CN112973646B - Carbon-coated nanosphere for water quality purification and preparation method thereof - Google Patents
Carbon-coated nanosphere for water quality purification and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a carbon-coated nanosphere for water quality purification and a preparation method thereof, wherein the nanosphere comprises four layers of structures, the pore diameter of each layer of material structure is from small to large, the inner core layer is porous active carbon, the surface layer of the active 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 the powder structures are used for ball milling and coating to form a stable structure which is mutually inlaid and coated. The nanosphere material prepared by the method can rapidly decompose organic pollutants in aquaculture water, improve water quality and increase 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 a carbon-coated nanosphere for water quality purification and a preparation method thereof.
Background
Along with the rapid development of aquaculture, the pollution of aquaculture water is increasingly serious, thereby causing the deterioration of the ecological environment of the water, the ecological balance of the water is destroyed, 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 the damaged ecological system to normal natural conditions, various methods and techniques for treating the water environment have been developed in recent years, and the biological purification technique has the advantages of rapid improvement of water quality, maintenance of ecological balance of the water, low cost, short period, quick response and the like, and is favored by people, so that the biological purification technique becomes a main water quality purification method.
The biological purification is a purification method for realizing odorless and harmless treatment by absorbing, decomposing and utilizing harmful substances as nutrients by microorganisms using the metabolic activities of the microorganisms and oxidizing the harmful substances to the final product. However, this method has the following problems when applied to the water purification treatment: firstly, indigenous microorganisms only degrade carbon pollutants effectively, and have little effect on nitrogen pollutants, and as the indigenous microorganisms in the pond have limited capability of decomposing organic pollutants in the culture water, microbial preparations are required to be put into the water body of the pond, but the current strains are too single and cannot meet the requirements of the culture environment, and the multi-strain multifunctional compound microbial preparation is required to be developed. Secondly, although the advantages of the immobilized microorganism technology are more, 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 can not achieve large-scale production yet. Thirdly, the development of beneficial bacteria has the problems of poor stability after processing treatment, easy inactivation of bacteria, easy reduction of efficacy and the like.
Nanotechnology is a new technology which appears in recent years, is successfully applied to a plurality of fields including medicine, pharmacy, chemical and biological detection, manufacturing industry and the like, is closely related to work and daily life of people, but is applied to the field of aquaculture, and is a problem to be solved urgently in the aquaculture industry because of the development of a water quality treatment method taking nano materials as a main body based on the wide application prospect of the nanotechnology.
Disclosure of Invention
Aiming at the problems, the invention aims to provide the carbon-coated nanospheres for purifying water quality and the preparation method thereof, and the nanosphere material prepared by the method can rapidly decompose organic pollutants of aquaculture water, improve water quality and increase yield and quality of aquatic products.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the carbon coated nanosphere for water quality purification is characterized by comprising spheres with four layers, wherein the pore diameter of each layer of substance structure is from small to large, the inner core layer is porous active carbon, the surface layer of the active 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 ball milling coating is carried out between the layers by using a powder structure to form a stable structure which is mutually inlaid and coated.
The preparation method of the carbon-coated nanospheres is characterized by comprising the following specific process steps:
1. the method comprises the steps of placing activated carbon powder with the diameter of 0.01-0.1um, zeolite powder with the diameter of 0.01-0.1um, composite powder of ferrous oxalate, potassium manganate, cuprous oxalate and zinc oxalate and polyethylene powder with the molecular weight of 100-200 ten thousand in a vacuum heat treatment furnace at the temperature of 800-1200 ℃ for sintering treatment for 5-10h. Wherein the mass ratio of the active carbon to the zeolite powder to the iron-manganese-copper-zinc composite powder to the polyethylene is 50-60:5-10:10-20:5-10, wherein the mass ratio of the ferrous oxalate, the potassium manganate, the cuprous oxalate and 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, and simultaneously high molecular weight polyethylene is thermally melted to form polymerized carbide, and active carbon, zeolite powder and metal oxide particles are embedded to form a eutectic.
2. Performing three-stage ball milling and crushing on the composite powder material subjected to the heat treatment by adopting 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 5-10um, the ball milling time is 15-20h, and the rotating speed is 2000-5000r/min; the diameter of zircon balls used in the second-stage ball milling is 1-5um, the ball milling time is 5-10h, and the rotating speed is 2000-5000r/min; the diameter of zircon balls used in the third-stage ball milling is 0.1-0.5um, the ball milling time is 5-10h, the rotating speed is 2000-5000r/min, and the diameter of the balls of the zeolite coated composite metal powder and the activated carbon obtained after crushing is 0.05-0.1um.
3. 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 of the second step, and the mass ratio of the titanium dioxide to the active carbon coated by the zeolite powder to the iron-manganese-copper-zinc composite powder is 0.5-1:7-8, wherein the titanium dioxide coating thickness is 0.005-0.02um, and the carbon-coated nanospheres are obtained.
Compared with the prior art, the invention has the advantages that:
1. the carbon-coated nanospheres have good biocompatibility, the maximum cell adsorption capacity can reach 1000-1500mg/g, the specific surface area is relatively large, the specific surface area is about 1000-2000m < 2 >/g, and the stability is strong.
2. The carbon-coated nanospheres have four layers of powder coating structures with different apertures, pores with different sizes are formed in the surfaces and the interiors, the pore volume is 0.1-2mL/g, the carbon-coated nanospheres not only have an adsorption function, but also can perform ion exchange, and the carried nano materials can rapidly regulate and control the water environment after entering the culture water.
3. After the carbon-coated nanospheres are applied to a culture water body, the maximum dissolved oxygen content in the water can be increased by 40 parts, and the maximum removal rates of ammonia nitrogen (NH 4-N), nitrite nitrogen (NO 2-), chemical Oxygen Demand (COD), total phosphorus (T-P) and Suspended Substances (SS) respectively reach 85 parts, 52 parts, 90 parts, 75 parts and 80 parts.
4. By hydration, microelements such as iron, manganese, copper, zinc and the like released by the carbon-coated nanospheres in the water treatment process can promote the growth of beneficial microorganisms (such as nitrifying bacteria, photosynthetic bacteria, bacillus subtilis, actinomycetes, lactobacillus, saccharomycetes, streptococcus and the like) and algae in the water body, and the beneficial microorganism can increase dissolved oxygen, reduce ammonia nitrogen and inhibit the growth of pathogenic bacteria. The invention combines the nano material water quality purifying technology with the microorganism water quality regulating technology, so that the ecological balance of the water environment is greatly improved, and finally the purposes of purifying and regulating the water quality are achieved.
Detailed Description
The preparation process of the present invention is described below in connection with specific embodiments.
Embodiment one:
the preparation method of the carbon-coated nanospheres for water quality 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, and placing the mixture in a vacuum heat treatment furnace at 800 ℃ for sintering treatment for 5 hours.
After the heat treatment, the inorganic metal salt is thermally decomposed to obtain metal oxide particles, and simultaneously, the high molecular weight polyethylene is thermally melted to form polymerized carbide, and the active carbon, the zeolite powder and the metal oxide particles are embedded to form a eutectic.
And step two, performing three-stage ball milling and crushing on the composite powder material subjected to the heat treatment in the step one by adopting ball milling nano powder equipment, wherein a ball milling medium adopts zircon balls.
Zircon balls with the diameter of 5um are adopted for the first-stage ball milling, the ball milling time is 15 hours, and the rotating speed is 2000r/min; the second-stage ball milling adopts zircon balls with the diameter of 1um, the ball milling time is 5 hours, and the rotating speed is 2000r/min; 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 ball diameter of the zeolite coated composite metal powder and the activated carbon obtained after crushing is 0.05um.
Ball milling is carried out on titanium dioxide powder with the diameter of 0.01um and the ball powder obtained in the step two, 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 obtained in the step two is 0.5:7, the titanium dioxide coating thickness is 0.005um, and the carbon-coated nanospheres are obtained.
Embodiment two:
the preparation method of the carbon-coated nanospheres for water quality 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 35:8:25:15.
mixing activated 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, and placing the mixture in a vacuum heat treatment furnace at the temperature of 1000 ℃ for sintering treatment for 8 hours.
After the heat treatment, the inorganic metal salt is thermally decomposed to obtain metal oxide particles, and simultaneously, the high molecular weight polyethylene is thermally melted to form polymerized carbide, and the active carbon, the zeolite powder and the metal oxide particles are embedded to form a eutectic.
And step two, performing three-stage ball milling and crushing on the composite powder material subjected to the 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 3500r/min; the second-stage ball milling adopts zircon balls with the diameter of 3um, the ball milling time is 8 hours, and the rotating speed is 3500r/min; the third stage ball milling adopts zircon balls with the diameter of 0.3um, the ball milling time is 8 hours, the rotating speed is 3500r/min, and the ball diameter of the zeolite coated composite metal powder and the activated carbon obtained after crushing is 0.08um.
Ball milling is carried out on titanium dioxide powder with the diameter of 0.05um and the ball powder obtained in the step two, 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 obtained in the step two is 0.8:7.5, the titanium dioxide coating thickness is 0.01um, and the carbon-coated nanospheres are obtained.
Embodiment III:
the preparation method of the carbon-coated nanospheres for water quality 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 40:10:30:20.
mixing activated 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 proportion of 60:10:20:10, and placing the mixture in a vacuum heat treatment furnace at a temperature of 1200 ℃ for sintering treatment for 10 hours.
After the heat treatment, the inorganic metal salt is thermally decomposed to obtain metal oxide particles, and simultaneously, the high molecular weight polyethylene is thermally melted to form polymerized carbide, and the active carbon, the zeolite powder and the metal oxide particles are embedded to form a eutectic.
And step two, performing three-stage ball milling and crushing on the composite powder material subjected to the 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 5000r/min; the second-stage ball milling adopts zircon balls with the diameter of 5um, the ball milling time is 10 hours, and the rotating speed is 5000r/min; 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 ball diameter of the zeolite coated composite metal powder and the activated carbon obtained after crushing is 0.1um.
Ball milling is carried out on titanium dioxide powder with the diameter of 0.1um and the ball powder obtained in the step two, 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 obtained in the step two is 1: and 8, the titanium dioxide coating thickness is 0.02um, so that the carbon-coated nanospheres are obtained.
The carbon-coated nanospheres prepared in the above examples were subjected to field tests with existing conventional microbial treatment materials, and specific parameters of the two tests after comparison are shown in the following table:
the data in the table show that the specific surface area of the carbon-coated nanospheres is larger than that of the existing microbial materials, the cycle use times are more, and the pressure resistance in water is stronger. 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 the existing microorganism water treatment materials. Through hydration, the carbon-coated nanospheres can release microelements such as iron, manganese, copper, zinc and the like which promote beneficial microorganisms and algae in a water body to grow in the water treatment process, and the beneficial microorganism thalli can further increase dissolved oxygen, reduce ammonia nitrogen and inhibit growth of pathogenic bacteria, so that the carbon-coated nanospheres have more remarkable effect and more excellent indexes compared with the effect of purely adopting microorganism materials to treat the water quality in purifying the water quality and improving the ecological balance of the water environment, thereby realizing the water quality regulation purpose of aquaculture water areas.
Claims (4)
1. The carbon-coated nanospheres for water quality purification are characterized by comprising spheres with four layers of structures, wherein the pore diameter of each layer of material structure is from small to large, the inner core layer is porous active carbon, the surface layer of the active 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 the titanium dioxide layer adopts a powder structure to carry out ball milling coating to form a mutually inlaid and coated stable structure; the preparation method of the carbon-coated nanospheres comprises the following steps:
1. mixing activated carbon powder with the diameter of 0.01-0.1 mu m with zeolite powder with the diameter of 0.01-0.1 mu m, ferrous oxalate, potassium manganate, cuprous oxalate and zinc oxalate composite powder, and polyethylene powder with the molecular weight of 100-200 ten thousand, sintering in a vacuum heat treatment furnace, wherein the sintering temperature in the vacuum heat treatment furnace is 800-1200 ℃; wherein the mass ratio of the active carbon to the zeolite powder to the iron-manganese-copper-zinc composite powder to the polyethylene is 50-60:5-10:10-20:5-10, wherein the mass ratio of ferrous oxalate, potassium manganate, cuprous oxalate and zinc oxalate in the iron-manganese-copper-zinc composite powder is 30-40:5-10:20-30:10-20 parts of a base; after heat treatment, inorganic metal salt is thermally decomposed to obtain metal oxide particles, and simultaneously high molecular weight polyethylene is thermally melted to form polymerized carbide, and active carbon, zeolite powder and metal oxide particles are embedded to form a eutectic;
2. performing three-stage ball milling and crushing on the composite powder material subjected to the heat treatment by adopting ball milling nanometer powder equipment, wherein a ball milling medium adopts zircon balls, the diameter of the zircon balls used in the first stage of ball milling is 5-10 mu m, the diameter of the zircon balls used in the second stage of ball milling is 1-5 mu m, the diameter of the zircon balls used in the third stage of ball milling is 0.1-0.5 mu m, and the diameters of the spherical bodies of the zeolite coated composite metal powder and the activated carbon obtained after crushing are 0.05-0.1 mu m;
3. ball milling is carried out on titanium dioxide powder with the diameter of 0.01-0.1 mu m and the spherical powder obtained in the second step, and the mass ratio of the titanium dioxide to the active carbon coated by the zeolite powder to the iron-manganese-copper-zinc composite powder is 0.5-1:7-8, wherein the titanium dioxide coating thickness is 0.005-0.02 mu m, and the carbon-coated nanospheres are obtained.
2. The carbon-coated nanosphere for water purification according to claim 1, wherein the sintering treatment time in the step one vacuum heat treatment furnace is 5 to 10 hours.
3. The carbon-coated nanosphere for water purification according to claim 2, wherein the first stage ball milling time in the second step is 15-20 hours and the rotational speed is 2000-5000r/min; the second-stage ball milling time is 5-10h, and the rotating speed is 2000-5000r/min; the third ball milling time is 5-10h, and the rotating speed is 2000-5000 r/min.
4. The carbon-coated nanosphere for water purification as recited in claim 3, wherein the ball milling process in step three is the same as that in step two.
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| CN110316785B (en) * | 2019-07-19 | 2022-02-11 | 深圳市深港产学研环保工程技术股份有限公司 | Water body repairing agent for controlling cyanobacterial bloom, preparation method thereof and eutrophic water body repairing method |
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| CN109231492A (en) * | 2018-07-30 | 2019-01-18 | 湖南领道农业环保科技有限公司 | A kind of livestock and poultry farm saprobia cleanser and preparation method thereof |
| CN109364940A (en) * | 2018-11-15 | 2019-02-22 | 湖南大学 | Charcoal loads ferrimanganic bimetallic oxide light Fenton composite material and preparation method |
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