CN112201465A - Preparation method of modified biological magnetic fluid for desulfurization wastewater treatment - Google Patents
Preparation method of modified biological magnetic fluid for desulfurization wastewater treatment Download PDFInfo
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- CN112201465A CN112201465A CN202011078692.3A CN202011078692A CN112201465A CN 112201465 A CN112201465 A CN 112201465A CN 202011078692 A CN202011078692 A CN 202011078692A CN 112201465 A CN112201465 A CN 112201465A
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- desulfurization wastewater
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- 239000011553 magnetic fluid Substances 0.000 title claims abstract description 40
- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 33
- 230000023556 desulfurization Effects 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000004065 wastewater treatment Methods 0.000 title claims abstract description 18
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000006247 magnetic powder Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000919 ceramic Substances 0.000 claims abstract description 12
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 11
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 11
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012620 biological material Substances 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 5
- 238000007885 magnetic separation Methods 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 25
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- -1 polybutylene succinate Polymers 0.000 claims description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims description 4
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003508 Dilauryl thiodipropionate Substances 0.000 claims description 3
- 108010020346 Polyglutamic Acid Proteins 0.000 claims description 3
- 239000000084 colloidal system Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 235000019304 dilauryl thiodipropionate Nutrition 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229920002961 polybutylene succinate Polymers 0.000 claims description 3
- 239000004631 polybutylene succinate Substances 0.000 claims description 3
- 229920002643 polyglutamic acid Polymers 0.000 claims description 3
- 238000003892 spreading Methods 0.000 claims description 3
- 238000005201 scrubbing Methods 0.000 claims description 2
- 229910000859 α-Fe Inorganic materials 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims 1
- 239000002351 wastewater Substances 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 10
- 238000000926 separation method Methods 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 8
- 238000005189 flocculation Methods 0.000 abstract description 8
- 230000016615 flocculation Effects 0.000 abstract description 8
- 230000005389 magnetism Effects 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 13
- 229910052742 iron Inorganic materials 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 229910052602 gypsum Inorganic materials 0.000 description 2
- 239000010440 gypsum Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 241000233866 Fungi Species 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
-
- 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
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
- H01F1/445—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a compound, e.g. Fe3O4
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/18—Nature of the water, waste water, sewage or sludge to be treated from the purification of gaseous effluents
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physical Water Treatments (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention discloses a preparation method of modified biological magnetic fluid for desulfurization wastewater treatment, which is prepared by modifying a high-molecular biological material, a ceramic colloidal material and an antioxidant in a combined manner, and comprises the step of preparing Fe by methane reduction3O4Magnet and production of Fe3O4Preparing modified biological magnetic powder at high temperature by using magnetic powder, performing high-magnetic separation and ball milling, and preparing the water-based modified biological magnetic fluid. The modified biological magnetic fluid prepared by the invention keeps better high magnetism and high density performance in the desulfurization wastewater, is more uniformly distributed and has stronger flocculation separation capacity, thereby reducing the concentration of pollutants such as salinity, heavy metal, suspended matters and the like in the desulfurization wastewater and improving the quality of gypsumThe method has the advantages of basic guarantee, establishment of a foundation for zero discharge of the wastewater of the whole plant, and good environmental benefit and social benefit.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method of a modified biological magnetic fluid for desulfurization wastewater treatment.
Background
The biological magnetic fluid has basic properties of high magnetism, high density, large specific surface area, uniform distribution and the like, and is widely researched and applied in various separation fields. With the continuous development of biological magnetic fluid in the field of wastewater treatment, the biological magnetic fluid wastewater treatment flocculation technology has the advantages of high separation efficiency, high settling speed, large specific surface area, low water production turbidity and the like, and has been preliminarily researched and demonstrated in the field of high-efficiency flocculation treatment of desulfurization wastewater of power plants. The biological magnetic fluid which has been researched at present is generally formed by sintering plant bodies with higher iron content. At present, Chinese patent CN106504844A entitled "method for preparing biological magnetic fluid" developed a method for preparing biological magnetic fluid, which mainly uses black fungus and other plants with high iron content to prepare, but after the biological magnetic fluid prepared by the method is subjected to contact reaction after being oxidized, a large amount of iron ions in the plants are oxidized to generate ferric oxide, so that the magnetism of the plants is lost, and the flocculation separation function is lost. Therefore, the development of a novel, antioxidant and modified biological magnetic fluid preparation method is urgently needed, so that the method is suitable for the application of efficient flocculation treatment of desulfurization wastewater.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a modified biological magnetic fluid for desulfurization wastewater treatment, so as to solve the problem that a large amount of iron ions in the biological magnetic fluid prepared by plant bodies are easily oxidized to lose flocculation separation capacity, and provide an antioxidant modified biological magnetic fluid.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows.
The preparation method of the modified biological magnetic fluid for desulfurization wastewater treatment comprises the following steps:
s1 reduction of methane to prepare Fe3O4Magnet body
High-purity micro-powder alpha-Fe2O3Spreading in ceramic plate, placing ceramic plate in reduction reactor, introducing gas to completely displace the air in the reactor, slowly introducing methane gas, heating at constant temperature for 1-2 hr, stopping, and displacing methane in the reactor with gasGas, finally taking out Fe3O4Magnet and cooling to room temperature;
s2 preparation of Fe3O4Magnetic powder
Mixing Fe prepared in step S13O4The magnet is grinded into Fe by a small and medium-sized ball mill3O4Magnetic powder;
s3 preparation of modified biomagnetic powder at high temperature
Taking Fe prepared in step S23O440-50 parts of magnetic powder, 25-30 parts of high molecular biological material, 20-25 parts of polyglutamic acid, 5-10 parts of nano ceramic colloid and 3-5 parts of antioxidant, and the mixture is transferred into a high-temperature furnace to be combusted in a closed constant temperature manner for 1-2 hours, and then taken out and cooled to room temperature;
s4 high magnetic separation and ball milling
Separating the modified biomagnetic powder prepared in the step S3 under the action of an external magnetic field, grinding the separated large-particle powder into powder of 100 meshes and 200 meshes by a small and medium-sized ball mill, and fully mixing;
s5 preparation of water-based modified biological magnetic fluid
Dispersing the modified biological magnetic powder in secondary deionized water, and carrying out ultrasonic crushing on the water-based magnetic powder in an ultrasonic crusher to obtain the stably dispersed water-based modified biological magnetic fluid.
Further optimizing the technical scheme that in the step S1, high-purity micro-powder alpha-Fe is obtained2O3The thickness of (A) is 2-3 mm.
In a further optimized technical scheme, the first gas in the step S1 is high-purity carbon dioxide gas with the purity of 99.99%.
The technical scheme is further optimized, wherein the methane in the step S1 is methane gas subjected to scrubbing treatment, the gas inlet flow rate of the methane gas is 0.5-1.0mL/min, and the heating temperature is controlled at 350 ℃.
Further optimizing the technical scheme, in the step S2, the rotating speed of the ball mill is 3-5r/min, and the fineness of the magnetic powder is 100-200 meshes.
According to the further optimized technical scheme, the high molecular biological material in the step S3 comprises polybutylene succinate, and the antioxidant comprises dilauryl thiodipropionate; the temperature in the high temperature furnace was controlled at 500 ℃ and the mixture was shaken every 20 min.
The technical scheme is further optimized, the external magnetic field in the step S4 is an external magnetic field of 2000-2200 gauss, the large-particle powder is powder with the diameter larger than 0.5mm, and the rotating speed of the small and medium-sized ball mill is controlled to be 5-8 r/min.
Further optimizing the technical scheme, in the step S5, the liquid level of the secondary deionized water is controlled to be 10cm above the magnetic powder, the ultrasonic crusher is an ultrasonic crusher with the power of 1000W, and the crushing time is 10-15 min.
Due to the adoption of the technical scheme, the technical progress of the invention is as follows.
The modified biological magnetic fluid for treating the desulfurization wastewater is prepared by modifying a high-molecular biological material, a ceramic colloidal material and an antioxidant, so that the modified biological magnetic fluid is more uniformly distributed in the desulfurization wastewater, better high magnetism and high density performance are kept, and the flocculation separation capability is stronger. After the biological magnetic fluid prepared by the method contacts desulfurization wastewater, better magnetism and separation effect can be kept; the method is suitable for coagulation clarification treatment of the desulfurization wastewater after ultralow emission modification of flue gas desulfurization, and effectively solves the problems of low input rate, high turbidity of produced water, system blockage, overlarge deposition amount and the like of a desulfurization wastewater treatment system, thereby providing basic guarantee for reducing the concentration of pollutants such as salinity, heavy metals, suspended matters and the like in the desulfurization wastewater and improving the quality of gypsum, laying a foundation for implementation of zero emission of wastewater in a whole plant, and having good environmental benefit and social benefit.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
The preparation method of the modified biological magnetic fluid for treating the desulfurization wastewater comprises the step of preparing Fe by reducing methane3O4Magnet and production of Fe3O4The method comprises the following steps of preparing modified biological magnetic powder from magnetic powder at high temperature, performing high-magnetic separation and ball milling, and preparing water-based modified biological magnetic fluid, and specifically comprises the following steps:
s1 reduction of methane to prepare Fe3O4Magnet body
High-purity micro-powder alpha-Fe2O3Spreading in ceramic plate to control high-purity micro-powder alpha-Fe2O3The thickness of the flat laying is 2-3 mm; putting the ceramic disc into a reduction reactor, introducing 99.99% high-purity carbon dioxide gas to completely displace the air in the reactor, slowly feeding methane gas subjected to gas washing treatment, heating at constant temperature, controlling the gas inlet flow rate of the methane gas to be 0.5-1.0mL/min, and controlling the heating temperature to be 350 ℃; stopping feeding methane gas and heating after 1-2h, replacing methane gas in the reactor with 99.99% high-purity carbon dioxide gas, and taking out Fe3O4Magnet and cool to room temperature.
S2 preparation of Fe3O4Magnetic powder
Mixing Fe prepared in step S13O4The magnet is grinded into Fe with the magnetic powder fineness of 100-3O4Magnetic powder, and the rotating speed of the ball mill is controlled to be 3-5r/min during grinding.
S3 preparation of modified biomagnetic powder at high temperature
Taking Fe prepared in step S23O440-50 parts of magnetic powder, 25-30 parts of high molecular biological material, 20-25 parts of polyglutamic acid, 5-10 parts of nano ceramic colloid and 3-5 parts of antioxidant, fully mixing, transferring into a high-temperature furnace for closed constant-temperature combustion, controlling the temperature in the high-temperature furnace to be 500 ℃, shaking the mixture once every 20min, and taking out and cooling to room temperature after 1-2 hours. Wherein the high molecular biological material is poly butylene succinate, and the antioxidant is dilauryl thiodipropionate.
S4 high magnetic separation and ball milling
Separating the modified biomagnetic powder prepared in the step S3 into large-particle powder with the diameter larger than 0.5mm under the action of an external magnetic field of 2000-2200 Gauss, polishing the separated large-particle powder by a small-medium ball mill, controlling the rotating speed of the small-medium ball mill to be 5-8r/min, polishing the powder into 100-mesh powder of 200 meshes, and fully mixing the powder.
S5 preparation of water-based modified biological magnetic fluid
Dispersing the modified biological magnetic powder in secondary deionized water, controlling the liquid level of the secondary deionized water to be 10cm above the magnetic powder, and carrying out ultrasonic crushing on the water-based magnetic powder in an ultrasonic crusher with the power of 1000W for 10-15min to obtain the stably dispersed water-based modified biological magnetic fluid.
The modified biological magnetic fluid for treating the desulfurization wastewater is prepared by modifying a high-molecular biological material, a ceramic colloidal material and an antioxidant, so that the modified biological magnetic fluid is more uniformly distributed in the desulfurization wastewater, better high magnetism and high density performance are kept, and the flocculation separation capability is stronger. After the biological magnetic fluid prepared by the method contacts desulfurization wastewater, better magnetism and separation effect can be kept; the method is suitable for coagulation clarification treatment of the desulfurization wastewater after ultralow emission modification of flue gas desulfurization, and effectively solves the problems of low input rate, high turbidity of produced water, system blockage, overlarge deposition amount and the like of a desulfurization wastewater treatment system, thereby providing basic guarantee for reducing the concentration of pollutants such as salinity, heavy metals, suspended matters and the like in the desulfurization wastewater and improving the quality of gypsum, laying a foundation for implementation of zero emission of wastewater in a whole plant, and having good environmental benefit and social benefit.
Claims (8)
1. The preparation method of the modified biological magnetic fluid for desulfurization wastewater treatment is characterized by comprising the following steps:
s1 reduction of methane to prepare Fe3O4Magnet body
High-purity micro-powder alpha-Fe2O3Spreading in ceramic plate, placing ceramic plate in reduction reactor, introducing gas to completely displace the air in the reactor, slowly introducing methane gas, heating at constant temperature for 1-2 hr, displacing the methane gas in the reactor with the gas, and taking out Fe3O4Magnet and cooling to room temperature;
s2 preparation of Fe3O4Magnetic powder
Mixing Fe prepared in step S13O4The magnet is grinded into Fe by a small and medium-sized ball mill3O4Magnetic powder；
S3 preparation of modified biomagnetic powder at high temperature
Taking Fe prepared in step S23O440-50 parts of magnetic powder, 25-30 parts of high molecular biological material, 20-25 parts of polyglutamic acid, 5-10 parts of nano ceramic colloid and 3-5 parts of antioxidant, and the mixture is transferred into a high-temperature furnace to be combusted in a closed constant temperature manner for 1-2 hours, and then taken out and cooled to room temperature;
s4 high magnetic separation and ball milling
Separating the modified biomagnetic powder prepared in the step S3 under the action of an external magnetic field, grinding the separated large-particle powder into powder of 100 meshes and 200 meshes by a small and medium-sized ball mill, and fully mixing;
s5 preparation of water-based modified biological magnetic fluid
Dispersing the modified biological magnetic powder in secondary deionized water, and carrying out ultrasonic crushing on the water-based magnetic powder in an ultrasonic crusher to obtain the stably dispersed water-based modified biological magnetic fluid.
2. The preparation method of the modified biological magnetic fluid for desulfurization wastewater treatment according to claim 1, characterized by comprising the following steps: high purity fine powder of alpha-Fe in step S12O3The thickness of (A) is 2-3 mm.
3. The preparation method of the modified biological magnetic fluid for desulfurization wastewater treatment according to claim 1, characterized by comprising the following steps: the first gas in the step S1 is high purity carbon dioxide gas of 99.99%.
4. The preparation method of the modified biological magnetic fluid for desulfurization wastewater treatment according to claim 1, characterized by comprising the following steps: the methane in the step S1 is methane gas subjected to scrubbing treatment, the gas inlet flow rate of the methane gas is 0.5-1.0mL/min, and the heating temperature is controlled at 350 ℃.
5. The preparation method of the modified biological magnetic fluid for desulfurization wastewater treatment according to claim 1, characterized by comprising the following steps: in the step S2, the rotating speed of the ball mill is 3-5r/min, and the fineness of the magnetic powder is 100-200 meshes.
6. The preparation method of the modified biological magnetic fluid for desulfurization wastewater treatment according to claim 1, characterized by comprising the following steps: the polymer biomaterial in the step S3 comprises polybutylene succinate, and the antioxidant comprises dilauryl thiodipropionate; the temperature in the high temperature furnace was controlled at 500 ℃ and the mixture was shaken every 20 min.
7. The preparation method of the modified biological magnetic fluid for desulfurization wastewater treatment according to claim 1, characterized by comprising the following steps: the external magnetic field in the step S4 is 2000-2200 gauss, the large-particle powder is powder with the diameter larger than 0.5mm, and the rotating speed of the small and medium-sized ball mill is controlled to be 5-8 r/min.
8. The preparation method of the modified biological magnetic fluid for desulfurization wastewater treatment according to claim 1, characterized by comprising the following steps: and in the step S5, the liquid level of the secondary deionized water is controlled to be 10cm above the magnetic powder, the ultrasonic crusher is an ultrasonic crusher with the power of 1000W, and the crushing time is 10-15 min.
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2020
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