CN111821979A - Novel method for preparing recyclable graphene composite titanium dioxide nano material - Google Patents
Novel method for preparing recyclable graphene composite titanium dioxide nano material Download PDFInfo
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- CN111821979A CN111821979A CN202010671513.0A CN202010671513A CN111821979A CN 111821979 A CN111821979 A CN 111821979A CN 202010671513 A CN202010671513 A CN 202010671513A CN 111821979 A CN111821979 A CN 111821979A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 31
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 14
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 13
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title abstract description 9
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 18
- 239000010439 graphite Substances 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 229910003264 NiFe2O4 Inorganic materials 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000012286 potassium permanganate Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 7
- 239000011941 photocatalyst Substances 0.000 claims description 6
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910021382 natural graphite Inorganic materials 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 239000004317 sodium nitrate Substances 0.000 claims description 5
- 235000010344 sodium nitrate Nutrition 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 3
- 150000002505 iron Chemical class 0.000 claims description 3
- 150000002815 nickel Chemical class 0.000 claims description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 230000005389 magnetism Effects 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a novel method for preparing a recyclable graphene composite titanium dioxide nano material. The preparation method is characterized by firstly preparing nickel ferrite by a hydrothermal method, preparing graphite oxide by a Hummers method, and synthesizing the nickel ferrite, graphene and titanium dioxide into the composite material by one step by the hydrothermal method. The preparation process is simple to operate, reaction conditions are easy to control, requirements on equipment are low, loss is low, high-temperature calcination is not needed, synthesis cost is reduced, the market prospect is good, the prepared composite material has excellent photocatalytic performance, magnetism is convenient to recover, the composite material can be repeatedly used, and economic benefits are improved.
Description
Technical Field
The invention relates to a novel method for preparing a recyclable graphene composite titanium dioxide nano material, and belongs to the technical field of processing application and inorganic chemical industry of nano materials.
Background
The nano titanium dioxide is a typical photocatalyst, has the advantages of stable performance, high catalytic activity, low price, no secondary pollution and the like, and has very wide application prospect in wastewater treatment. However, the nano titanium dioxide has the disadvantages of poor dispersibility, difficult recovery and the like in the actual use process, thereby limiting the industrial application of the nano titanium dioxide.
Disclosure of Invention
The invention aims to provide a method for preparing a recyclable graphene composite titanium dioxide nano material, the composite material prepared by the method has excellent photocatalytic performance, can overcome the defect of difficult recycling of nano titanium dioxide, can be repeatedly used, and has good market prospect.
The characteristic steps of the invention are as follows:
the first step is as follows: preparation of graphite oxide
Adding 2g of natural graphite and 1g of sodium nitrate into a 250mL three-neck flask at room temperature, and cooling to 0 ℃; slowly adding 50mL of concentrated sulfuric acid into a three-neck bottle, and fully stirring for 30 min; then, 0.3g of potassium permanganate is added and fully stirred for 30 min; 7g of potassium permanganate are added into a three-mouth bottle in three batches within 1 h. Removing ice bath, heating to (35 + -3) deg.C with water bath, and stirring thoroughly for 2h to obtain brown suspension. Slowly adding 90mL of deionized water into a three-mouth bottle, and suddenly raising the temperature to 90 ℃; after reacting for 15min, adding a mixed solution of 7mL of hydrogen peroxide and 55mL of ultrapure water (45 ℃) to obtain a golden yellow graphite oxide dispersion, filtering while hot, washing to be neutral, and drying to obtain graphite oxide.
The second step is that: preparation of magnetic nickel ferrite
Weighing nickel salt and iron salt (n (Ni) in certain mass2+):n(Fe3+) 1:2) in deionized water to give solution a. Weighing a certain mass of NaOH and dissolving in deionized water to obtain a solution B. Dropwise adding the solution B into the solution A, stirring vigorously for 20min, transferring into a 100ml hydrothermal reaction kettle, reacting at 180-220 ℃ for 10-12 h, naturally cooling, taking out, separating in a magnetic field, washing for 3 times, drying at 200 ℃ for 4h, and grinding to obtain NiFe2O4And (3) powder.
The third step: preparation of magnetic graphene composite titanium dioxide
Adding a certain volume of absolute ethyl alcohol into a 100mL beaker at room temperature, dropwise adding a certain volume of tetrabutyl titanate under magnetic stirring, stirring for 10min, then adding acid, and continuously stirring for 10min to obtain a solution A. Taking a certain mass of NiFe2O4Adding the solution into deionized water with a certain volume, finally adding graphite oxide with a certain mass, and carrying out ultrasonic treatment for 10min to obtain a solution B. Adding the solution B into the solution A, carrying out ultrasonic treatment for 30min, transferring the solution B into a 100mL hydrothermal reaction kettle, and carrying out reverse reaction at 80-120 DEG CFiltering the mixture for 18 to 22 hours while the mixture is hot, washing, drying and grinding the mixture to obtain the magnetic TiO2-GO photocatalyst powder.
The nickel salt is as follows: NiCl2、Ni(NO3)2Or NiSO4One kind of (1).
The iron salt is as follows: FeCl3、Fe2(SO4)3Or Fe (NO)3)3One kind of (1).
The acid is: HCl, CH3One kind of COOH.
The magnetic graphene-titanium dioxide composite material is prepared by carrying out hydrothermal reaction on graphene, nickel ferrite and titanium dioxide for 18-22 h at 80-120 ℃ for compounding.
The invention has the beneficial effects that:
(1) the preparation process is simple to operate, reaction conditions are easy to control, requirements on equipment are low, loss is low, high-temperature calcination is not needed, the synthesis cost is reduced, and the method has a good market prospect.
(2) The addition of the graphene improves the photocatalytic performance of the titanium dioxide, and the addition of the nickel ferrite enables the composite catalyst to be easily recycled and to be used for multiple times.
Detailed Description
The present invention will be further described with reference to examples and comparative examples, but the scope of the present invention is by no means limited thereto:
embodiment 1:
adding 2g of natural graphite and 1g of sodium nitrate into a 250mL three-neck flask at room temperature, and cooling to 0 ℃; slowly adding 50mL of concentrated sulfuric acid into a three-neck bottle, and fully stirring for 30 min; then, 0.3g of potassium permanganate is added and fully stirred for 30 min; 7g of potassium permanganate are added into a three-mouth bottle in three batches within 1 h. Removing ice bath, heating to (35 + -3) deg.C with water bath, and stirring thoroughly for 2h to obtain brown suspension. Slowly adding 90mL of deionized water into a three-mouth bottle, and suddenly raising the temperature to 90 ℃; after reacting for 15min, adding a mixed solution of 7mL of hydrogen peroxide and 55mL of ultrapure water (45 ℃) to obtain a golden yellow graphite oxide dispersion, filtering while hot, washing to be neutral, and drying to obtain graphite oxide.
Weighing 2.6284g NiSO4·6H2O and 5.4059gFeCl3·6H2And dissolving the O in 15ml of deionized water respectively, uniformly mixing the two solutions, and magnetically stirring for 10min to obtain a solution A. 3.20g NaOH was weighed out and dissolved in 45ml deionized water to obtain solution B. Dropwise adding the solution B into the solution A, stirring vigorously for 20min, transferring into a 100ml hydrothermal reaction kettle, reacting at 180 deg.C for 10h, naturally cooling, taking out, separating in a magnetic field, washing with water for 3 times, drying at 200 deg.C for 4h, and grinding to obtain NiFe2O4And (3) powder.
At room temperature, 5mL of absolute ethyl alcohol is added into a 100mL beaker, 5mL of tetrabutyl titanate is dropwise added under magnetic stirring, after stirring for 10min, 6mL of hydrochloric acid is added, and after stirring is continued for 10min, solution A is obtained. Taking a certain mass of NiFe2O4Adding the solution into 75mL of deionized water, finally adding 0.0020g of graphite oxide, and carrying out ultrasonic treatment for 10min to obtain a solution B. Adding the solution B into the solution A, carrying out ultrasonic treatment for 30min, transferring the solution B into a 100mL hydrothermal reaction kettle, reacting for 22h at 80 ℃, filtering while the solution is hot, washing, drying and grinding to obtain the magnetic TiO2-GO photocatalyst powder.
Embodiment 2:
adding 2g of natural graphite and 1g of sodium nitrate into a 250mL three-neck flask at room temperature, and cooling to 0 ℃; slowly adding 50mL of concentrated sulfuric acid into a three-neck bottle, and fully stirring for 30 min; then, 0.3g of potassium permanganate is added and fully stirred for 30 min; 7g of potassium permanganate are added into a three-mouth bottle in three batches within 1 h. Removing ice bath, heating to (35 + -3) deg.C with water bath, and stirring thoroughly for 2h to obtain brown suspension. Slowly adding 90mL of deionized water into a three-mouth bottle, and suddenly raising the temperature to 90 ℃; after reacting for 15min, adding a mixed solution of 7mL of hydrogen peroxide and 55mL of ultrapure water (45 ℃) to obtain a golden yellow graphite oxide dispersion, filtering while hot, washing to be neutral, and drying to obtain graphite oxide.
Weighing 2.9081gNi (NO)3)2·6H2O and 8.0799gFe (NO)3)3·9H2And dissolving the O in 15ml of deionized water respectively, uniformly mixing the two solutions, and magnetically stirring for 10min to obtain a solution A. 3.20g NaOH was weighed out and dissolved in 45ml deionized water to obtain solution B. The solution B is gradually mixedDropwise adding into the solution A, stirring vigorously for 20min, transferring into 100ml hydrothermal reaction kettle, reacting at 200 deg.C for 10 hr, naturally cooling, taking out, separating in magnetic field, washing with water for 3 times, drying at 200 deg.C for 4 hr, and grinding to obtain NiFe2O4And (3) powder.
At room temperature, 5mL of absolute ethyl alcohol is added into a 100mL beaker, 5mL of tetrabutyl titanate is dropwise added under magnetic stirring, after stirring for 10min, 6mL of acetic acid is added, and after stirring is continued for 10min, solution A is obtained. Taking a certain mass of NiFe2O4Adding the solution into 75mL of deionized water, finally adding 0.0030g of graphite oxide, and carrying out ultrasonic treatment for 10min to obtain a solution B. Adding the solution B into the solution A, carrying out ultrasonic treatment for 30min, transferring the solution B into a 100mL hydrothermal reaction kettle, reacting for 20h at 100 ℃, filtering while the solution is hot, washing, drying and grinding to obtain the magnetic TiO2-GO photocatalyst powder.
Embodiment 3:
adding 2g of natural graphite and 1g of sodium nitrate into a 250mL three-neck flask at room temperature, and cooling to 0 ℃; slowly adding 50mL of concentrated sulfuric acid into a three-neck bottle, and fully stirring for 30 min; then, 0.3g of potassium permanganate is added and fully stirred for 30 min; 7g of potassium permanganate are added into a three-mouth bottle in three batches within 1 h. Removing ice bath, heating to (35 + -3) deg.C with water bath, and stirring thoroughly for 2h to obtain brown suspension. Slowly adding 90mL of deionized water into a three-mouth bottle, and suddenly raising the temperature to 90 ℃; after reacting for 15min, adding a mixed solution of 7mL of hydrogen peroxide and 55mL of ultrapure water (45 ℃) to obtain a golden yellow graphite oxide dispersion, filtering while hot, washing to be neutral, and drying to obtain graphite oxide.
Weighing 2.3769g NiCl2·6H2O and 5.5606gFe2(SO4)3·7H2And dissolving the O in 15ml of deionized water respectively, uniformly mixing the two solutions, and magnetically stirring for 10min to obtain a solution A. 3.20g NaOH was weighed out and dissolved in 45ml deionized water to obtain solution B. Dropwise adding the solution B into the solution A, stirring vigorously for 20min, transferring into a 100ml hydrothermal reaction kettle, reacting at 220 deg.C for 9h, naturally cooling, taking out, separating in a magnetic field, washing with water for 3 times, drying at 200 deg.C for 4h, and grinding to obtain NiFe2O4And (3) powder.
At room temperature, 5mL of absolute ethyl alcohol is added into a 100mL beaker, 5mL of tetrabutyl titanate is dropwise added under magnetic stirring, after stirring for 10min, 6mL of hydrochloric acid is added, and after stirring is continued for 10min, solution A is obtained. Taking a certain mass of NiFe2O4Adding the solution into 75mL of deionized water, finally adding 0.0030g of graphite oxide, and carrying out ultrasonic treatment for 10min to obtain a solution B. Adding the solution B into the solution A, carrying out ultrasonic treatment for 30min, transferring the solution B into a 100mL hydrothermal reaction kettle, reacting for 18h at 120 ℃, filtering while the solution is hot, washing, drying and grinding to obtain the magnetic TiO2-GO photocatalyst powder.
Claims (2)
1. A preparation method of a magnetic graphene composite titanium dioxide nano material is characterized by comprising the following steps: the first step is as follows: and (3) preparing graphite oxide. Adding 2g of natural graphite and 1g of sodium nitrate into a 250mL three-neck flask at room temperature, and cooling to 0 ℃; slowly adding 50mL of concentrated sulfuric acid into a three-neck bottle, and fully stirring for 30 min; then, 0.3g of potassium permanganate is added and fully stirred for 30 min; 7g of potassium permanganate are added into a three-mouth bottle in three batches within 1 h. Removing ice bath, heating to (35 + -3) deg.C with water bath, and stirring thoroughly for 2h to obtain brown suspension. Slowly adding 90mL of deionized water into a three-mouth bottle, and suddenly raising the temperature to 90 ℃; after reacting for 15min, adding a mixed solution of 7mL of hydrogen peroxide and 55mL of ultrapure water (45 ℃) to obtain a golden yellow graphite oxide dispersion, filtering while hot, washing to be neutral, and drying to obtain graphite oxide. The second step is that: preparing magnetic nickel ferrite. Weighing nickel salt and iron salt (n (Ni) in certain mass2+):n(Fe3+) 1:2) in deionized water to give solution a. Weighing a certain mass of NaOH and dissolving in deionized water to obtain a solution B. Dropwise adding the solution B into the solution A, stirring vigorously for 20min, transferring into a 100ml hydrothermal reaction kettle, reacting at 180-220 ℃ for 10-12 h, naturally cooling, taking out, separating in a magnetic field, washing for 3 times, drying at 200 ℃ for 4h, and grinding to obtain NiFe2O4And (3) powder. The third step: and (3) preparing the magnetic graphene composite titanium dioxide. At room temperature, adding a certain volume of absolute ethyl alcohol into a 100mL beaker, dropwise adding a certain volume of tetrabutyl titanate dropwise under magnetic stirring, stirring for 10min,then adding acid, and continuing stirring for 10min to obtain a solution A. Taking a certain mass of NiFe2O4Adding the solution into deionized water with a certain volume, finally adding graphite oxide with a certain mass, and carrying out ultrasonic treatment for 10min to obtain a solution B. Adding the solution B into the solution A, carrying out ultrasonic treatment for 30min, transferring the solution B into a 100mL hydrothermal reaction kettle, reacting for 18-22 h at 80-120 ℃, filtering while the solution is hot, washing, drying and grinding to obtain the magnetic TiO2-GO photocatalyst powder.
2. The preparation method according to claim 1, characterized in that the magnetic graphene composite titanium dioxide composite material is prepared by carrying out hydrothermal reaction on graphene, nickel ferrite and titanium dioxide at 80-120 ℃ for 18-22 h.
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| CN202010671513.0A CN111821979A (en) | 2020-07-13 | 2020-07-13 | Novel method for preparing recyclable graphene composite titanium dioxide nano material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113120977A (en) * | 2021-04-30 | 2021-07-16 | 佛山经纬纳科环境科技有限公司 | Method for preparing nickel ferrite nano material from nickel-containing iron electroplating wastewater and application |
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2020
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113120977A (en) * | 2021-04-30 | 2021-07-16 | 佛山经纬纳科环境科技有限公司 | Method for preparing nickel ferrite nano material from nickel-containing iron electroplating wastewater and application |
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