocatalytic material according to a set proportion to prepare the mesoporous quantum photocatalytic material;
compounding quantitative biological bacteria and a mesoporous quantum photocatalytic material to prepare a mesoporous quantum photocatalytic material composite biological bacteria material with a biodegradation function, namely a microorganism-mesoporous quantum photocatalyst;
loading a microorganism-mesoporous quantum photocatalyst on the surface of a fiber substrate to prepare a microorganism-mesoporous quantum photocatalytic biological filler with photocatalytic activity;
extruding and pouring the microorganism-mesoporous quantum photocatalyst to prepare a microorganism-mesoporous quantum photocatalytic microorganism generator with a honeycomb structure;
the microorganism-mesoporous quantum photocatalyst, the microorganism-mesoporous quantum photocatalytic biological filler and the microorganism-mesoporous quantum photocatalytic microorganism generator have a limited-area oxygen increasing function, the limited-area oxygen increasing function means that due to the rich mesoporous structure of the mesoporous quantum photocatalytic material, the light irradiation depth can be increased, light is reflected and refracted for multiple times in a pore channel, so that the porous material can absorb a light source of 200-1200 nm, the use efficiency of incident sunlight is higher than 10%, the mesoporous quantum photocatalytic material generates electron hole pairs under illumination, and the dissolved oxygen concentration of 1-2 m around the material can be increased by 0.1-10 mg/L through oxygen generated by water splitting.
2. The preparation method of the composite material of the mesoporous quantum photocatalytic material and the biological bacteria based on the limited-area oxygenation technology according to claim 1, wherein the porous material is at least one selected from zeolite powder, a molecular sieve, activated carbon, porous alumina, mesoporous silica, mesoporous carbon, mesoporous silicon, carbon black, attapulgite, bentonite, diatomite, three-dimensional graphene, a metal organic framework material, a covalent organic framework material, a two-dimensional metal carbide or a nitride.
3. The preparation method of the composite material of the mesoporous quantum photocatalytic material and the biological bacteria based on the limited-area oxygenation technology according to claim 1, wherein the specific surface area of the porous material is not less than 150m2A pore diameter of 0.1 to 10nm and a pore volume of not less than 0.1cm3The porous material has surface hydrophilicity, and the contact angle is not more than 30 degrees.
4. The preparation method of the composite material of the mesoporous quantum photocatalytic material and the biological bacteria based on the limited-area oxygenation technology according to claim 1, wherein the photocatalytic material is at least one selected from titanium oxide, zinc oxide, tungsten oxide, carbon nitride, silver halide photocatalytic materials, silver phosphate, indium trioxide, strontium titanate, bismuth vanadate, zinc sulfide, copper sulfide and cuprous oxide.
5. The preparation method of the composite material of the mesoporous quantum photocatalytic material and the biological bacteria based on the limited-area oxygenation technology according to claim 1, wherein the physical stirring, grinding and compositing of the porous material with a certain specific surface area and the photocatalytic material according to a set proportion means that the porous material and the photocatalytic material are mixed in a ball milling, sand milling or air flow milling mode and a high-speed shearing mode, and the porous material and the photocatalytic material are composited in a physical adsorption and electrostatic force adsorption mode.
6. The preparation method of the composite material of the mesoporous quantum photocatalytic material and the biological bacteria based on the limited-area oxygenation technology according to claim 1, wherein the mass ratio of the porous material to the photocatalytic material is 1-1000: 1-1000, and the size of the photocatalytic material is 1-10 nm after physical stirring and grinding treatment.
7. The preparation method of the composite material of the mesoporous quantum photocatalytic material and the biological bacteria based on the limited-area oxygenation technology according to claim 1, wherein the mesoporous quantum photocatalytic material is formed by a micron porous framework-mesoporous photocatalytic material and has a two-stage fractal structure of micron pores and nanometer mesopores, and the specific surface area of the mesoporous quantum photocatalytic material is not less than 50m2A pore diameter of 0.1 to 3nm and a pore volume of not less than 0.1cm3The light absorption waveband is 200-1200 nm.
8. The preparation method of the composite material of the mesoporous quantum photocatalytic material and the biological bacteria based on the limited-area oxygenation technology according to claim 1, wherein the biological bacteria comprise aerobic biological bacteria and facultative biological bacteria, the aerobic biological bacteria adopt bacillus or/and nitrobacteria, and the facultative biological bacteria adopt denitrifying bacteria or/and nitrifying and denitrifying composite bacteria.
9. The preparation method of the composite material of the mesoporous quantum photocatalytic material and the biological bacteria based on the limited-area oxygenation technology according to claim 1, wherein the mass ratio of the biological bacteria to the mesoporous quantum photocatalytic material is 1-100: 1-100 ℃, the pH value of the use environment of the biological bacteria is controlled to be 6-9, the water temperature is controlled to be 5-35 ℃, the composite mode of the biological bacteria and the mesoporous quantum photocatalytic material is mechanical mixing and electrostatic adsorption, the electrostatic adsorption refers to adsorption of the mesoporous quantum photocatalytic material on the biological bacteria in a solvent, the adsorption time is not less than 0.1h, the temperature of the solvent is not less than 5 ℃, and the pH value of the solvent is not less than 1.
10. The preparation method of the composite material of the mesoporous quantum photocatalytic material and the biological bacteria based on the limited-area oxygenation technology according to claim 1, wherein the microorganism-mesoporous quantum photocatalyst is loaded on the surface of the fiber substrate by an immersion method or a spraying method, the loading amount of the microorganism-mesoporous quantum photocatalyst on the surface of the fiber substrate is 0.1-10 g/g, and the fiber is at least one selected from polyester cotton, nylon, terylene, polypropylene and acrylic fiber.
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| CN115518642B (en) * | 2022-10-10 | 2024-02-09 | 辽宁华泰环保科技集团有限公司 | Composite catalyst for treating high-concentration organic wastewater and preparation method and application method thereof |
| CN116371393A (en) * | 2023-04-19 | 2023-07-04 | 重庆华谱信息技术有限公司 | Method for efficiently sterilizing and degrading organic pollutants |
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