CN110302753B - Preparation method of magnesium oxide-carbon composite microspheres - Google Patents
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- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 239000004005 microsphere Substances 0.000 title claims abstract description 31
- ZBQLSHTXSSTFEW-UHFFFAOYSA-N [C+4].[O-2].[Mg+2].[O-2].[O-2] Chemical compound [C+4].[O-2].[Mg+2].[O-2].[O-2] ZBQLSHTXSSTFEW-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 14
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 11
- 159000000003 magnesium salts Chemical class 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 239000012159 carrier gas Substances 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 239000000443 aerosol Substances 0.000 claims description 6
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 6
- 239000003570 air Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000007790 solid phase Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims description 4
- 229920000858 Cyclodextrin Polymers 0.000 claims description 3
- 239000001116 FEMA 4028 Substances 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 3
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 3
- 229960004853 betadex Drugs 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims description 2
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 claims description 2
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical group O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 claims description 2
- WRUGWIBCXHJTDG-UHFFFAOYSA-L magnesium sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Mg+2].[O-]S([O-])(=O)=O WRUGWIBCXHJTDG-UHFFFAOYSA-L 0.000 claims description 2
- 229940061634 magnesium sulfate heptahydrate Drugs 0.000 claims description 2
- 239000007858 starting material Substances 0.000 claims 1
- 239000000975 dye Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 4
- 239000003242 anti bacterial agent Substances 0.000 abstract description 3
- 229940088710 antibiotic agent Drugs 0.000 abstract description 3
- 241000894006 Bacteria Species 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 description 18
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 9
- 239000000395 magnesium oxide Substances 0.000 description 8
- 230000000844 anti-bacterial effect Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 238000000197 pyrolysis Methods 0.000 description 4
- 241000588724 Escherichia coli Species 0.000 description 3
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L magnesium chloride Substances [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 229940091250 magnesium supplement Drugs 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 239000013118 MOF-74-type framework Substances 0.000 description 1
- 239000004098 Tetracycline Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229960003907 linezolid Drugs 0.000 description 1
- TYZROVQLWOKYKF-ZDUSSCGKSA-N linezolid Chemical compound O=C1O[C@@H](CNC(=O)C)CN1C(C=C1F)=CC=C1N1CCOCC1 TYZROVQLWOKYKF-ZDUSSCGKSA-N 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000005691 oxidative coupling reaction Methods 0.000 description 1
- 238000005839 oxidative dehydrogenation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910021649 silver-doped titanium dioxide Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- 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
- C02F2101/20—Heavy metals or heavy metal compounds
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- 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)
- Treating Waste Gases (AREA)
Abstract
The invention belongs to the technical field of new materials, and provides a preparation method of magnesium oxide-carbon composite microspheres. The method has the characteristics of simple and convenient operation, no use of surfactant and continuous preparation. The prepared composite microsphere material has high specific surface area, can adsorb heavy metal ions, antibiotics and organic dyes in sewage, and can kill bacteria in water.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a preparation method and application of magnesium oxide-carbon composite microspheres.
Background
As an important adsorbent, catalyst and antibacterial material, the nano magnesium oxide (MgO) has wide application in the fields of water treatment, industrial catalysis, antibacterial products and the like. The preparation of nano-magnesia in different shapes of sheet, flower, fiber and the like by thermal decomposition of different magnesium-containing precursors has been reported in a large quantity. In order to improve the dispersibility and stability of nano-magnesia, magnesia-based composites with different compositions and application properties are reported in succession, for example, Li-MgO compositesThe composite structure can be used for oxidative coupling of methane and oxidative dehydrogenation of ethane, and MgO-TiO2The composite film can be used for gas sensing, the ZnO-MgO composite material has good adsorption property on linezolid antibiotics, and the MgO coats Ag/TiO2The composite material can be used for photocatalytic degradation of phenol in water under sunlight.
The carbon material has rich pore structure and large specific surface area, so the magnesium oxide-carbon composite material has wide application prospect in the fields of adsorbents and catalysis. There are reports of preparing a hollow spherical MgO-C composite material by an arc spraying method using magnesium graphite, and also reports of preparing a massive or spongy magnesium oxide-carbon composite material by a direct calcination method using Mg-MOF-74, mesoporous carbon containing magnesium salts, or biomass containing magnesium salts as a precursor. Many methods also have the problems of high cost, irregular particle morphology, difficult continuous preparation and the like, and currently, a method for simply preparing the magnesium oxide-carbon composite microspheres is lacked.
Disclosure of Invention
The invention aims to provide a preparation method of magnesium oxide-carbon composite microspheres, and the prepared magnesium oxide-carbon composite material can be used in the field of water treatment, in particular to the adsorption of metal ions and organic dyes in water.
The technical scheme of the invention is as follows:
a preparation method of magnesium oxide-carbon composite microspheres comprises the following steps:
step 1, mixing a magnesium salt solution and a carbon-containing raw material solution, and preparing into a precursor solution under the stirring condition;
and 2, under the stirring condition of 200-500 r/min at the temperature of 10-90 ℃, enabling the precursor solution to pass through an aerosol generator by carrier gas, then enabling the precursor solution to enter a tubular furnace for calcination reaction, then separating a gas phase and a solid phase by the carrier gas through a solid-gas separator, and collecting solid powder to obtain the magnesium oxide-carbon composite microspheres.
Washing the magnesium oxide-carbon composite microsphere primary product with water, drying in a 60 ℃ oven, and then putting the product in an N oven2Calcining for 2h in the atmosphere to obtain the magnesium oxide-carbon composite microspheres.
The molar ratio of the magnesium salt to the carbon-containing raw material is 1: 0.2-1: 2.
The calcination temperature is 400-1000 ℃.
The magnesium salt is magnesium chloride hexahydrate, magnesium nitrate hexahydrate or magnesium sulfate heptahydrate, and the concentration of the magnesium salt solution is 0.01-4 mol/L; the carbon-containing raw materials are glucose, maltose and a mixture of the raw materials with a molar ratio of 1: 0.2-4 of formaldehyde and resorcinol, and the molar ratio is 1: 0.4-4 of phenol and formaldehyde or beta-cyclodextrin, wherein the concentration of the carbon-containing raw material solution is 0.01-4 mol/L.
The carrier gas is air, nitrogen or helium.
Compared with the prior art, the invention has the following effects and benefits: the magnesium salt and the carbon-containing raw material are mixed with water solution or sol, the precursor is formed after atomization by an aerosol generator, and then the precursor is continuously calcined by carrier gas, so that the magnesium oxide-carbon composite microsphere can be simply and conveniently obtained, and the preparation method has the characteristics of simple and convenient operation, no surfactant and continuous preparation. The prepared composite microsphere material has high specific surface area, can adsorb heavy metal ions, antibiotics and organic dyes in sewage, and can kill bacteria in water.
Drawings
Fig. 1 is a scanning electron microscope image of the prepared magnesium oxide-carbon composite microspheres.
Fig. 2 is a transmission electron microscope image of the prepared magnesium oxide-carbon composite microsphere.
Fig. 3 is an isotherm of prepared magnesium oxide-carbon composite microspheres adsorbing congo red.
Fig. 4 is an isotherm of adsorption of pb (ii) of the prepared magnesium oxide-carbon composite microsphere.
Detailed Description
The following describes specific embodiments of the present invention with reference to the technical solutions, but the scope of the present invention is not limited thereto.
Example 1
2mol/L of 100mL MgCl2Mixing with 0.5 mol/L100 mL glucose solution, stirring, passing through an aerosol generator and a tubular pyrolysis furnace with air flow rate of 1.0L/min, wherein the temperature of the tubular furnace is 600 ℃, and separating gas phase and solid phase by a solid-gas separator to obtain a primary product. After the primary product is washed by water for three times,drying in an oven at 60 ℃ followed by N2Placing the mixture in a tubular furnace in the atmosphere, and calcining the mixture for 2 hours at the temperature of 600 ℃ to obtain the magnesium oxide-carbon composite microspheres. The structure is shown in fig. 1 and 2.
The magnesium oxide-carbon composite microspheres have excellent adsorption performance on organic dyes represented by Congo red and heavy metal ions represented by Pb (II). Respectively using Congo red of 100ppm, 500ppm and 1000ppm as test solution, selecting 5min, 10min, 15min, 20min and 25min as test time points, wherein the adsorption experiment result shows that the absorption balance is basically achieved within 5min, the adsorption rate is high, the removal rates are respectively 99.85%, 99.2% and 96.8%, and the pseudo-second-stage kinetic adsorption model is met; as shown in the figure 3, the Congo red adsorption isotherm shows that the adsorption conforms to the Langmuir model, and the theoretical adsorption amount is as high as 4024 mg/g.
Studies have shown that the adsorption of Pb (II) by the magnesium oxide-carbon composite microspheres conforms to the Langmuir model with theoretical adsorption amounts of 5166mg/g, using 1000ppm, 2000ppm, 3000ppm, 4000ppm and 5000ppm aqueous solutions of Pb (II) as test solutions, respectively, as shown in FIG. 4.
Experimental results of experiments on tetracycline adsorption of the magnesium oxide-carbon composite microspheres show that under 50ppm, adsorption balance is basically achieved within 5min, the adsorption rate is high, and the removal rate is 95.5%; at 100ppm, the adsorption balance is basically achieved within 15min, and the removal rate is 82.1 percent respectively.
In addition, antibacterial experiments show that the antibacterial rate of the prepared composite microspheres to escherichia coli and staphylococcus aureus is more than 98%.
Example 2
2mol/L of 100mLMgCl2Mixing with 0.5 mol/L100 mL resorcinol and formaldehyde solution (molar ratio is 1: 2), stirring uniformly, passing through an aerosol generator and a tubular pyrolysis furnace of a reaction device by nitrogen with flow rate of 1.5L/min, wherein the temperature of the tubular pyrolysis furnace is 600 ℃, separating gas phase and solid phase by a solid-gas separator, and collecting solid powder to obtain a primary product; washing the collected crude product with water for three times, centrifuging, drying the collected solid powder in an oven at 60 deg.C, and then N2Calcining for 2h at 500 ℃ in the atmosphere to obtain the magnesium oxide-carbon composite microspheres.The magnesium oxide-carbon composite microspheres have excellent adsorption performance on organic dyes represented by Congo red and heavy metal ions represented by Pb (II); antibacterial experiments show that the antibacterial rate of the composite microspheres to escherichia coli and staphylococcus aureus reaches 99%.
Example 3
1mol/L of 100mL MgCl2Mixing with 100mL beta-cyclodextrin solution dissolved in hot water at a concentration of 0.1mol/L, stirring under heating, passing through an aerosol generator and a tubular pyrolysis furnace of a reaction device at a flow rate of 1.5L/min under a temperature of 600 deg.C, separating gas phase and solid phase by a solid-gas separator, collecting solid powder to obtain an initial product, washing with water for three times, centrifuging, drying in an oven at 80 deg.C, and drying in N2Calcining for 2h at 500 ℃ in the atmosphere to obtain the magnesium oxide-carbon composite microspheres. The prepared magnesium oxide-carbon composite microspheres have excellent adsorption performance on Congo red and Pb (II), and the antibacterial rate on escherichia coli and staphylococcus aureus reaches 99%.
Claims (8)
1. The preparation method of the magnesium oxide-carbon composite microsphere is characterized by comprising the following steps:
step 1, mixing a magnesium salt solution and a carbon-containing raw material solution, and preparing a precursor solution under the stirring condition;
step 2, under the stirring condition of 200-500 r/min at the temperature of 10-90 ℃, enabling the precursor solution to pass through an aerosol generator by carrier gas, then enabling the precursor solution to enter a tubular furnace for calcination reaction, then separating a gas phase and a solid phase by the carrier gas through a solid-gas separator, and collecting solid powder to obtain the magnesium oxide-carbon composite microspheres;
the magnesium salt is magnesium chloride hexahydrate, magnesium nitrate hexahydrate or magnesium sulfate heptahydrate, and the concentration of the magnesium salt solution is 0.01-4 mol/L; the carbon-containing raw materials are glucose, maltose and a mixture of the raw materials with a molar ratio of 1: 0.2-4 of formaldehyde and resorcinol, and the molar ratio is 1: 0.4-4 of phenol and formaldehyde or beta-cyclodextrin, wherein the concentration of the carbon-containing raw material solution is 0.01-4 mol/L.
2. The method according to claim 1, wherein the magnesium oxide-carbon composite microspheres are washed with water, dried in an oven at 60 ℃, and then N-dried2Calcining for 2h in the atmosphere to obtain the magnesium oxide-carbon composite microspheres.
3. The method according to claim 1 or 2, wherein the molar ratio of the magnesium salt to the carbonaceous starting material is 1:0.2 to 1: 2.
4. The method according to claim 1 or 2, wherein the calcination temperature is 400 to 1000 ℃.
5. The preparation method according to claim 3, wherein the calcination temperature is 400 to 1000 ℃.
6. The method according to claim 1, 2 or 5, wherein the carrier gas is air, nitrogen or helium.
7. The method according to claim 3, wherein the carrier gas is air, nitrogen or helium.
8. The method according to claim 4, wherein the carrier gas is air, nitrogen or helium.
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