CN107803202B - Preparation method of Cs/Ti-Fe composite photocatalyst - Google Patents
Preparation method of Cs/Ti-Fe composite photocatalyst Download PDFInfo
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- CN107803202B CN107803202B CN201711122433.4A CN201711122433A CN107803202B CN 107803202 B CN107803202 B CN 107803202B CN 201711122433 A CN201711122433 A CN 201711122433A CN 107803202 B CN107803202 B CN 107803202B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 229910011212 Ti—Fe Inorganic materials 0.000 title claims abstract description 20
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 115
- NLSCHDZTHVNDCP-UHFFFAOYSA-N caesium nitrate Chemical compound [Cs+].[O-][N+]([O-])=O NLSCHDZTHVNDCP-UHFFFAOYSA-N 0.000 claims abstract description 102
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 56
- 238000001354 calcination Methods 0.000 claims abstract description 16
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 8
- 125000005456 glyceride group Chemical group 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 23
- 239000002994 raw material Substances 0.000 abstract description 19
- 239000003513 alkali Substances 0.000 abstract 1
- 238000010335 hydrothermal treatment Methods 0.000 abstract 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 15
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000013329 compounding Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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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
- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a preparation method of a Cs/Ti-Fe composite photocatalyst, which synthesizes the Cs/Ti-Fe composite photocatalyst by using titanium dioxide, cesium nitrate, ferric nitrate, sodium carbonate and other raw materials through hydrothermal treatment, alkali treatment, calcination and other methods.
Description
Technical Field
The invention relates to a preparation method of a Cs/Ti-Fe composite photocatalyst, belonging to the field of catalysis.
Background
TiO was discovered by Fujishima and Honaa et al, Japan scholars in 19722The single crystal electrode can realize photocatalytic water decomposition and nano TiO2TiO is used for degrading organic matters by photocatalysis2The semiconductor photocatalytic material has the unique advantages of being capable of utilizing the energy of the ultraviolet band of sunlight to carry out photocatalytic degradation on organic matters and photolysis water to produce hydrogen, and becomes a focus of attention in the field of materials. However, TiO2In the case of the anatase crystal form, the band gap is 3.2eV, only the wavelength can be absorbed<Ultraviolet light in the range of 380Inn cannot be fully utilized and accounts for about 43 percent of the solar spectrumThe visible light (400-750 lun) energy limits its wide application. The preparation method of the Cs/Ti-Fe composite photocatalyst can effectively solve the problem of utilization efficiency by compounding the Cs/Ti-Fe composite photocatalyst with cesium nitrate and ferric nitrate, and is simple to prepare and good in catalytic effect.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a Cs/Ti-Fe composite photocatalyst.
In order to achieve the purpose, the invention adopts the technical scheme that the preparation method of the Cs/Ti-Fe composite photocatalyst. The method comprises the following steps:
step 1, weighing titanium dioxide powder, dissolving in deionized water, and simultaneously carrying out ultrasonic treatment for 40min to serve as a solvent;
step 2, dissolving the weighed cesium nitrate and ferric nitrate in the prepared titanium dioxide solution, and stirring in a water bath at 50 ℃ for 2 hours until the solute is completely dissolved;
step 3, simultaneously mixing a certain amount of NaOH and Na2CO3Stirring in the prepared titanium dioxide solution at 40 ℃ in an oil bath until the solute is completely dissolved;
step 4, sucking the prepared NaOH and Na by using a rubber head dropper2CO3The cesium nitrate is dropwise added into the mixed solution, and the milky solution is found to generate a reddish-brown flocculent precipitate after the dropwise addition is finished in 30 minutes in the ferric nitrate mixed solution;
step 5, transferring the mixture into a vacuum glove box, and carrying out vibration treatment for 2 hours under a reciprocating type oscillator and simultaneously carrying out ultraviolet treatment;
step 6, then, dropwise adding surfactant fatty glyceride, dropwise adding at the speed of 30 per minute, and simultaneously stirring in an ice-water bath;
step 7, after the ice-water bath treatment is finished, transferring the mixture into a polytetrafluoroethylene reaction kettle, heating the mixture to 200 ℃ at the speed of 5 ℃/min, and reacting the mixture for 5 hours in a nitrogen atmosphere;
step 8, stopping heating after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, sequentially washing the taken sample with deionized water and ethanol for 5-8 times, and drying in a vacuum drying oven at 120 ℃ for 24 hours;
and 9, calcining in a tube furnace: firstly, CO2Calcining at 150 ℃ under the atmosphere for 2h under 0.4kpa, then calcining at 180 ℃ under 0.5kpa under the atmosphere of ammonia for 3h, and finally calcining at 240 ℃ under 0.6kpa under the atmosphere of nitrogen for 4h to finally obtain the Cs/Ti-Fe composite photocatalyst.
The preparation method of the Cs/Ti-Fe composite photocatalyst has the beneficial effect. According to the invention, the problems of low catalytic efficiency and the like of single titanium dioxide can be effectively solved by compounding titanium dioxide, cesium nitrate and ferric nitrate together, the synergistic effect can be further improved by calcining treatment in different atmospheres through ultrasound, ultraviolet and during the preparation process, the high specific surface area can be obtained, the recombination probability of electrons and holes is reduced, the adsorption capacity of particles on the surface of pollutants is improved, and the degradation activity is obviously improved. Wherein, in example 1, titanium dioxide, cesium nitrate, iron nitrate 44: 15:7 (parts per unit). 44 parts of titanium dioxide, 15 parts of cesium nitrate and 7 parts of ferric nitrate. 10 portions of NaOH and Na2CO38 parts of surfactant fatty glyceride and 5 parts of surfactant fatty glyceride. Example 2 preparation of titanium dioxide, cesium nitrate, iron nitrate 54: 18:6 (parts per unit). 54 parts of titanium dioxide, 18 parts of cesium nitrate and 6 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials. The prepared Cs/Ti-Fe composite photocatalyst has the best catalytic effect.
Detailed Description
Example 1 preparation of titanium dioxide, cesium nitrate, iron nitrate 44: 15:7 (parts per unit). 44 parts of titanium dioxide, 15 parts of cesium nitrate and 7 parts of ferric nitrate. 10 portions of NaOH and Na2CO38 parts of surfactant fatty glyceride and 5 parts of surfactant fatty glyceride.
Step 1, weighing 44 parts of titanium dioxide powder, dissolving in 200 parts of deionized water, and simultaneously carrying out ultrasonic treatment for 40min to serve as a solvent;
step 2, weighing 15 parts of cesium nitrate and 7 parts of ferric nitrate, dissolving in the prepared titanium dioxide solution, and stirring in a water bath at 50 ℃ for 2 hours until the solute is completely dissolved;
step 3, mixing 10 parts of NaOH and8 parts of Na2CO3Stirring in the other half of the prepared titanium dioxide solution at 40 ℃ in an oil bath until the solute is completely dissolved;
step 4, sucking the prepared NaOH and Na by using a rubber head dropper2CO3The cesium nitrate is dropwise added into the mixed solution, and the milky solution is found to generate a reddish-brown flocculent precipitate after the dropwise addition is finished in 30 minutes in the ferric nitrate mixed solution;
step 5, transferring the mixture into a vacuum glove box, and carrying out vibration treatment for 2 hours under a reciprocating type oscillator and simultaneously carrying out ultraviolet treatment;
step 6, then 5 parts of surfactant fatty glyceride are dripped at the speed of 30 per minute, and the mixture is stirred in an ice-water bath;
step 7, after the ice-water bath treatment is finished, transferring the mixture into a polytetrafluoroethylene reaction kettle, heating the mixture to 200 ℃ at the speed of 5 ℃/min, and reacting the mixture for 5 hours in a nitrogen atmosphere;
step 8, stopping heating after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, sequentially washing the taken sample with deionized water and ethanol for 5-8 times, and drying in a vacuum drying oven at 120 ℃ for 24 hours;
and 9, calcining in a tube furnace: firstly, CO2Calcining at 150 ℃ under the atmosphere for 2h under 0.4kpa, then calcining at 180 ℃ under 0.5kpa under the atmosphere of ammonia for 3h, and finally calcining at 240 ℃ under 0.6kpa under the atmosphere of nitrogen for 4h to finally obtain the Cs/Ti-Fe composite photocatalyst.
Example 2 preparation of titanium dioxide, cesium nitrate, iron nitrate 54: 18:6 (parts per unit). 54 parts of titanium dioxide, 18 parts of cesium nitrate and 6 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials.
Example 3 preparation of titanium dioxide, cesium nitrate, iron nitrate 42: 15:7 (parts per unit). 42 parts of titanium dioxide, 15 parts of cesium nitrate and 7 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials.
Example 4 preparation of titanium dioxide, cesium nitrate, iron nitrate 40: 15:7 (parts per unit). 40 parts of titanium dioxide, 15 parts of cesium nitrate and 7 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials.
Example 5 preparation of titanium dioxide, cesium nitrate, iron nitrate 46: 15:7 (parts per unit). 46 parts of titanium dioxide, 15 parts of cesium nitrate and 7 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials.
Example 6 preparation of titanium dioxide, cesium nitrate, iron nitrate 48: 15:7 (parts per unit). 48 parts of titanium dioxide, 15 parts of cesium nitrate and 7 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials.
Example 7 preparation of titanium dioxide, cesium nitrate, iron nitrate 50: 15:7 (parts per unit). 50 parts of titanium dioxide, 15 parts of cesium nitrate and 7 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials.
Example 8 preparation of titanium dioxide, cesium nitrate, iron nitrate 44: sample 16:7 (unit parts). 44 parts of titanium dioxide, 16 parts of cesium nitrate and 7 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials.
Example 9 preparation of titanium dioxide, cesium nitrate, iron nitrate 44: 17:7 (parts per unit). 44 parts of titanium dioxide, 17 parts of cesium nitrate and 7 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials.
Example 10 preparation of titanium dioxide, cesium nitrate, iron nitrate 44: 18:7 (parts per unit). 44 parts of titanium dioxide, 18 parts of cesium nitrate and 7 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials.
Example 11 preparation of titanium dioxide, cesium nitrate, iron nitrate 44: 15:8 (parts per unit). 44 parts of titanium dioxide, 15 parts of cesium nitrate and 8 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials.
Example 12 preparation of titanium dioxide, cesium nitrate, iron nitrate 44: 15:9 (parts per unit). 44 parts of titanium dioxide, 15 parts of cesium nitrate and 9 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials.
Example 13 preparation of titanium dioxide, cesium nitrate, iron nitrate 44: 15:10 (parts per unit). 44 parts of titanium dioxide, 15 parts of cesium nitrate and 10 parts of ferric nitrate. The procedure was the same as in example 1 except for the amounts of other raw materials.
Comparative example 1 preparation of titanium dioxide, cesium nitrate, iron nitrate 44: 15:7 (parts per unit). 44 parts of titanium dioxide, 15 parts of cesium nitrate and 7 parts of ferric nitrate, 1 part. The procedure was the same as in example 1 except that the titanium dioxide solution was not subjected to ultrasonic treatment and the amount of the other raw materials was changed.
Comparative example 2 preparation of titanium dioxide, cesium nitrate, iron nitrate 44: 15:7 (parts per unit). 44 parts of titanium dioxide, 15 parts of cesium nitrate and 7 parts of ferric nitrate. In which the water bath treatment was not carried out, the procedure was the same as in example 1.
Comparative example 3 preparation of titanium dioxide, cesium nitrate, iron nitrate 44: 15:7 (parts per unit). 44 parts of titanium dioxide, 15 parts of cesium nitrate and 7 parts of ferric nitrate. The procedure was the same as in example 1 except that no UV treatment was performed, and the amounts of the other raw materials were used.
Comparative example 4 preparation of titanium dioxide, cesium nitrate, iron nitrate 44: 15:7 (parts per unit). 44 parts of titanium dioxide, 15 parts of cesium nitrate and 7 parts of ferric nitrate. In which the calcination treatment was not carried out in different atmospheres, the procedure was the same as in example 1.
Comparative example 5 titanium dioxide, iron nitrate 44: 15:7 (parts per unit). 44 parts of titanium dioxide and 7 parts of ferric nitrate. The procedure was the same as in example 1 except that cesium nitrate was not added for compounding and the other raw materials were used.
Comparative example 6 preparation of titanium dioxide, cesium nitrate 44: sample 15 (unit parts). 44 parts of titanium dioxide and 15 parts of cesium nitrate. The procedure was the same as in example 1 except that no iron nitrate was added in combination and the other raw materials were used.
And (3) catalytic test: and adding the prepared Cs/Ti-Fe composite photocatalyst into a water sample containing phenolphthalein, and carrying out light irradiation treatment for 20 min. Measuring the UV-Vis spectrum curve before and after the target object (phenolphthalein) is degraded by using a Hitachiuv4100 type ultraviolet-visible spectrometer under the test conditions of slit width of 2nrn and scanning speed of 60nm/min, and calculating the residual concentration of the target object by using the UV-Vis spectrum standard curve of the target object, thereby representing the degradation rate of the target object.
η=（C0One C)/C0×100%
Wherein, C0And C is the concentration of the target degradation product before and after degradation (mg/L), respectively.
TABLE-catalysis test results
| Group of | Phenolphthalein degradation rate% |
| Example 1 | 96.3 |
| Example 2 | 95.6 |
| Example 3 | 69.7 |
| Example 4 | 68.2 |
| Example 5 | 73.3 |
| Example 6 | 76.8 |
| Example 7 | 69.7 |
| Example 8 | 77.3 |
| Example 9 | 65.6 |
| Example 10 | 73.5 |
| Example 11 | 75.7 |
| Example 12 | 68.5 |
| Example 13 | 68.4 |
| Comparative example 1 | 56.9 |
| Comparative example 2 | 44.4 |
| Comparative example 3 | 56.5 |
| Comparative example 4 | 53.1 |
| Comparative example 5 | 33.6 |
| Comparative example 6 | 35.9 |
The experimental results show that: it can be found that the Cs/Ti-Fe composite photocatalyst prepared in comparative example, examples 1 and 2 has the best effect of catalytically degrading phenolphthalein. The raw material ratio has better synergistic effect, and the operation process is most beneficial to synthesizing the Cs/Ti-Fe composite photocatalyst with good catalytic effect. The Cs/Ti-Fe composite photocatalyst prepared by other processes has general catalytic performance. Comparative example 1, comparative examples 1,2,3,4,5, 6 can be found. Carrying out ultrasonic treatment on a titanium dioxide solution, carrying out water bath treatment, carrying out ultraviolet treatment, carrying out calcination treatment under different atmospheres, and adding cesium nitrate and ferric nitrate for composite treatment to obtain the Cs/Ti-Fe composite photocatalyst with better catalytic effect.
Claims (1)
1. A preparation method of a Cs/Ti-Fe composite photocatalyst is characterized by comprising the following steps:
step 1, weighing 44 parts of titanium dioxide powder, dissolving in 200 parts of deionized water, and simultaneously carrying out ultrasonic treatment for 40min to serve as a solvent;
step 2, weighing 15 parts of cesium nitrate and 7 parts of ferric nitrate, dissolving the cesium nitrate and the 7 parts of ferric nitrate in the half of the titanium dioxide solution prepared in the step 1, and stirring in a water bath at 50 ℃ for 2 hours until solutes are completely dissolved;
step 3, simultaneously mixing 10 parts of NaOH and 8 parts of Na2CO3Dissolving the titanium dioxide solution in the other half prepared in the step 1, and stirring the solution in an oil bath at 40 ℃ until the solute is completely dissolved;
step 4, sucking the mixed solution prepared in the step 3 by using a rubber head dropper, dropwise adding the mixed solution into the mixed solution prepared in the step 2 within 30 minutes, and then, finding that the milky solution generates a reddish-brown flocculent precipitate;
step 5, transferring the mixture into a vacuum glove box, and carrying out vibration treatment for 2 hours under a reciprocating type oscillator and simultaneously carrying out ultraviolet treatment;
step 6, then 5 parts of surfactant fatty glyceride are dripped at the speed of 30 drops per minute, and the mixture is stirred in an ice-water bath;
step 7, after the ice-water bath treatment is finished, transferring the mixture into a polytetrafluoroethylene reaction kettle, heating the mixture to 200 ℃ at the speed of 5 ℃/min, and reacting the mixture for 5 hours in a nitrogen atmosphere;
step 8, stopping heating after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, sequentially washing the taken sample with deionized water and ethanol for 5-8 times, and drying in a vacuum drying oven at 120 ℃ for 24 hours;
and 9, calcining in a tube furnace: headFirstly, CO is first introduced2Calcining at 150 ℃ under the atmosphere for 2h under 0.4kPa, then calcining at 180 ℃ under 0.5kPa for 3h under the ammonia atmosphere, and finally calcining at 240 ℃ under 0.6kPa for 4h under the nitrogen atmosphere to finally obtain the Cs/Ti-Fe composite photocatalyst.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1655869A (en) * | 2002-03-25 | 2005-08-17 | 住友钛株式会社 | Titanium oxide-based photocatalyst, manufacturing method therefor and its application |
| CN101254469A (en) * | 2008-04-10 | 2008-09-03 | 杭州电子科技大学 | Preparation of common adulterate nano pipe photochemical catalyst material |
| CN101411982A (en) * | 2008-11-14 | 2009-04-22 | 复旦大学 | Iron modified titanic oxide microsphere photocatalyst as well as method for producing the same and use |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1655869A (en) * | 2002-03-25 | 2005-08-17 | 住友钛株式会社 | Titanium oxide-based photocatalyst, manufacturing method therefor and its application |
| CN101254469A (en) * | 2008-04-10 | 2008-09-03 | 杭州电子科技大学 | Preparation of common adulterate nano pipe photochemical catalyst material |
| CN101411982A (en) * | 2008-11-14 | 2009-04-22 | 复旦大学 | Iron modified titanic oxide microsphere photocatalyst as well as method for producing the same and use |
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