CN110776095B - Preparation method of composite magnetic particles based on alnico - Google Patents
Preparation method of composite magnetic particles based on alnico 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
- C02F3/28—Anaerobic digestion processes
- C02F3/2806—Anaerobic processes using solid supports for microorganisms
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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
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/481—Treatment of water, waste water, or sewage with magnetic or electric fields using permanent magnets
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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
- C02F2003/001—Biological treatment of water, waste water, or sewage using granular carriers or supports for the microorganisms
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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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Abstract
A preparation method of composite magnetic particles based on alnico belongs to the technical field of wastewater treatment materials and comprises the following steps of (1) screening alnico magnetic powder and ferroferric oxide powder through a screen respectively, and then drying the powder in an oven at 80-100 ℃ for later use; (2) mixing the raw material obtained in the step (1) and a coupling agent in absolute ethyl alcohol and uniformly stirring; (3) uniformly mixing the dry powder mixture obtained in the step (2) with an adhesive, and extruding the mixture into raw material balls under a spherical die with the inner diameter of 1-4 mm; (4) soaking the raw material balls obtained in the step (3) in a coating agent for coating; (5) and (5) drying the raw material balls obtained in the step (4) in an oven at the temperature of 60-80 ℃ to obtain finished products.
Description
The patent application is a divisional application of a patent application with the application date of 2017, 2 and 21, and the application number of 201710092221.X, and the invention and creation name of 'an alnico-based composite magnetic particle and a preparation method thereof'.
Technical Field
The invention belongs to the technical field of wastewater treatment materials, and relates to a preparation method of composite magnetic particles based on alnico.
Background
The traditional biological wastewater denitrification treatment technology usually adopts an AO (anaerobic-aerobic) or AAO (anaerobic-anoxic-aerobic) process, and nitrogen is removed from a water body finally through an ammoniation reaction, a nitration reaction and a denitrification reaction. The ammoniation reaction can be carried out under anaerobic or aerobic conditions, the nitration reaction can be carried out under aerobic conditions, and the denitrification reaction can be carried out under anaerobic conditions. In order to ensure the nitrogen removal effect, the nitrification reaction and the denitrification reaction are usually carried out in different reactors, the nitrification process needs aeration to ensure sufficient dissolved oxygen, the denitrification process needs to add a carbon source to ensure a carbon-nitrogen ratio, the operation cost of the denitrification process is increased through the links of aeration and carbon source addition, and the occupied area of the traditional biological denitrification process is larger.
The principle of the autotrophic nitrogen removal process is that ammonia oxidizing bacteria convert ammonia nitrogen into nitrite nitrogen by using a small amount of dissolved oxygen in water, and then anaerobic ammonia oxidizing bacteria perform anaerobic ammonia oxidation reaction by using the nitrite nitrogen and the ammonia nitrogen to generate nitrogen so as to remove nitrogen from the water. Compared with the traditional AO and AAO processes, the autotrophic nitrogen removal process can be completed in the same reactor, no additional carbon source is needed, and the demand on dissolved oxygen is low, so that the occupied area can be greatly reduced, and the operation cost can be reduced. In the autotrophic denitrification process, the anaerobic ammonia oxidation reaction is a key link influencing the denitrification efficiency of the reactor, and the generation period of anaerobic ammonia oxidation bacteria is long, and enrichment is difficult, so that the autotrophic denitrification process is slow to develop.
Research proves that the atoms composing the enzyme present paramagnetic characteristics under most conditions, and the enzyme activity can be indirectly influenced by the action of a magnetic field on the paramagnetic atoms. The magnetic field can effectively improve the activity of the anaerobic ammonium oxidation bacteria in the autotrophic denitrification reactor, and is beneficial to the rapid enrichment of the anaerobic ammonium oxidation bacteria.
In the 'biological effect test for magnetizing treated sewage' published in 'environmental science and technology' by Wangxiang Sanqi et al 2000, the magnetic field is found to promote the increase of the number of mitochondria in aerobic respiration places, so that the microbial activity is also improved. Korean Qingxiang, which is published in 2002 of "strengthening effect of magnetic field on wastewater treatment by activated sludge process" in the proceedings of the Fushun Petroleum institute, states that the activity of kinase can be improved when the magnetic field strength is less than 0.05T, and the wastewater treatment efficiency is also improved by 11%. Wangqiang indicated that the removal rate of nitrate nitrogen is improved by 7.2% when the external magnetic field strength is 150mT and the activity of dehydrogenase is also improved by 2.38 times in the biological denitrification mechanism and efficiency of magnetically enhanced aerobic denitrifying bacteria in the doctor's academic paper of the university of Harbin industry in 2010; when the magnetic field intensity is 30-90 mT, the removal of ammonia nitrogen is promoted, and when the magnetic field intensity is 60mT, the ammonia nitrogen removal effect is optimal. The above results are all researched by adopting an external magnetic field mode, but the magnetic field intensity of the external magnetic field in water is rapidly attenuated along with the increase of the distance from a magnetic field source, and the uniform distribution of the magnetic field intensity in the reactor is difficult to ensure.
In order to solve the problem of uneven distribution of the magnetic field, the 'action mechanism of magnetic effect on sewage treatment by an activated sludge process and application thereof' published in 'resource conservation and environmental protection' of Dakolin, et al 2010 proposes a mode of adding magnetic powder into sewage to improve the distribution of the magnetic field. According to the description, the dehydrogenase activity increases when the amount of added magnetic powder is increased from 0.0g to 1.5g, and if the increase of the dehydrogenase activity is increased based on the increase of the amount of added magnetic powder, the increase is slightly decreased.
In conclusion, the magnetic field is applied to the reactor, so that the activity of the anaerobic ammonia oxidizing bacteria in the reactor is improved, and the ammonia nitrogen treatment efficiency of the reactor is improved; the manner in which the magnetic field source is applied within the reactor helps to improve the uniformity of the magnetic field strength distribution within the reactor. However, in the mode of directly adding magnetic powder into the reactor, the magnetic powder is easy to run off along with the drainage process of the reactor in the actual operation process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a composite magnetic particle to overcome the problems of nonuniform magnetic field distribution, easy loss of magnetic powder and the like of a magnetic induction autotrophic nitrogen removal reactor in the prior art.
The composite magnetic particle based on the alnico comprises, by weight, 78% -88% of alnico magnetic powder, 5% -17% of ferroferric oxide powder, 1% -2% of an adhesive and 2% -4% of a coupling agent, wherein the particle size of the particle is 1-4 mm.
Preferably, the particles are coated on the outside, and the thickness of the coating is not more than 0.5 mm.
The adhesive is a mixture of polyvinyl alcohol and sodium alginate, and the mixing weight ratio of the polyvinyl alcohol: sodium alginate is equal to 5: 3.
the coupling agent is silane KH 550.
The coupling agent is an aluminate.
A preparation method of alnico-based composite magnetic particles comprises the following steps:
(1) screening alnico magnetic powder by a screen mesh, wherein the specification of the screen mesh is between 200 meshes and 400 meshes, drying the powder in an oven at 80-100 ℃ for later use, screening ferroferric oxide powder by a screen mesh, wherein the specification of the screen mesh is between 200 meshes and 400 meshes, and drying the powder in the oven at 80-100 ℃ for later use;
(2) mixing the dried alnico magnetic powder obtained in the step (1), the dried ferroferric oxide powder and the coupling agent in the anhydrous ethanol according to the following weight percentage, uniformly stirring, standing for 20-40min, drying in an oven at 80-100 ℃, and taking the dried powder for later use; the weight percentage is as follows: 80-92% of dry alnico magnetic powder, 6-17% of dry ferroferric oxide and 2-5% of coupling agent;
(3) mixing the dry powder mixture obtained in the step (2) with a binder according to the following weight percentage: 84-90% of the dry powder mixture and 10-16% of the adhesive solution, uniformly mixing, and extruding under a spherical mold with an internal aperture of 1-4mm to form raw material balls;
(4) and (4) drying the raw material balls obtained in the step (3) in an oven at the temperature of 60-80 ℃ to obtain finished products.
Preferably, the raw material ball obtained in the step (3) is soaked in a coating agent, coated for 5-15min under the conditions of ultrasonic frequency of 35 kHz and ultrasonic intensity of 0.6W/m L, and the thickness of the coating layer is not more than 0.5mm, and then the step (4) is carried out.
Preferably, the adhesive solution is a mixture of a 5% polyvinyl alcohol aqueous solution and a 3% sodium alginate aqueous solution in a volume ratio of 1: 1 in a liquid mixture.
Preferably, the coupling agent is silane KH 550.
Preferably, the coupling agent is an aluminate.
Preferably, the coating agent comprises, by weight, 18% of dry polyvinylidene fluoride (PVDF), 72% of dimethylacetamide and 10% of a pore-forming agent NaCl.
The composite magnetic particle based on the alnico provided by the invention has moderate particle size and small density, and can be suspended in a reaction device under a certain hydraulic condition. The method can be applied to an autotrophic denitrification reactor, is beneficial to improving the activity of anaerobic ammonium oxidation bacteria in the reactor, is beneficial to the attachment and growth of microorganisms in the reactor, reduces the loss of the microorganisms, improves the biomass in the reactor, and is also beneficial to the quick start of an autotrophic denitrification reaction system. The magnetic particles are added into a wastewater treatment device, and can be in a suspended state along with hydraulic stirring in the reactor, so that the uniform distribution of the magnetic field in the reactor is facilitated, and the problems of weak magnetic field intensity, nonuniform magnetic field distribution and slow formation of granular sludge in the magnetic biological coupling technology are solved. The magnetic particles have good settling property and are not easy to run off along with the drainage of the reactor.
According to the composite magnetic particle prepared by the preparation method of the alnico-based composite magnetic particle, the magnetic powder and the adhesive are taken as main raw materials, and a layer of coating agent is coated after the magnetic particle raw material balls are prepared, so that the raw material balls are prevented from agglomerating, and a certain anticorrosion effect is achieved. The coating agent contains a pore-forming agent, and the large specific surface area of the coated particles has better adsorption effect on pollutants in wastewater, so that the enrichment of microorganisms on the surfaces of the particles is facilitated, and the formation of granular sludge is accelerated. The magnetic particles perform long-term stable magnetic stimulation on microorganisms in the reactor, and the large specific surface area provides more attachment points for the microorganisms and serves as an inner core of granular sludge, so that the formation of the granular sludge is accelerated, and the pollutant removal efficiency is improved. The preparation method of the alnico-based composite magnetic particles provided by the invention has the advantages that high-temperature firing is not needed, the preparation method is simple and easy, energy is saved, and the requirement on processing equipment is lower.
Detailed Description
The present invention will be described in detail with reference to examples.
The first embodiment is as follows:
the composite magnetic particle based on the alnico comprises 78% of alnico magnetic powder, 17% of ferroferric oxide powder, 2% of an adhesive, 3% of silane KH550, 1mm of particle size, a coating layer outside the particle, 0.1mm of the coating layer, a mixture of polyvinyl alcohol and sodium alginate as the adhesive, and polyvinyl alcohol in a mixing weight ratio: sodium alginate is equal to 5: 3.
example two:
the alnico-based composite magnetic particle comprises, by weight, 88% of alnico magnetic powder, 7% of ferroferric oxide powder, 1% of a binder and 4% of aluminate, wherein the particle size of the particle is 4mm, a coating layer is arranged outside the particle, the thickness of the coating layer is 0.5mm, the binder is a mixture of polyvinyl alcohol and sodium alginate, and the weight ratio of the polyvinyl alcohol to the sodium alginate is as follows: sodium alginate is equal to 5: 3.
example three:
a preparation method of alnico-based composite magnetic particles comprises the following steps:
(1) sieving alnico magnetic powder with a 400-mesh sieve, placing the powder in an oven to be dried at 100 ℃ for later use, sieving ferroferric oxide powder with a 400-mesh sieve, and placing the powder in the oven to be dried at 100 ℃ for later use;
(2) mixing the dried alnico magnetic powder obtained in the step (1), the dried ferroferric oxide powder and silane KH550 in the following weight percentage in absolute ethyl alcohol, uniformly stirring, standing for 30min, drying in an oven at 100 ℃, and taking the dried powder for later use; the weight percentage is as follows: 80% of dry alnico magnetic powder, 15% of dry ferroferric oxide and 5% of silane KH 550;
(3) mixing the dry powder mixture obtained in the step (2) with a binder according to the following weight percentage: after the dry powder mixture accounts for 84 percent and the adhesive solution accounts for 16 percent, uniformly mixing, extruding the mixture into raw material balls under a die with a ball shape arranged inside, wherein the particle size of the raw material balls is 1 mm; the adhesive solution is prepared from a 5% polyvinyl alcohol aqueous solution and a 3% sodium alginate aqueous solution according to the volume ratio of 1: 1;
(4) and (3) soaking the coating agent in the step (3), coating for 10min under the conditions of ultrasonic frequency of 35 kHz and ultrasonic intensity of 0.6W/m L, wherein the thickness of the coating layer is 0.3mm, and then drying the coating agent in an oven at the temperature of 60 ℃, wherein the coating agent comprises 18% of dried polyvinylidene fluoride (PVDF), 72% of dimethylacetamide and 10% of pore-forming agent NaCl in percentage by weight.
The alnico-based composite magnetic particles prepared in the first example were filled in a reactor in an amount of 20g/L, and a magnetic field strength of 0.78mT could be formed. Magnetic particles by countingAfter the activated sludge is added for 1 day, the total number of heterotrophic bacteria reaches 8 multiplied by 105Each.ml-1。
Example four:
a preparation method of alnico-based composite magnetic particles comprises the following steps:
(1) sieving the alnico magnetic powder with a 200-mesh sieve, placing the powder in an oven to be dried for later use at 90 ℃, sieving the ferroferric oxide powder with a 400-mesh sieve, and placing the powder in the oven to be dried for later use at 90 ℃;
(2) mixing the dried alnico magnetic powder obtained in the step (1), the dried ferroferric oxide powder and the aluminate in the following weight percentage in absolute ethyl alcohol, uniformly stirring, standing for 30min, drying in an oven at 90 ℃, and taking the dried powder for later use; the weight percentage is as follows: 90% of dry alnico magnetic powder, 6% of dry ferroferric oxide and 4% of aluminate;
(3) mixing the dry powder mixture obtained in the step (2) with a binder according to the following weight percentage: the dry powder mixture accounts for 88 percent, the adhesive solution accounts for 12 percent, and after being uniformly mixed, the mixture is extruded into raw material balls under a die with a ball shape arranged inside, and the particle size of the raw material balls is 2 mm; the adhesive solution is prepared from a 5% polyvinyl alcohol aqueous solution and a 3% sodium alginate aqueous solution according to the volume ratio of 1: 1;
(4) and (3) soaking the coating agent in the step (3), coating for 8min under the conditions of ultrasonic frequency of 35 kHz and ultrasonic intensity of 0.6W/m L, wherein the thickness of the coating layer is 0.2mm, and then drying the coating agent in an oven at the temperature of 60 ℃, wherein the coating agent comprises 18% of dried polyvinylidene fluoride (PVDF), 72% of dimethylacetamide and 10% of pore-forming agent NaCl in percentage by weight.
The composite magnetic particles prepared in the above examples were filled in a reactor in an amount of 20g/L, and a magnetic field strength of 0.8mT was achieved. The total number of heterotrophic bacteria reaches 8.5 multiplied by 10 after the magnetic particles are added into the activated sludge for 1d measured by a counting method5Each.ml-1。
Claims (4)
1. A preparation method of composite magnetic particles based on alnico is characterized by comprising the following steps:
(1) screening alnico magnetic powder by a screen mesh, wherein the specification of the screen mesh is between 200 meshes and 400 meshes, drying the powder in an oven at 80-100 ℃ for later use, screening ferroferric oxide powder by a screen mesh, wherein the specification of the screen mesh is between 200 meshes and 400 meshes, and drying the powder in the oven at 80-100 ℃ for later use;
(2) mixing the dried alnico magnetic powder obtained in the step (1), the dried ferroferric oxide powder and the coupling agent in the anhydrous ethanol according to the following weight percentage, uniformly stirring, standing for 20-40min, drying in an oven at 80-100 ℃, and taking the dried powder for later use; the weight percentage is as follows: 80-92% of dry alnico magnetic powder, 6-17% of dry ferroferric oxide and 2-5% of coupling agent;
(3) mixing the dry powder mixture obtained in the step (2) with a binder according to the following weight percentage: 84-90% of the dry powder mixture and 10-16% of the adhesive solution, uniformly mixing, and extruding under a spherical mold with an internal aperture of 1-4mm to form raw material balls;
(4) soaking the raw material balls obtained in the step (3) in a coating agent, and coating for 5-15min under the conditions of ultrasonic frequency of 35 kHz and ultrasonic intensity of 0.6W/m L, wherein the thickness of the coating layer is not more than 0.5 mm; the coating agent comprises 18% of dry polyvinylidene fluoride (PVDF), 72% of dimethylacetamide and 10% of pore-forming agent NaCl in percentage by weight;
(5) and (5) drying the raw material balls obtained in the step (4) in an oven at the temperature of 60-80 ℃ to obtain finished products.
2. The method of claim 1, wherein the binder solution is a 5% polyvinyl alcohol aqueous solution and a 3% sodium alginate aqueous solution at a volume ratio of 1: 1 in a liquid mixture.
3. The method of claim 2, wherein the coupling agent is silane KH 550.
4. The method of claim 2, wherein the coupling agent is an aluminate.
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