CN113244879A - Application of iron phosphate microspheres in treatment of wastewater containing methylene blue - Google Patents
Application of iron phosphate microspheres in treatment of wastewater containing methylene blue Download PDFInfo
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- CN113244879A CN113244879A CN202110649084.1A CN202110649084A CN113244879A CN 113244879 A CN113244879 A CN 113244879A CN 202110649084 A CN202110649084 A CN 202110649084A CN 113244879 A CN113244879 A CN 113244879A
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- iron phosphate
- microspheres
- copper slag
- methylene blue
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- 239000004005 microsphere Substances 0.000 title claims abstract description 34
- 229910000398 iron phosphate Inorganic materials 0.000 title claims abstract description 30
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 title claims abstract description 30
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229960000907 methylthioninium chloride Drugs 0.000 title claims abstract description 16
- 239000002351 wastewater Substances 0.000 title claims abstract description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052802 copper Inorganic materials 0.000 claims abstract description 35
- 239000010949 copper Substances 0.000 claims abstract description 35
- 239000002893 slag Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 6
- 239000010452 phosphate Substances 0.000 claims abstract description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 6
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 17
- 229920002545 silicone oil Polymers 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 13
- 229910021538 borax Inorganic materials 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 10
- 239000004328 sodium tetraborate Substances 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 238000004062 sedimentation Methods 0.000 claims 1
- 239000003463 adsorbent Substances 0.000 abstract description 4
- 239000003086 colorant Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 238000003723 Smelting Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000005389 magnetism Effects 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 description 27
- 239000000523 sample Substances 0.000 description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical group [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 7
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 7
- 235000019837 monoammonium phosphate Nutrition 0.000 description 7
- 230000008901 benefit Effects 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000003208 petroleum Substances 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 230000035939 shock Effects 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 241000609240 Ambelania acida Species 0.000 description 1
- 235000017060 Arachis glabrata Nutrition 0.000 description 1
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- 229910017976 MgO 4 Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000010920 waste tyre Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0292—Phosphates of compounds other than those provided for in B01J20/048
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0248—Compounds of B, Al, Ga, In, Tl
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a new application of iron phosphate microspheres, namely the application of the iron phosphate microspheres in treating wastewater containing methylene blue; the iron phosphate microspheres are porous phosphate chemically-bonded material microspheres prepared by using smelting copper slag as a raw material, and are used for adsorbing and treating wastewater containing a coloring agent methylene blue, and experimental results show that the iron phosphate microspheres can effectively remove the methylene blue in a water body; and the adsorbent has certain magnetism, is easy to recover, can be repeatedly utilized, and cannot cause secondary pollution to the water body.
Description
Technical Field
The invention relates to the field of wastewater treatment containing a coloring agent and secondary utilization of solid waste, in particular to a technique for treating wastewater containing a coloring agent methylene blue.
Background
Along with the annual increase of the copper yield in China, the accumulated copper slag is more and more, and the task of recycling the copper slag is more difficult. According to the statistics of the statistical bureau of China, the copper yield in China in 2012 is 606 ten thousand tons, and the copper slag amount in China only in 2012 reaches thousands of tons according to the calculation of about 2.2 tons of copper slag generated by 1 ton of refined copper. So far, no economic and efficient comprehensive utilization technology for copper slag exists, and the copper slag is basically stockpiled and treated, occupies a large amount of land, and causes serious environmental pollution and resource waste. The content of iron in the copper slag is 20-25%, and the iron olivine (Fe) is mainly used2SiO4) And magnetite (Fe)3O4) The form of (2) exists, and the recovery of the iron element cannot be realized through the conventional mineral separation or smelting process. In addition, compared with slag, copper slag has lower activity and cannot be applied to the fields of cement and building materials on a large scale. How to realize the resource utilization of high-quantity valuable elements (Fe and Si) in the copper slag, the method has higher economic benefit and environmental benefit for improving the economic benefit of the copper industry, relieving the iron ore resource pressure of the sustainable development of the steel industry in China, and being beneficial to resource saving and environmental protection.
The adsorption technology is one of the most common methods for treating dye wastewater at present, and mainly utilizes a material with high specific surface area and a porous structure to adhere pollutants on an adsorbent through intermolecular interaction. Activated carbon is the most common adsorbent material, but its level of regeneration is low. The MOF and nano powder materials are synthesized and applied to dye wastewater treatment, have extremely high adsorption efficiency, but have high preparation cost, and cannot be popularized and utilized on a large scale. The research is focused on the development of cheaper and recyclable adsorbents, including clay minerals (montmorillonite, hematite, kaolinite, bentonite, etc.), industrial wastes (fly ash, waste tires, etc.), metal oxides or Layered Double Hydroxides (LDH), agricultural wastes (rice hulls, peanut shells, bagasse, etc.), etc. The preparation cost is low, but the stability of the adsorption performance is poor, and the cyclic utilization is difficult.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a new application of iron phosphate microspheres, namely an application of the iron phosphate microspheres in treatment of wastewater containing methylene blue.
The iron phosphate microspheres are prepared by adding phosphate and borax into copper slag powder and uniformly stirring; adding deionized water into the mixture, and uniformly stirring to obtain slurry; under the conditions of heating and stirring, the slurry is dripped into dimethyl silicone oil at the temperature of 70-80 ℃, the dripped liquid is rapidly solidified into small balls at the temperature of 70-80 ℃ and dispersed in the dimethyl silicone oil, the high-viscosity dimethyl silicone oil generates shearing force under mechanical stirring, the small balls are crushed into microspheres and rapidly settled, the microspheres are filtered, washed by petroleum ether and boiling water, and dried, and the iron phosphate microspheres are obtained.
The phosphate is ammonium dihydrogen phosphate.
The copper slag comprises the following main components: fe2O3 55～60wt%、SiO2 20～23wt%、MgO 4～5wt%、Al2O3 3～4wt%、CaO 3～4wt%、ZnO 1～2wt%；
The copper slag powder is prepared by drying copper slag at the temperature of 75-85 ℃ for 24h, grinding and sieving with a 80-mesh sieve;
the mass ratio of the phosphate to the copper slag powder is 0.25-0.5, and the mass ratio of the borax to the copper slag powder is 0.01-0.1;
the mass ratio of the mixture to the deionized water is 4.5-6.0;
the viscosity of the dimethyl silicone oil is 1000cs, and the stirring speed is 900-1100 r/min;
the drying temperature is 30-60 ℃, and the drying time is 2-4 h.
The invention has the beneficial effects that:
the invention provides an effective way for recycling waste, and has the advantages of rich raw material source, lower cost, simple process operation, no need of catalyst and capability of carrying out reaction at room temperature; the invention adopts acid excitation to prepare the iron phosphate microspheres, the balling degree exceeds 80 percent, and the iron phosphate microspheres can be directly used for adsorbing a coloring agent methylene blue in waste water; the iron phosphate microspheres have a porous structure, so that the adsorption capacity of the iron phosphate microspheres is enhanced, and the iron phosphate microspheres are spherical, are easy to recover, can be repeatedly used and cannot cause secondary pollution to a water body; the invention has better application prospect in wastewater treatment.
Detailed Description
In order to better embody the content of the present invention, the present invention is further described in detail by the following specific examples, but the scope of the present invention is not limited to the content; the copper slag used in the examples mainly comprises the following components: fe2O358.09wt%、SiO222.84wt%、MgO 4.99wt%、Al2O33.4wt%, CaO 3.28wt%, ZnO 1.67 wt%; the viscosity of the dimethyl silicone oil is 1000 cs;
example 1:
(1) adding ammonium dihydrogen phosphate and borax into copper slag powder (prepared by drying at 80 ℃ for 24h and grinding and sieving with a 80-mesh sieve) and uniformly stirring, wherein the mass ratio of ammonium dihydrogen phosphate to copper slag powder is 0.33, and the mass ratio of borax to copper slag powder is 0.1; adding deionized water into the mixture, and uniformly stirring to obtain slurry, wherein the mass ratio of the mixture to the deionized water is 6.0; under the conditions of heating and stirring at 900 revolutions per minute, dropwise adding the slurry into the dimethyl silicone oil at 75 ℃, rapidly solidifying the liquid drops at 75 ℃ into small balls, dispersing the small balls into the dimethyl silicone oil, settling the small balls into balls, filtering the balls, washing the balls with petroleum ether and boiling water, removing residual dimethyl silicone oil, and drying the balls at 50 ℃ for 3 hours to obtain the iron phosphate microspheres;
(2) screening the iron phosphate microspheres prepared in the step (1), and selecting spheres with the particle size of 300-750 mu m for an adsorption test;
(3) respectively preparing 50mL of 0.2g/L three groups of methylene blue solutions which are respectively numbered as (i), (ii) and (iii);
(4) regulating the pH value of the No. sample solution to 3, regulating the pH value of the No. sample solution to 7 and regulating the pH value of the No. sample solution to 11;
(5) respectively adding 1.5g of the iron phosphate microspheres obtained in the step (1) into the three groups of samples obtained in the step (4), and performing shock adsorption at normal temperature for 24 hours;
(6) through determination, the adsorption rate of the sample No. I: 81.58%, sample adsorption rate No. + -: 91.92%, sample adsorption rate III: 88.48 percent.
Example 2:
(1) adding ammonium dihydrogen phosphate and borax into copper slag powder (prepared by drying at 75 ℃ for 24h and grinding and sieving with a 80-mesh sieve) and uniformly stirring, wherein the mass ratio of ammonium dihydrogen phosphate to copper slag powder is 0.4, and the mass ratio of borax to copper slag powder is 0.05; adding deionized water into the mixture, and uniformly stirring to obtain slurry, wherein the mass ratio of the mixture to the deionized water is 5.5; under the conditions of heating and stirring at 1000 revolutions per minute, dropwise adding the slurry into dimethyl silicone oil at 80 ℃, quickly solidifying the liquid drops at 80 ℃ into small balls, dispersing the small balls into the dimethyl silicone oil, settling the small balls into balls, filtering the balls, washing the balls with petroleum ether and boiling water, removing residual dimethyl silicone oil, and drying the balls at 60 ℃ for 2 hours to obtain the iron phosphate microspheres;
(2) screening the iron phosphate microspheres prepared in the step (1), and selecting spheres with the particle size of 300-750 mu m for an adsorption test;
(3) preparing three groups of methylene blue solutions with the concentrations of 0.2g/L, 0.4g/L and 0.6g/L, wherein 50mL of each methylene blue solution is respectively numbered as (i), (ii) and (iii);
(4) the pH of the three sets of samples was adjusted to 7;
(5) respectively adding 1.5g of the iron phosphate microspheres obtained in the step (1) into the three groups of samples obtained in the step (4), and performing shock adsorption at normal temperature for 6 hours;
(6) through determination, the adsorption rate of the sample No. I: 87.62%, sample adsorption rate No. + -: 67.17%, sample adsorption rate No.: 58.24 percent.
Example 3:
(1) adding ammonium dihydrogen phosphate and borax into copper slag powder (prepared by drying at 75 ℃ for 24h and grinding and sieving with a 80-mesh sieve) and uniformly stirring, wherein the mass ratio of ammonium dihydrogen phosphate to copper slag powder is 0.5, and the mass ratio of borax to copper slag powder is 0.02; adding deionized water into the mixture, and uniformly stirring to obtain slurry, wherein the mass ratio of the mixture to the deionized water is 4.5; under the conditions of heating and stirring at 1100 r/min, dropwise adding the slurry into dimethyl silicone oil at 70 ℃, rapidly solidifying the liquid drops at 70 ℃ into small balls, dispersing the small balls in the dimethyl silicone oil, settling the small balls into balls, filtering the balls, washing the balls with petroleum ether and boiling water, removing residual dimethyl silicone oil, and drying the balls at 40 ℃ for 4 hours to obtain the iron phosphate microspheres;
(2) screening the iron phosphate microspheres prepared in the step (1), and selecting spheres with the particle size of 300-750 mu m for an adsorption test;
(3) preparing three groups of methylene blue solutions with the concentration of 0.2g/L, wherein 50mL of each methylene blue solution is respectively numbered as (i), (ii) and (iii);
(4) the pH of the three sets of samples was adjusted to 7;
(5) adding the iron phosphate microspheres obtained in the step (1) into the three groups of samples obtained in the step (4), adding 1g of No. 1 sample, adding 1.5g of No. 2 sample, adding 2g of No. 2 sample, and performing shock adsorption at normal temperature for 6 hours;
(6) through determination, the adsorption rate of the sample No. I: 74.08%, sample adsorption rate No. + -: 80.42%, sample adsorption rate # C: 90.78 percent.
Example 4:
(1) the preparation method of the iron phosphate microspheres is the same as that of example 1;
(2) screening the iron phosphate microspheres prepared in the step (1), and selecting spheres with the particle size of 300-750 mu m for an adsorption test;
(3) preparing three groups of methylene blue solutions with the concentration of 0.2g/L, wherein 50mL of each methylene blue solution is respectively numbered as (i), (ii) and (iii);
(4) the pH of the three sets of samples was adjusted to 7;
(5) respectively adding 1.5g of the iron phosphate microspheres obtained in the step (1) into the three groups of samples in the step (4), and performing shock adsorption at normal temperature, wherein the adsorption time of the No. sample is 4 hours, the adsorption time of the No. sample is 5 hours, and the adsorption time of the No. sample is 6 hours;
(6) through determination, the adsorption rate of the sample No. I: 71.20%, sample adsorption rate No. + -: 83.58%, sample adsorption rate # C: 84.08 percent.
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