CN113149211A - High-mechanical-strength magnetic MBBR filler and preparation method thereof - Google Patents
High-mechanical-strength magnetic MBBR filler and preparation method thereof 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
- C02F3/30—Aerobic and anaerobic processes
- C02F3/302—Nitrification and denitrification treatment
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Abstract
The invention belongs to the technical field of high polymer materials and water treatment, and discloses a high-mechanical-strength magnetic MBBR filler which comprises 1-65 parts of a hydrophilic base material, 1-19 parts of a toughening material, 3-90 parts of magnetic particles, 10-55 parts of a density adjustment coating layer, 0-3.8 parts of a biological enzyme active agent, 0-7.5 parts of biological nutrient salt and 0.1-7 parts of other additives by mass; the magnetic particle solution is a mixed solution containing ferric salt and ferrous salt. The MBBR filler prepared by the invention has strong mechanical strength and strong adsorption performance due to the coupling effect of the resin on the base material, and effectively reduces the treatment cost on the basis of improving the comprehensive performance of the material by adding the magnetic material and adjusting the density.
Description
Technical Field
The invention relates to a water treatment suspended filler, in particular to a high-mechanical-strength MBBR filler containing magnetic particles and a preparation method thereof, belonging to the technical field of high polymer materials and water treatment.
Background
In recent years, with the stricter policy of national ecological environment protection and the increased attention of people on environmental protection and ecological improvement, the sewage treatment of China has more and more increased intensity, and various new technologies, new materials and new processes are more and more widely applied to the technical field of water treatment. The MBBR technology is a water treatment technology newly developed in recent years, can purify polluted water body through the metabolism of anaerobic microorganisms and aerobic microorganisms, and is an efficient and stable sewage treatment mode. The core of the MBBR is two interrelated biological enzymatic reactions of nitration and denitrification, and the key point of the process is the selection of the suspended filler, and the hydrophilicity and the biological affinity of the suspended filler directly influence the effect of the biological enzymatic reactions; also, suspended fillers are generally the same or similar in density to water, and their durability and loss of filler directly impact the cost of the process.
Through retrieval, the publication number CN104961227B discloses a modified polyurethane suspension filler, a preparation method and application thereof, the technical scheme discloses that the invention discloses a modified polyurethane suspension filler which is prepared from the following components in parts by weight: 10-80 parts of polyhydroxyalkanoate, 10-80 parts of activated carbon, 60-80 parts of polyurethane, 1-10 parts of water-soluble polyurethane solution, 0-10 parts of biological active agent, 0-1 part of inorganic metal salt, 0-20 parts of organic high polymer and 0-10 parts of inorganic flocculate. However, the filler prepared by the technical scheme has the following defects: the specific gravity of the filler can not be adjusted according to the quality of the inlet water and the mixing and stirring conditions so as to fully ensure that the filler is in a suspension state. The magnetic recovery can not be utilized, and the loss of the filter material along with the effluent is avoided.
The novel MBBR filler which has good hydrophilicity, high mechanical strength, difficult loss, environmental protection, no toxicity and easy degradation recently becomes a research hotspot.
Disclosure of Invention
The purpose of the invention is as follows: based on the prior art, an MBBR filler with high hydrophilicity, high mechanical strength and recoverable magnetism and a preparation method thereof are provided.
The technical scheme is as follows: a high mechanical strength magnetism MBBR packs characterized in that: the MBBR filler comprises, by mass, 1-65 parts of a hydrophilic base material, 1-19 parts of a toughening material, 3-90 parts of magnetic particles, 10-55 parts of a density adjustment coating layer, 0-3.8 parts of a biological enzyme active agent, 0-7.5 parts of biological nutrient salt and 0.1-7 parts of other additives; the magnetic particles are ferric iron salt and ferrous iron salt.
The invention further defines the technical scheme as follows: the hydrophilic base material comprises polyhydroxyalkanoate, one or more of butylene terephthalate, polyethylene oxide, polypropylene carbonate and polylactic acid, and one or more of glycerol, pentaerythritol and glycerol triacetate.
Preferably, the toughening agent comprises an inorganic modified resin material.
Preferably, the density-adjusting wrapping layer includes hollow glass beads.
Preferably, the biological enzyme active agent comprises at least two of iron salt, aluminum salt and magnesium salt, and the biological nutrient salt comprises at least two of chitosan, chitin and polyphosphate.
Preferably, the other auxiliary agents comprise one or more of an antioxidant, a coupling agent, a dispersing agent, ammonia water or alcohol.
The invention also provides a preparation method of the high-mechanical-strength magnetic MBBR filler, which is characterized by comprising the following steps: the method comprises the following steps:
(1) blending 15-75 parts by mass of polyhydroxyalkanoate, 3-25 parts by mass of one or more of butylene terephthalate, polyethylene oxide, polypropylene carbonate and polylactic acid, and 3-22 parts by mass of one or more of glycerol, pentaerythritol and glycerol triacetate to prepare a hydrophilic base material;
(2) mixing a hydrophilic base material blending material with a mass ratio of 1: 3-1: 30 with a mixed solution of a ferric salt and a ferrous salt to prepare a mixed solution containing magnetic particles; the mass ratio of the mixed solution of the ferric salt and the ferrous salt is 6: 1-8: 1;
(3) filtering and drying the mixed solution in the step (2), and reacting the filtered and dried mixed solution with ammonia water for 1-3 hours under the condition of water bath reflux at the temperature of 30-95 ℃; the mass concentration of the ammonia water is 5-20%.
(4) Adding a coupling agent and alcohol into the step (3), and stirring in a water bath at the temperature of 25-95 ℃ to react for 1-3 hours;
(5) filtering the mixed solution obtained in the step (4), sequentially adding a coupling agent, alcohol and ammonia water, and carrying out water bath stirring reaction for 1-3 hours at the temperature of 25-95 ℃; the materials are added in sequence, and each newly added material needs to be added after the last material reacts for 5-15 minutes;
(6) filtering, washing and drying the material in the step (5) to constant weight, putting the material into an extruder for mixing and extruding, and adding 10-55 parts by mass of a density adjusting wrapping layer raw material in the extruding process; the temperature of each extrusion interval of the extruder is set to be 105-120 ℃, 120-135 ℃, 135-150 ℃, 150-165 ℃, 165-180 ℃, 180-195 ℃ and 185-195 ℃ respectively;
(7) and (4) cutting the material extruded in the step (6) to obtain the MBBR filler.
The method further defines the technical scheme as follows: the coupling agent comprises at least two of vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (beta-methoxyethoxy) silane and tetraethyl silicate.
Has the advantages that: compared with the prior art, the invention has the following advantages:
1) compared with the maleic anhydride or modified materials thereof which are used only in the field, the toughening agent adopted by the invention can improve the toughness of the finished MBBR filler, ensure the interface strength, improve the physicochemical property of the surface of the MBBR filler through resin controllable preparation, and regulate and control the hydrophilicity and the biocompatibility. Provides necessary conditions for obtaining the composite material base material with excellent comprehensive performance.
2) According to the invention, the density-adjusting wrapping layer is prepared by the silane coupling agent, and the resin toughening agent is matched to synthesize and adjust the density of the filler, so that the problem of high density of the hydrophilic filler can be solved, and the interface strength of the silicon-based wrapping layer and the hydrophilic base layer can be effectively increased.
3) And the iron-based material is coupled on the surface of the hydrophilic base layer through the coupling agent, so that the recycling performance of the material is improved.
4) The MBBR filler prepared by the invention has strong mechanical strength and strong adsorption performance due to the coupling effect of the resin on the base material, and effectively reduces the treatment cost on the basis of improving the comprehensive performance of the material by adding the magnetic material and adjusting the density.
Detailed Description
The invention will be further elucidated with reference to specific examples 1 to 4.
Example 1
The embodiment provides a preparation method of a high-mechanical-strength magnetic MBBR filler, which comprises the following steps:
(1) 15 parts of polyhydroxyalkanoate, 3 parts of butylene terephthalate and 3 parts of glycerol are blended to prepare the hydrophilic base material blending material.
(2) Mixing a hydrophilic base material blending material with a mass ratio of 1:3 with a mixed solution of a ferric salt and a ferrous salt; the mass ratio of the mixed solution of the ferric salt and the ferrous salt is 6: 1.
(3) Filtering and drying the mixed solution in the step (2), and reacting the mixed solution with ammonia water for 1 hour under the condition of water bath reflux at the temperature of 65 ℃; the mass concentration of the ammonia water is 10%.
(4) And (3) adding vinyltriethoxysilane, vinyltrimethoxysilane and propanol into the mixture, and stirring the mixture in a water bath at the temperature of 55 ℃ for reacting for 1 hour.
(5) Filtering the mixed solution obtained in the step (4), and then sequentially adding vinyltriethoxysilane, vinyltrimethoxysilane, propanol and ammonia water to react for 1 hour in a water bath under the condition of 45 ℃; the sequential addition is such that each newly added material is added after the last material has reacted for 5 minutes.
(6) Filtering, washing and drying the material in the step (5) to constant weight, putting the material into an extruder, mixing and extruding the material, and adding 10 parts by mass of hollow glass beads, 2.5 parts by mass of magnesium oxide and 0.1 part by mass of ethanol in the extrusion process; the temperature of each extrusion interval of the extruder is respectively set to be 105 ℃, 120 ℃, 135 ℃, 150 ℃, 165 ℃, 180 ℃ and 185 ℃.
(7) And (4) cutting the extruded material in the step (6) to obtain the MBBR filler.
As shown in Table 1, the filler prepared by the above steps has significantly improved comprehensive properties compared with commercial MBBR filler, when the physical properties of the base material are measured by a national standard method.
Example 2
The embodiment provides a preparation method of a high-mechanical-strength magnetic MBBR filler, which comprises the following steps:
(1) blending 40 parts by mass of polyhydroxyalkanoate, 10 parts by mass of polybutylene terephthalate and 5 parts by mass of polylactic acid, 5 parts by mass of glycerol and 5 parts by mass of pentaerythritol, 3 parts by mass of chitosan and 3 parts by mass of chitin to prepare a hydrophilic base material blending material.
(2) Mixing a hydrophilic base material blending material with a mass ratio of 1:10 with a mixed solution of a ferric salt and a ferrous salt; the mass ratio of the mixed solution of the ferric salt and the ferrous salt is 7: 1.
(3) Filtering and drying the mixed solution in the step (2), and reacting with ammonia water for 2 hours under the condition of water bath reflux at 65 ℃; the mass concentration of the ammonia water is 20%.
(4) And (3) adding vinyltriethoxysilane, vinyltrimethoxysilane and ethanol into the mixture, and stirring the mixture in a water bath at the temperature of 65 ℃ for reacting for 2 hours.
(5) Filtering the mixed solution obtained in the step (4), and then adding vinyl triethoxysilane, vinyl trimethoxysilane, ethanol and ammonia water in sequence to react for 2 hours at the temperature of 55 ℃ in a water bath under stirring; the sequential addition is such that each newly added material is added after 10 minutes of reaction of the previous material.
(6) Filtering, washing and drying the material in the step (5) to constant weight, putting the material into an extruder, mixing and extruding the material, and adding 20 parts by mass of hollow glass beads, 2 parts by mass of ferric chloride, 1 part by mass of polyphosphate and 4 parts by mass of propanol in the extrusion process; the temperature of each extrusion interval of the extruder is respectively set to be 120 ℃, 135 ℃, 150 ℃, 165 ℃, 180 ℃ and 195 ℃.
(7) And (4) cutting the extruded material in the step (6) to obtain the MBBR filler.
As shown in Table 2, the physical properties of the base material were measured by the national standard method, and the filler prepared by the above steps had significantly improved overall properties compared with commercial MBBR filler.
Example 3
The embodiment provides a preparation method of a high-mechanical-strength magnetic MBBR filler, which comprises the following steps:
(1) 75 parts by mass of polyhydroxyalkanoate, 25 parts by mass of polylactic acid, 10 parts by mass of pentaerythritol and 3 parts by mass of glycerol triacetate are blended to prepare the hydrophilic base material blending material.
(2) Mixing a hydrophilic base material blending material with a mass ratio of 1:15 with a mixed solution of a ferric salt and a ferrous salt; the mass ratio of the mixed solution of the ferric salt and the ferrous salt is 7: 1.
(3) Filtering and drying the mixed solution in the step (2), and reacting the mixed solution with ammonia water for 1.5 hours under the condition of water bath reflux at the temperature of 95 ℃; the mass concentration of the ammonia water is 20%.
(4) And (3) adding vinyltri (beta-methoxyethoxy) silane, tetraethyl silicate and propanol into the mixture, and reacting the mixture in a water bath at the temperature of 85 ℃ for 2 hours by stirring.
(5) Filtering the mixed solution obtained in the step (4), and then sequentially adding vinyl tri (beta-methoxyethoxy) silane, tetraethyl silicate, propanol and ammonia water to perform water bath stirring reaction for 1 hour at the temperature of 75 ℃; the sequential addition is such that each newly added material is added after the last material has reacted for 5 minutes.
(6) Filtering, washing and drying the material in the step (5) to constant weight, putting the material into an extruder, mixing and extruding the material, and adding 30 parts by mass of hollow glass microspheres, 3.8 parts by mass of chitosan, 7.5 parts by mass of chitin, 7 parts by mass of magnesium oxide and 1.8 parts by mass of ethanol in the extrusion process; the temperature of each extrusion interval of the extruder is respectively set to be 110 ℃, 120 ℃, 150 ℃, 160 ℃, 180 ℃ and 195 ℃.
(7) And (4) cutting the extruded material in the step (6) to obtain the MBBR filler.
As shown in Table 3, the base material performance is measured by adopting an element analyzer and a contact angle measuring instrument, compared with a commercial MBBR filler, the filler prepared by the steps has the advantages of improved hydrophilic performance, less iron dissolution, good stability, certain adsorption capacity and contribution to pollutant adsorption and degradation.
Example 4
The embodiment provides a preparation method of a high-mechanical-strength magnetic MBBR filler, which comprises the following steps:
(1) 75 parts by mass of polyhydroxyalkanoate, 10 parts by mass of polyethylene oxide, 5 parts by mass of pentaerythritol and 5 parts by mass of glycerol triacetate are blended to prepare the hydrophilic base material blending material.
(2) Mixing a hydrophilic base material blending material with a mass ratio of 1:25 with a mixed solution of a ferric salt and a ferrous salt; the mass ratio of the mixed solution of the ferric salt and the ferrous salt is 6: 1.
(3) Filtering and drying the mixed solution in the step (2), and reacting with ammonia water for 3 hours under the condition of water bath reflux at 55 ℃; the mass concentration of the ammonia water is 10%.
(4) And (3) adding vinyltrimethoxysilane, vinyltris (beta-methoxyethoxy) silane and methanol into the mixture, and stirring the mixture in a water bath at the temperature of 55 ℃ for reacting for 3 hours.
(5) Filtering the mixed solution obtained in the step (4), and then sequentially adding vinyl trimethoxy silane, vinyl tri (beta-methoxy ethoxy) silane, methanol and ammonia water to react for 3 hours in a water bath under the condition of 75 ℃; the sequential addition is such that each newly added material is added after the last material has reacted for 5 minutes.
(6) Filtering, washing and drying the material in the step (5) to constant weight, putting the material into an extruder for mixing and extruding, and adding 10-55 parts by mass of hollow glass microspheres, 2.7 parts by mass of chitin, 1.1 parts by mass of magnesium oxide and 3.2 parts by mass of propanol in the extruding process; the temperature of each extrusion interval of the extruder is respectively set to be 110 ℃, 120 ℃, 150 ℃, 165 ℃, 180 ℃ and 190 ℃.
(7) And (4) cutting the extruded material in the step (6) to obtain the MBBR filler.
As shown in Table 4, the commercial MBBR filler and the filler prepared in the above steps are added into a commercial reactor, the same reaction conditions are adopted, and the water quality of effluent is detected by sampling, so that the result shows that the filler prepared in the above steps is obviously superior to the commercial filler in the film forming time and the effluent quality, and the good cost performance is shown.
TABLE 1
TABLE 2
TABLE 3
TABLE 4
The embodiments described above are presented to enable those skilled in the art to make and use the invention. It will be readily apparent to those skilled in the art that various modifications can be made to the embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should understand that they can make improvements and modifications within the scope of the present invention according to the disclosure of the present invention.
Claims (8)
1. A high mechanical strength magnetism MBBR packs characterized in that: the MBBR filler comprises, by mass, 1-65 parts of a hydrophilic base material, 1-19 parts of a toughening material, 3-90 parts of magnetic particles, 10-55 parts of a density adjustment coating layer, 0-3.8 parts of a biological enzyme active agent, 0-7.5 parts of biological nutrient salt and 0.1-7 parts of other additives; the magnetic particles are ferric salt and ferrous salt.
2. A high mechanical strength magnetic MBBR filler according to claim 1, wherein: the hydrophilic base material comprises polyhydroxyalkanoate, one or more of butylene terephthalate, polyethylene oxide, polypropylene carbonate and polylactic acid, and one or more of glycerol, pentaerythritol and glycerol triacetate.
3. A high mechanical strength magnetic MBBR filler according to claim 1, wherein: the toughening agent comprises an inorganic modified resin material.
4. A high mechanical strength magnetic MBBR filler according to claim 1, wherein: the density adjusting wrapping layer comprises hollow glass beads.
5. A high mechanical strength magnetic MBBR filler according to claim 1, wherein: the biological enzyme active agent comprises at least two of iron salt, aluminum salt and magnesium salt, and the biological nutrient salt comprises at least two of chitosan, chitin and polyphosphate.
6. A high mechanical strength magnetic MBBR filler according to claim 1, wherein: the other auxiliary agents comprise one or more of an antioxidant, a coupling agent, a dispersing agent, ammonia water or alcohol.
7. A preparation method of a magnetic MBBR filler with high mechanical strength is characterized by comprising the following steps: the method comprises the following steps:
(1) blending 15-75 parts by mass of polyhydroxyalkanoate, 3-25 parts by mass of one or more of butylene terephthalate, polyethylene oxide, polypropylene carbonate and polylactic acid, and 3-22 parts by mass of one or more of glycerol, pentaerythritol and glycerol triacetate to prepare a hydrophilic base material;
(2) mixing a hydrophilic base material blending material with a mass ratio of 1: 3-1: 30 with a mixed solution of a ferric salt and a ferrous salt to prepare a mixed solution containing magnetic particles; the mass ratio of the mixed solution of the ferric salt and the ferrous salt is 6: 1-8: 1;
(3) filtering and drying the mixed solution in the step (2), and reacting the filtered and dried mixed solution with ammonia water for 1-3 hours under the condition of water bath reflux at the temperature of 30-95 ℃; the mass concentration of the ammonia water is 5-20%.
(4) Adding a coupling agent and alcohol into the step (3), and stirring in a water bath at the temperature of 25-95 ℃ to react for 1-3 hours;
(5) filtering the mixed solution obtained in the step (4), sequentially adding a coupling agent, alcohol and ammonia water, and carrying out water bath stirring reaction for 1-3 hours at the temperature of 25-95 ℃; the materials are added in sequence, and each newly added material needs to be added after the last material reacts for 5-15 minutes;
(6) filtering, washing and drying the material in the step (5) to constant weight, putting the material into an extruder for mixing and extruding, and adding 10-55 parts by mass of a density adjusting wrapping layer raw material in the extruding process; the temperature of each extrusion interval of the extruder is set to be 105-120 ℃, 120-135 ℃, 135-150 ℃, 150-165 ℃, 165-180 ℃, 180-195 ℃ and 185-195 ℃ respectively;
(7) and (4) cutting the material extruded in the step (6) to obtain the MBBR filler.
8. The method of preparing a high mechanical strength magnetic MBBR filler according to claim 7, wherein: the coupling agent comprises at least two of vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (beta-methoxyethoxy) silane and tetraethyl silicate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116534999A (en) * | 2023-03-07 | 2023-08-04 | 中国科学院生态环境研究中心 | Enhanced removal process for nitrogen in industrial wastewater |
| CN117361750A (en) * | 2023-10-31 | 2024-01-09 | 漳州市善御水环保科技有限责任公司 | Magnetic hydrophilic MBBR filler and preparation method thereof |
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