CN112973646A - Carbon-coated nanosphere for water purification and preparation method thereof - Google Patents
Carbon-coated nanosphere for water purification and preparation method thereof Download PDFInfo
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- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
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- 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
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- B01J20/28054—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 surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
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- 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
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- B01J20/28054—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 surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/06—Nutrients for stimulating the growth of microorganisms
Abstract
The invention discloses a carbon-coated nanosphere for water purification and a preparation method thereof, wherein the nanosphere comprises a four-layer structure, the pore diameter of each layer of the material structure is from small to large, an inner core layer is porous activated carbon, iron-manganese-copper-zinc nano composite powder is compounded on the surface layer of the activated carbon, an intermediate layer is a zeolite layer, and the outermost layer is a titanium dioxide layer, and each layer is ball-milled and coated by a powder-shaped structure to form a stable structure which is embedded and coated with each other. The nano-sphere material prepared by the method can rapidly decompose organic pollutants in aquaculture water, improve water quality and improve yield and quality of aquatic products.
Description
Technical Field
The invention relates to a water quality adjusting and treating technology in the field of aquaculture, in particular to carbon-coated nanospheres for water quality purification and a preparation method thereof.
Background
With the rapid development of aquaculture, the pollution of aquaculture water is increasingly serious, so that the ecological environment of the water is worsened, the ecological balance of the water is damaged, the problem of water diseases is more serious, and available water resources are less and less. In order to restore the structure and function of damaged ecosystem to normal natural state, people have developed various methods and techniques for treating water environment in recent years, and the biological purification technique has the advantages of fast water quality improvement, water ecological balance maintenance, low cost, short period, fast effect and the like, so that the biological purification technique is favored by people and becomes a main water quality purification method.
Biological purification is a purification method in which harmful substances are absorbed, decomposed and utilized as nutrients by microorganisms using metabolic activities of the microorganisms, and oxidized into final products to remove the harmful substances, thereby realizing deodorization and harmlessness. However, the method is applied to the process of water purification treatment, and has the following problems: firstly, it is effective that the indigenous microorganism only degrades carbon series pollutant, and the effect to nitrogen series pollutant is not big, because the indigenous microorganism in the pond is limited to the decomposition capacity of aquaculture aquatic organic pollutant, consequently need put into microbial preparation in the pond water, but present bacterial is too single, can not satisfy the requirement of aquaculture environment, is waited to develop the multi-functional compound microbial preparation of many bacterial strains. Secondly, although the immobilized microorganism technology has more advantages, the technology is still in an indoor simulation stage at present mainly because the cost of the carrier is too high, the carrier has resistance to the diffusion of the matrix and the product, and the manufacturing process cannot achieve large-scale production. Thirdly, the research and the preparation of beneficial bacteria have the problems of poor stability after processing, easy inactivation of bacteria, easy reduction of efficacy and the like.
Nanotechnology is a high and new technology appearing in recent years, and the technology is successfully used in many fields, including medicine, pharmacy, chemistry, biological detection, manufacturing industry and the like, and is closely related to the work and daily life of people, but the technology is less applied in the field of aquaculture at present, and a method for treating water quality by taking a nanometer material as a main body is developed based on the wide application prospect of the nanotechnology, so that the technology becomes a problem to be solved urgently in the aquaculture industry.
Disclosure of Invention
In view of the above problems, the present invention aims to provide carbon-coated nanospheres for water purification and a preparation method thereof, wherein the nanospheres prepared by the method of the present invention can rapidly decompose organic pollutants in aquaculture water, improve water quality, and increase yield and quality of aquatic products.
In order to achieve the purpose, the invention adopts the following technical scheme:
a carbon-coated nanosphere for water purification is characterized by comprising a sphere with a four-layer structure, wherein the pore diameter of each layer of the structure is from small to large, an inner core layer is porous activated carbon, the surface layer of the activated carbon is compounded with iron-manganese-copper-zinc nano composite powder, an intermediate layer is a zeolite layer, the outermost layer is a titanium dioxide layer, and each layer is ball-milled and coated by a powder structure to form a stable structure which is embedded and coated mutually.
The preparation method of the carbon-coated nanosphere is characterized by comprising the following specific process steps of:
firstly, putting activated carbon powder with the diameter of 0.01-0.1um, zeolite powder with the diameter of 0.01-0.1um, ferrous oxalate, potassium manganate, cuprous oxalate, zinc oxalate composite powder and polyethylene powder with the molecular weight of 100 plus one 200 ten thousand into a vacuum heat treatment furnace for sintering treatment for 5-10h at the temperature of 800 plus one 1200 ℃. Wherein the mass ratio of the active carbon, the zeolite powder, the iron-manganese-copper-zinc composite powder and the polyethylene is 50-60: 5-10: 10-20: 5-10, wherein the mass ratio of the ferrous oxalate to the potassium manganate to the cuprous oxalate to the zinc oxalate composite powder is 30-40: 5-10: 20-30: 10-20. After heat treatment, inorganic metal salt is thermally decomposed to obtain metal oxide particles, high molecular weight polyethylene is thermally melted to form polymeric carbide, and the active carbon, zeolite powder and metal oxide particles are embedded to form a eutectic body.
Performing three-stage ball milling crushing on the heat-treated composite powder material by using ball milling nano powder equipment, wherein a ball milling medium adopts zircon balls, the diameter of the zircon balls used in the first-stage ball milling is 5-10 mu m, the ball milling time is 15-20h, and the rotating speed is 2000-5000 r/min; the diameter of the zircon ball used for the second-stage ball milling is 1-5um, the ball milling time is 5-10h, and the rotating speed is 2000-5000 r/min; the diameter of the zircon ball used for the third-stage ball milling is 0.1-0.5um, the ball milling time is 5-10h, the rotating speed is 2000-.
Thirdly, ball milling is carried out on titanium dioxide powder with the diameter of 0.01-0.1um and the spherical powder obtained in the second step, the ball milling process is the same as that in the second step, and the mass ratio of the titanium dioxide to the zeolite powder coated active carbon to the iron-manganese-copper-zinc composite powder is 0.5-1: 7-8, and the coating thickness of the titanium dioxide is 0.005-0.02um, thus obtaining the carbon-coated nanosphere.
Compared with the prior art, the invention has the advantages that:
1. the carbon-coated nanosphere has good biocompatibility, the maximum cell adsorption capacity can reach 1000-1500mg/g, the carbon-coated nanosphere has a larger specific surface area of about 1000-2000m2/g, and the carbon-coated nanosphere has strong stability.
2. The carbon-coated nanosphere has a four-layer powder coating structure with different apertures, pores with different sizes are formed on the surface and in the carbon-coated nanosphere, the pore volume is 0.1-2mL/g, the carbon-coated nanosphere not only has an adsorption function, but also can perform ion exchange, and the water environment can be quickly regulated and controlled after the carried nanomaterial enters the culture water body.
3. After the carbon-coated nanospheres are applied to the culture water body, the maximum dissolved oxygen in water can be increased by 40 parts, and the removal rates of ammonia nitrogen (NH 4-N), nitrite nitrogen (NO 2-), Chemical Oxygen Demand (COD), total phosphorus (T-P) and suspended matters (SS) respectively reach 85 parts, 52 parts, 90 parts, 75 parts and 80 parts.
4. Through hydration, in the water treatment process, microelements such as iron, manganese, copper and zinc released in the carbon-coated nanospheres can promote the growth of beneficial microorganisms (such as nitrobacteria, photosynthetic bacteria, bacillus subtilis, actinomycetes, lactic acid bacteria, saccharomycetes, streptococcus and the like) and algae in the water body, and the beneficial microorganisms can increase dissolved oxygen, reduce ammonia nitrogen and inhibit the growth of pathogenic bacteria. The invention combines the water quality purifying technology of nano materials with the water quality adjusting technology of microorganisms, greatly improves the ecological balance of water environment, and finally achieves the purposes of purifying and adjusting water quality.
Detailed Description
The preparation process of the present invention will be described below with reference to specific embodiments.
The first embodiment is as follows:
a preparation method of carbon-coated nanospheres for water purification comprises the following steps:
step one, in the step, the mixing proportion of the ferrous oxalate, the potassium manganate, the cuprous oxalate and the zinc oxalate composite powder is 30: 5: 20: 10.
mixing activated carbon powder with the diameter of 0.01um, zeolite powder with the diameter of 0.01um, mixed iron-manganese-copper-zinc composite powder and polyethylene powder with the molecular weight of 100 ten thousand according to the weight ratio of 50: 5: 10: 5, placing the mixture in a vacuum heat treatment furnace at 800 ℃ and sintering the mixture for 5 hours.
After the heat treatment, inorganic metal salt is thermally decomposed to obtain metal oxide particles, high molecular weight polyethylene is thermally melted to form polymeric carbide, and the activated carbon, zeolite powder and metal oxide particles are embedded to form a eutectic body.
And step two, performing three-stage ball milling crushing on the composite powder material subjected to heat treatment in the step one by adopting ball milling nano powder equipment, wherein a ball milling medium adopts zircon balls.
The first-stage ball milling adopts zircon balls with the diameter of 5um, the ball milling time is 15h, and the rotating speed is 2000 r/min; the second-stage ball milling adopts zircon balls with the diameter of 1um, the ball milling time is 5h, and the rotating speed is 2000 r/min; and the third-stage ball milling adopts zircon balls with the diameter of 0.1um, the ball milling time is 5 hours, the rotating speed is 2000r/min, and the diameter of the balls of the zeolite-coated composite metal powder and the activated carbon obtained after crushing is 0.05 um.
Step three, carrying out ball milling on titanium dioxide powder with the diameter of 0.01um and the sphere powder obtained in the step two, wherein the ball milling process is the same as that of the step two, and the mass ratio of the titanium dioxide powder to the spheres subjected to ball milling in the step two is 0.5: 7, coating the titanium dioxide with the thickness of 0.005um to obtain the carbon-coated nanosphere.
Example two:
a preparation method of carbon-coated nanospheres for water purification comprises the following steps:
step one, in the step, the mixing ratio of the ferrous oxalate, the potassium manganate, the cuprous oxalate and the zinc oxalate composite powder is 35: 8: 25: 15.
mixing active carbon powder with the diameter of 0.05um, zeolite powder with the diameter of 0.05um, mixed iron-manganese-copper-zinc composite powder and polyethylene powder with the molecular weight of 150 ten thousand according to the weight ratio of 55: 8: 15: 8, placing the mixture in a vacuum heat treatment furnace at 1000 ℃ and sintering for 8 hours.
After the heat treatment, inorganic metal salt is thermally decomposed to obtain metal oxide particles, high molecular weight polyethylene is thermally melted to form polymeric carbide, and the activated carbon, zeolite powder and metal oxide particles are embedded to form a eutectic body.
And step two, performing three-stage ball milling crushing on the composite powder material subjected to heat treatment in the step one by adopting ball milling nano powder equipment, wherein a ball milling medium adopts zircon balls.
The first-stage ball milling adopts zircon balls with the diameter of 8um, the ball milling time is 19h, and the rotating speed is 3500 r/min; the second-stage ball milling adopts zircon balls with the diameter of 3um, the ball milling time is 8h, and the rotating speed is 3500 r/min; and the third-stage ball milling adopts zircon balls with the diameter of 0.3um, the ball milling time is 8h, the rotating speed is 3500r/min, and the diameter of the balls of the zeolite-coated composite metal powder and the activated carbon obtained after crushing is 0.08 um.
Step three, carrying out ball milling on titanium dioxide powder with the diameter of 0.05um and the sphere powder obtained in the step two, wherein the ball milling process is the same as that of the step two, and the mass ratio of the titanium dioxide powder to the spheres subjected to ball milling in the step two is 0.8: 7.5, the coating thickness of the titanium dioxide is 0.01um, and the carbon-coated nanosphere is obtained.
Example three:
a preparation method of carbon-coated nanospheres for water purification comprises the following steps:
step one, in the step, the mixing ratio of the ferrous oxalate, the potassium manganate, the cuprous oxalate and the zinc oxalate composite powder is 40: 10: 30: 20.
mixing active carbon powder with the diameter of 0.1um, zeolite powder with the diameter of 0.1um, mixed iron-manganese-copper-zinc composite powder and polyethylene powder with the molecular weight of 200 ten thousand according to the weight ratio of 60: 10: 20: 10, placing the mixture in a temperature of 1200 ℃, and sintering the mixture in a vacuum heat treatment furnace for 10 hours.
After the heat treatment, inorganic metal salt is thermally decomposed to obtain metal oxide particles, high molecular weight polyethylene is thermally melted to form polymeric carbide, and the activated carbon, zeolite powder and metal oxide particles are embedded to form a eutectic body.
And step two, performing three-stage ball milling crushing on the composite powder material subjected to heat treatment in the step one by adopting ball milling nano powder equipment, wherein a ball milling medium adopts zircon balls.
The first-stage ball milling adopts zircon balls with the diameter of 10um, the ball milling time is 20 hours, and the rotating speed is 5000 r/min; the second-stage ball milling adopts zircon balls with the diameter of 5um, the ball milling time is 10h, and the rotating speed is 5000 r/min; and the third-stage ball milling adopts zircon balls with the diameter of 0.5um, the ball milling time is 10 hours, the rotating speed is 5000r/min, and the diameter of the balls of the zeolite-coated composite metal powder and the activated carbon obtained after crushing is 0.1 um.
Step three, carrying out ball milling on titanium dioxide powder with the diameter of 0.1um and the ball powder obtained in the step two, wherein the ball milling process is the same as that of the step two, and the mass ratio of the titanium dioxide powder to the ball milled in the step two is 1: 8, coating the titanium dioxide with the thickness of 0.02um to obtain the carbon-coated nanosphere.
The carbon-coated nanospheres prepared in the above examples were tested on site with conventional microbial treatment materials, and the specific parameters of the tests are shown in the following table after comparison:
the data in the table show that the carbon-coated nanospheres have a specific surface area larger than that of the existing microbial material, are more recyclable and have stronger pressure resistance when placed in a water body. Other data such as ammonia nitrogen removal rate, chemical oxygen demand removal rate, total phosphorus removal rate and suspended matter removal rate are superior to those of the existing microbial water body treatment material. Through hydration, in the water treatment process, the carbon-coated nanospheres can release trace elements such as iron, manganese, copper and zinc which promote the growth of beneficial microorganisms and algae in the water body, and the beneficial microorganisms can further increase dissolved oxygen, reduce ammonia nitrogen and inhibit the growth of pathogenic bacteria, so that the carbon-coated nanospheres have the effects of purifying water quality and improving water environment ecological balance.
Claims (5)
1. The carbon-coated nanosphere for water purification is characterized by comprising a sphere with a four-layer structure, wherein the pore diameter of each layer of the structure is from small to large, the inner core layer is porous activated carbon, the surface layer of the activated carbon is compounded with iron-manganese-copper-zinc nano composite powder, the middle layer is a zeolite layer, the outermost layer is a titanium dioxide layer, and each layer is ball-milled and coated by a powder structure to form a stable structure which is embedded and coated mutually.
2. The method for preparing carbon-coated nanospheres for water purification as claimed in claim 1, wherein the specific process steps are as follows:
firstly, sintering activated carbon powder with the diameter of 0.01-0.1um, zeolite powder with the diameter of 0.01-0.1um, ferrous oxalate, potassium manganate, cuprous oxalate, zinc oxalate composite powder and polyethylene powder with the molecular weight of 100 plus one 200 ten thousand in a vacuum heat treatment furnace; wherein the mass ratio of the active carbon, the zeolite powder, the iron-manganese-copper-zinc composite powder and the polyethylene is 50-60: 5-10: 10-20: 5-10, wherein the mass ratio of the ferrous oxalate to the potassium manganate to the cuprous oxalate to the zinc oxalate composite powder is 30-40: 5-10: 20-30: 10-20 parts of; after heat treatment, inorganic metal salt is thermally decomposed to obtain metal oxide particles, high molecular weight polyethylene is thermally melted to form polymeric carbide, and the active carbon, zeolite powder and the metal oxide particles are embedded to form a eutectic body;
secondly, performing three-stage ball milling crushing on the heat-treated composite powder material by using ball milling nano powder equipment, wherein a ball milling medium adopts zircon balls, the diameter of the zircon balls used for the first-stage ball milling is 5-10um, the diameter of the zircon balls used for the second-stage ball milling is 1-5um, the diameter of the zircon balls used for the third-stage ball milling is 0.1-0.5um, and the diameter of the crushed zeolite-coated composite metal powder and activated carbon balls is 0.05-0.1 um;
thirdly, ball-milling titanium dioxide powder with the diameter of 0.01-0.1um and the spherical powder obtained in the second step, wherein the mass ratio of the titanium dioxide to the zeolite powder coated active carbon to the iron-manganese-copper-zinc composite powder is (0.5-1): 7-8, and the coating thickness of the titanium dioxide is 0.005-0.02um, thus obtaining the carbon-coated nanosphere.
3. The method for preparing carbon-coated nanospheres for water purification as claimed in claim 2, wherein the sintering temperature in the vacuum heat treatment furnace in the step one is 800-1200 ℃ and the sintering time is 5-10 h.
4. The method for preparing carbon-coated nanospheres for water purification as claimed in claim 2, wherein the time of the first-stage ball milling in the second step is 15-20h, and the rotation speed is 2000-; the time of the second-stage ball milling is 5-10h, and the rotating speed is 2000-; the time of the third-stage ball milling is 5-10h, and the rotating speed is 2000-.
5. The method of preparing carbon-coated nanospheres for water purification as claimed in claim 2, wherein the ball milling process in step three is the same as that in step two.
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