CN108704641A - A kind of preparation method of high-efficiency composite photocatalyst - Google Patents
A kind of preparation method of high-efficiency composite photocatalyst Download PDFInfo
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- CN108704641A CN108704641A CN201810607469.XA CN201810607469A CN108704641A CN 108704641 A CN108704641 A CN 108704641A CN 201810607469 A CN201810607469 A CN 201810607469A CN 108704641 A CN108704641 A CN 108704641A
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- reaction
- chloroplatinic acid
- platinum
- temperature
- titanium dioxide
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 95
- 239000002253 acid Substances 0.000 claims abstract description 72
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 63
- 238000003756 stirring Methods 0.000 claims abstract description 56
- MACBSXIPRLPFDJ-UHFFFAOYSA-N oxygen(2-) platinum(2+) titanium(4+) Chemical compound [O-2].[O-2].[Ti+4].[Pt+2] MACBSXIPRLPFDJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000012153 distilled water Substances 0.000 claims abstract description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 239000006185 dispersion Substances 0.000 claims abstract description 26
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 21
- 239000002270 dispersing agent Substances 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 230000003287 optical effect Effects 0.000 claims abstract description 10
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 14
- MMCOUVMKNAHQOY-UHFFFAOYSA-N carbonoperoxoic acid Chemical compound OOC(O)=O MMCOUVMKNAHQOY-UHFFFAOYSA-N 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 8
- 230000008859 change Effects 0.000 claims description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 37
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 29
- 229910052697 platinum Inorganic materials 0.000 abstract description 19
- 239000004408 titanium dioxide Substances 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 8
- 238000006722 reduction reaction Methods 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 238000001556 precipitation Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 20
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 12
- 239000010936 titanium Substances 0.000 description 12
- 229910052719 titanium Inorganic materials 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- -1 platinum ion Chemical class 0.000 description 7
- 238000006467 substitution reaction Methods 0.000 description 7
- 239000001913 cellulose Substances 0.000 description 6
- 229920002678 cellulose Polymers 0.000 description 6
- 229910000510 noble metal Inorganic materials 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000010970 precious metal Substances 0.000 description 3
- HBBATKAUXPHIQN-UHFFFAOYSA-N [Cl].[Ti] Chemical compound [Cl].[Ti] HBBATKAUXPHIQN-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 238000007540 photo-reduction reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- VHSHLMUCYSAUQU-UHFFFAOYSA-N 2-hydroxypropyl methacrylate Chemical compound CC(O)COC(=O)C(C)=C VHSHLMUCYSAUQU-UHFFFAOYSA-N 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- XEEVLJKYYUVTRC-UHFFFAOYSA-N oxomalonic acid Chemical compound OC(=O)C(=O)C(O)=O XEEVLJKYYUVTRC-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/12—Oxidising
-
- 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
- B01J37/16—Reducing
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to photocatalysis technology fields, and in particular to a kind of preparation method of high-efficiency composite photocatalyst includes the following steps：Step 1, low temperature is added into absolute ethyl alcohol in chloroplatinic acid to stir to being completely dissolved, dispersant is then added and stirs evenly to form chloroplatinic acid dispersion liquid；Step 2, oxalic acid is slowly added dropwise into chloroplatinic acid dispersion liquid until being completely dissolved, ultrasonic reaction 1-2h, then addition titanous chloride sealed thermostat reacts 2-4h, obtains reaction solution；Step 3, distilled water is added and is stirred evenly into reaction solution, vacuum distillation reaction 2-4h obtains platinum-titanium dioxide mixed liquor；Step 4, platinum-titanium dioxide mixed liquor heating stirring is reacted into 30-60min, platinum-titanium dioxide precipitation is then obtained by filtration while hot, platinum-titanium dioxide optical catalyst is obtained after distilled water constant temp.The present invention promotes catalyst by the reduction reaction of titanous chloride and chloroplatinic acid and combines inner, while platinum particles activity is big, and good with the electron-transporting of titanium dioxide, photocatalysis performance is good.
Description
Technical field
The invention belongs to photocatalysis technology fields, and in particular to a kind of preparation method of high-efficiency composite photocatalyst.
Background technology
Currently, titanium dioxide optical catalyst because have many advantages, such as stabilization, it is nontoxic, inexpensive due to cause domestic and international researcher
Extensive concern has broad application prospects in fields such as wastewater treatment, air purification, antibacterial and deodouring, automatically cleanings.Anatase
Single crystal titanium dioxide nanometer sheet has obtained prodigious concern due to high energy active face (001) large percentage.Theoretical and experimental study
Show compared to other active faces, (001) face more efficiently adsorption reaction object molecule, promotion can be catalyzed the progress of reaction.
But lower photo-quantum efficiency and slower reaction rate limit the practical application of titanium dioxide.Photoproduction current-carrying
Son migration, capture and its it is compound between competition determine titanium dioxide nanoplate light-catalyzed reaction quantum efficiency height and
The speed of reaction rate, and titanium dioxide-noble metal compound system is because having special contact interface structure and chemistry and electronics
Property and catalysis react in be widely applied.
There are two types of complex methods for titanium dioxide-noble metal systems：(1) titanium in precious metal atom substitution titanium dioxide is former
Son；(2) noble metal loading is in titanium dioxide surface.The common method of noble metal loading has photoreduction met hod and conventional impregnation reduction
Method.Photoreduction met hod is that semiconductor is immersed in precious metal salt and sacrifices the molten of organic matter (free radical aceeptor, such as acetic acid, methanol)
In liquid, under ultraviolet light, noble metal is reduced and is deposited on titanium dioxide surface；Conventional impregnation reduction method is by dioxy
Change titanium to be immersed in the solution containing precious metal salt, then uses hydrogen high temperature reduction under inert gas protection.Your common gold
Owner will include Pt, Ag, Au, Pd, Ru etc. of third main group, wherein the report in relation to supporting Pt is most, effect is preferably also.
For current preparation method the problem is that step is relatively complicated, energy expenditure is more, and platinum is unevenly distributed.
The Chinese invention patent of Publication No. CN107096519A discloses a kind of platinum dopant nano titanium dioxide photocatalysis
Agent, preparation process are as follows：Step 1, nano-titanium dioxide is added in absolute ethyl alcohol, and HPMA is added as dispersant, stirred
Suspended dispersion liquid is obtained after mixing 2-5h；Step 2, chloroplatinic acid is added in absolute ethyl alcohol, polyvinylpyrrolidone is added, is returned
It flows slightly boiling and reacts 1-2h, then rapid drawdown to low temperature, rotary evaporation forms gel, obtains platinum particles gel；It step 3, will be suspended
Dispersion liquid is put into Ultrasound Instrument, and water bath sonicator while is slowly added to platinum particles gel, until gel is completely dissolved, is hanged
Turbid mixed liquor；Step 4, the suspended mixed liquor of step 3 is sealed ultrasonic reaction 8-12h, cooled to room temperature obtains anti-
Answer liquid；Step 5, reaction solution after cooling is filtered, obtains white particle, then ultraviolet lighting reacts 3-8h, obtains platinum
Doped titanium dioxide photocatalyst.
Although the technical solution simplifies step, improve the dispersing uniformity of platinum element, but platinum is during doping,
Platinum easily aoxidizes in electrolytic process, and the binding force of catalyst is not only caused to decline, but also the activity of platinum is caused to decline.
Invention content
For the problems of the prior art, the present invention provides a kind of preparation method of high-efficiency composite photocatalyst, solves
Prior art platinum activity declines and platinum-bad problem of titanium dioxide binding force, and the reduction by titanous chloride and chloroplatinic acid is anti-
Catalyst should be promoted and combine inner, while platinum particles activity is big, and good with the electron-transporting of titanium dioxide, photocatalysis performance is good.
To realize the above technical purpose, the technical scheme is that：
A kind of preparation method of high-efficiency composite photocatalyst, includes the following steps：
Step 1, low temperature is added into absolute ethyl alcohol in chloroplatinic acid to stir to being completely dissolved, it is equal that dispersant stirring is then added
Even formation chloroplatinic acid dispersion liquid；
Step 2, oxalic acid is slowly added dropwise into chloroplatinic acid dispersion liquid up to being completely dissolved, then ultrasonic reaction 1-2h adds
Enter titanous chloride sealed thermostat reaction 2-4h, obtains reaction solution；
Step 3, distilled water is added and is stirred evenly into reaction solution, vacuum distillation reaction 2-4h obtains platinum-titanium dioxide
Mixed liquor；
Step 4, platinum-titanium dioxide mixed liquor heating stirring is reacted into 30-60min, platinum-dioxy is then obtained by filtration while hot
Change titanium precipitation, platinum-titanium dioxide optical catalyst is obtained after distilled water constant temp.
A concentration of 20-40g/L of the chloroplatinic acid in absolute ethyl alcohol in the step 1, the dispersant are replaced using high
Hydroxypropyl cellulose, the addition of the Hydroxypropylcelliloxe are the 20-40% of chloroplatinic acid quality.
The temperature of low temperature stirring in the step 1 is 20-30 DEG C, mixing speed 500-1000r/min, the stirring
Uniform mixing speed is 1000-2000r/min.
Oxalic acid addition in the step 2 is the 40-70% of chloroplatinic acid quality, and the rate of addition being slowly added dropwise is 2-
The temperature of 5mL/min, the ultrasonic reaction are 30-50 DEG C, supersonic frequency 20-50kHz.
The addition of titanous chloride in the step 2 is the 20-50% of chloroplatinic acid quality, the sealed thermostat reaction
Temperature is 60-90 DEG C.
Percarbonic acid ammonium isothermal reaction 2-4h is added in sealed thermostat after reaction in the step 2, obtains described in step 2
Reaction solution.
The addition of the percarbonic acid ammonium is the 2-6% of chloroplatinic acid quality, and the temperature of the isothermal reaction is 30-40 DEG C.
Distilled water addition in the step 3 is the 80-120% of absolute ethyl alcohol volume, is evaporated under reduced pressure the pressure of reaction
For the 70-80% of atmospheric pressure, temperature is 70-80 DEG C.
The temperature of heating stirring reaction in the step 4 is 70-80 DEG C, and mixing speed 2000-3000r/min takes advantage of
The temperature of heat filtering is 70-80 DEG C.
The temperature of distilled water constant temp in the step 4 is 60-80 DEG C.
Aluminium foil is calculated to be added to low temperature in absolute ethyl alcohol and be stirred by step 1, can form good dissolving, then utilizes dispersion
Aluminum foil acid is dispersed in absolute ethyl alcohol by agent, forms good dispersion.
Step 2 slow transits through oxalic acid in dispersion liquid, is reacted with chloroplatinic acid formation by oxalic acid, by super in reaction system
Phonoresponse fully reacts oxalic acid rapid dispersion to whole system, guarantee oxalic acid with chloroplatinic acid, prevents local accumulation；By chlorination
Titanous is added into dispersion liquid, and evenly dispersed in whole system, in the reproducibility and chlorine of sealing constant voltage process mesoxalic acid
Platinum particles can be restored to by platinum ion under conditions of sealed thermostat by changing the reproducibility of titanous, achieve the purpose that reduction, while chlorine
Change the titanous ionic oxide formation in titanous into titanium ion, and is converted into titanium dioxide under this condition.
Distilled water is added into reaction solution step 3, can form ethanol water with absolute ethyl alcohol, and dispersant exists
Dissolubility can ensure the dispersibility of internal material in water；The mode of vacuum distillation can evaporate absolute ethyl alcohol, and will reaction
Liquid smooth transition is to aqueous solution.
Chlorion can be converted the hydrogen chloride to be formed by the mode of step 4 mixed liquor heating stirring during heating stirring
Vaporization removal, and Hydroxypropylcelliloxe surface goes out good hydrophobicity and gel characteristic, forms platinum-dioxy after filtration
Change titanium precipitation, and precipitate the dispersion effect by Hydroxypropylcelliloxe at this time, forms good dispersibility, therefore obtain
Precipitation dispersibility is splendid.
From the above, it can be seen that the present invention has following advantages：
1. the present invention solves the problems, such as that prior art platinum activity declines and platinum-titanium dioxide binding force is bad, pass through chlorine
The reduction reaction for changing titanous and chloroplatinic acid promotes catalyst and combines inner, while platinum particles activity is big, is passed with the electronics of titanium dioxide
Defeated property is good, and photocatalysis performance is good.
2. the present invention is using solving the problems, such as that titanous ionic oxide formation is incomplete, percarbonic acid ammonium promotes the oxygen of titanous ion
Change, stabilized chlorine titanium can be formed, and reaction is decomposed to form gaseous state after percarbonic acid ammonium excess, residual is not present in a solvent.
3. the photocatalytic of the present invention is good, good stability, anti-toxicity is good.
Specific implementation mode
The specific embodiment that the present invention will be described in detail in conjunction with the embodiments, but the claim of the present invention is not done any
It limits.
Embodiment 1
A kind of preparation method of high-efficiency composite photocatalyst, includes the following steps：
Step 1, low temperature is added into absolute ethyl alcohol in chloroplatinic acid to stir to being completely dissolved, it is equal that dispersant stirring is then added
Even formation chloroplatinic acid dispersion liquid；
Step 2, oxalic acid is slowly added dropwise into chloroplatinic acid dispersion liquid until being completely dissolved, then ultrasonic reaction 1h is added
Titanous chloride sealed thermostat reacts 2h, obtains reaction solution；
Step 3, distilled water is added and is stirred evenly into reaction solution, it is mixed to obtain platinum-titanium dioxide by vacuum distillation reaction 2h
Close liquid；
Step 4, platinum-titanium dioxide mixed liquor heating stirring is reacted into 30min, platinum-titanium dioxide is then obtained by filtration while hot
Titanium precipitates, and platinum-titanium dioxide optical catalyst is obtained after distilled water constant temp.
A concentration of 20g/L of the chloroplatinic acid in absolute ethyl alcohol in the step 1, the dispersant is using high substitution hydroxypropyl
Base cellulose, the addition of the Hydroxypropylcelliloxe are the 20% of chloroplatinic acid quality.
The temperature of low temperature stirring in the step 1 is 20 DEG C, mixing speed 500r/min, it is described stir evenly stir
It is 1000r/min to mix speed.
Oxalic acid addition in the step 2 is the 40% of chloroplatinic acid quality, and the rate of addition being slowly added dropwise is 2mL/
The temperature of min, the ultrasonic reaction are 30 DEG C, supersonic frequency 20kHz.
The addition of titanous chloride in the step 2 is the 20% of chloroplatinic acid quality, the temperature of the sealed thermostat reaction
Degree is 60 DEG C.
Distilled water addition in the step 3 is the 80% of absolute ethyl alcohol volume, and the pressure for being evaporated under reduced pressure reaction is big
The 70% of air pressure, temperature are 70 DEG C.
The temperature of heating stirring reaction in the step 4 is 70 DEG C, and mixing speed 2000r/min is filtered while hot
Temperature is 70 DEG C.
The temperature of distilled water constant temp in the step 4 is 60 DEG C.
Embodiment 2
A kind of preparation method of high-efficiency composite photocatalyst, includes the following steps：
Step 1, low temperature is added into absolute ethyl alcohol in chloroplatinic acid to stir to being completely dissolved, it is equal that dispersant stirring is then added
Even formation chloroplatinic acid dispersion liquid；
Step 2, oxalic acid is slowly added dropwise into chloroplatinic acid dispersion liquid until being completely dissolved, then ultrasonic reaction 2h is added
Titanous chloride sealed thermostat reacts 4h, obtains reaction solution；
Step 3, distilled water is added and is stirred evenly into reaction solution, it is mixed to obtain platinum-titanium dioxide by vacuum distillation reaction 4h
Close liquid；
Step 4, platinum-titanium dioxide mixed liquor heating stirring is reacted into 60min, platinum-titanium dioxide is then obtained by filtration while hot
Titanium precipitates, and platinum-titanium dioxide optical catalyst is obtained after distilled water constant temp.
A concentration of 40g/L of the chloroplatinic acid in absolute ethyl alcohol in the step 1, the dispersant is using high substitution hydroxypropyl
Base cellulose, the addition of the Hydroxypropylcelliloxe are the 40% of chloroplatinic acid quality.
The temperature of low temperature stirring in the step 1 is 30 DEG C, mixing speed 1000r/min, described to stir evenly
Mixing speed is 2000r/min.
Oxalic acid addition in the step 2 is chloroplatinic acid quality 70%, and the rate of addition being slowly added dropwise is 5mL/min,
The temperature of the ultrasonic reaction is 50 DEG C, supersonic frequency 50kHz.
The addition of titanous chloride in the step 2 is the 50% of chloroplatinic acid quality, the temperature of the sealed thermostat reaction
Degree is 90 DEG C.
Distilled water addition in the step 3 is the 120% of absolute ethyl alcohol volume, and the pressure for being evaporated under reduced pressure reaction is big
The 80% of air pressure, temperature are 80 DEG C.
The temperature of heating stirring reaction in the step 4 is 80 DEG C, and mixing speed 3000r/min is filtered while hot
Temperature is 80 DEG C.
The temperature of distilled water constant temp in the step 4 is 80 DEG C.
Embodiment 3
A kind of preparation method of high-efficiency composite photocatalyst, includes the following steps：
Step 1, low temperature is added into absolute ethyl alcohol in chloroplatinic acid to stir to being completely dissolved, it is equal that dispersant stirring is then added
Even formation chloroplatinic acid dispersion liquid；
Step 2, oxalic acid is slowly added dropwise into chloroplatinic acid dispersion liquid until being completely dissolved, then ultrasonic reaction 2h is added
Titanous chloride sealed thermostat reacts 3h, obtains reaction solution；
Step 3, distilled water is added and is stirred evenly into reaction solution, it is mixed to obtain platinum-titanium dioxide by vacuum distillation reaction 3h
Close liquid；
Step 4, platinum-titanium dioxide mixed liquor heating stirring is reacted into 50min, platinum-titanium dioxide is then obtained by filtration while hot
Titanium precipitates, and platinum-titanium dioxide optical catalyst is obtained after distilled water constant temp.
A concentration of 30g/L of the chloroplatinic acid in absolute ethyl alcohol in the step 1, the dispersant is using high substitution hydroxypropyl
Base cellulose, the addition of the Hydroxypropylcelliloxe are the 30% of chloroplatinic acid quality.
The temperature of low temperature stirring in the step 1 is 25 DEG C, mixing speed 800r/min, it is described stir evenly stir
It is 1500r/min to mix speed.
Oxalic acid addition in the step 2 is the 60% of chloroplatinic acid quality, and the rate of addition being slowly added dropwise is 4mL/
The temperature of min, the ultrasonic reaction are 40 DEG C, supersonic frequency 30kHz.
The addition of titanous chloride in the step 2 is the 40% of chloroplatinic acid quality, the temperature of the sealed thermostat reaction
Degree is 80 DEG C.
Distilled water addition in the step 3 is the 110% of absolute ethyl alcohol volume, and the pressure for being evaporated under reduced pressure reaction is big
The 70% of air pressure, temperature are 75 DEG C.
The temperature of heating stirring reaction in the step 4 is 75 DEG C, and mixing speed 2500r/min is filtered while hot
Temperature is 75 DEG C.
The temperature of distilled water constant temp in the step 4 is 70 DEG C.
Embodiment 4
A kind of preparation method of high-efficiency composite photocatalyst, includes the following steps：
Step 1, low temperature is added into absolute ethyl alcohol in chloroplatinic acid to stir to being completely dissolved, it is equal that dispersant stirring is then added
Even formation chloroplatinic acid dispersion liquid；
Step 2, oxalic acid is slowly added dropwise into chloroplatinic acid dispersion liquid until being completely dissolved, then ultrasonic reaction 1h is added
Titanous chloride sealed thermostat reacts 2h, and sealed thermostat is added percarbonic acid ammonium isothermal reaction 2h, obtains reaction solution after reaction；Institute
The addition for stating percarbonic acid ammonium is the 2% of chloroplatinic acid quality, and the temperature of the isothermal reaction is 30 DEG C；
Step 3, distilled water is added and is stirred evenly into reaction solution, it is mixed to obtain platinum-titanium dioxide by vacuum distillation reaction 2h
Close liquid；
Step 4, platinum-titanium dioxide mixed liquor heating stirring is reacted into 30min, platinum-titanium dioxide is then obtained by filtration while hot
Titanium precipitates, and platinum-titanium dioxide optical catalyst is obtained after distilled water constant temp.
A concentration of 20g/L of the chloroplatinic acid in absolute ethyl alcohol in the step 1, the dispersant is using high substitution hydroxypropyl
Base cellulose, the addition of the Hydroxypropylcelliloxe are the 20% of chloroplatinic acid quality.
The temperature of low temperature stirring in the step 1 is 20 DEG C, mixing speed 500r/min, it is described stir evenly stir
It is 1000r/min to mix speed.
Oxalic acid addition in the step 2 is the 40% of chloroplatinic acid quality, and the rate of addition being slowly added dropwise is 2mL/
The temperature of min, the ultrasonic reaction are 30 DEG C, supersonic frequency 20kHz.
The addition of titanous chloride in the step 2 is the 20% of chloroplatinic acid quality, the temperature of the sealed thermostat reaction
Degree is 60 DEG C.
Distilled water addition in the step 3 is the 80% of absolute ethyl alcohol volume, and the pressure for being evaporated under reduced pressure reaction is big
The 70% of air pressure, temperature are 70 DEG C.
The temperature of heating stirring reaction in the step 4 is 70 DEG C, and mixing speed 2000r/min is filtered while hot
Temperature is 70 DEG C.
The temperature of distilled water constant temp in the step 4 is 60 DEG C.
Embodiment 5
A kind of preparation method of high-efficiency composite photocatalyst, includes the following steps：
Step 1, low temperature is added into absolute ethyl alcohol in chloroplatinic acid to stir to being completely dissolved, it is equal that dispersant stirring is then added
Even formation chloroplatinic acid dispersion liquid；
Step 2, oxalic acid is slowly added dropwise into chloroplatinic acid dispersion liquid until being completely dissolved, then ultrasonic reaction 2h is added
Titanous chloride sealed thermostat reacts 4h, and sealed thermostat is added percarbonic acid ammonium isothermal reaction 4h, obtains reaction solution after reaction；Institute
The addition for stating percarbonic acid ammonium is the 6% of chloroplatinic acid quality, and the temperature of the isothermal reaction is 40 DEG C；
Step 3, distilled water is added and is stirred evenly into reaction solution, it is mixed to obtain platinum-titanium dioxide by vacuum distillation reaction 4h
Close liquid；
Step 4, platinum-titanium dioxide mixed liquor heating stirring is reacted into 60min, platinum-titanium dioxide is then obtained by filtration while hot
Titanium precipitates, and platinum-titanium dioxide optical catalyst is obtained after distilled water constant temp.
A concentration of 40g/L of the chloroplatinic acid in absolute ethyl alcohol in the step 1, the dispersant is using high substitution hydroxypropyl
Base cellulose, the addition of the Hydroxypropylcelliloxe are the 40% of chloroplatinic acid quality.
The temperature of low temperature stirring in the step 1 is 30 DEG C, mixing speed 1000r/min, described to stir evenly
Mixing speed is 2000r/min.
Oxalic acid addition in the step 2 is chloroplatinic acid quality 70%, and the rate of addition being slowly added dropwise is 5mL/min,
The temperature of the ultrasonic reaction is 50 DEG C, supersonic frequency 50kHz.
The addition of titanous chloride in the step 2 is the 50% of chloroplatinic acid quality, the temperature of the sealed thermostat reaction
Degree is 90 DEG C.
Distilled water addition in the step 3 is the 120% of absolute ethyl alcohol volume, and the pressure for being evaporated under reduced pressure reaction is big
The 80% of air pressure, temperature are 80 DEG C.
The temperature of heating stirring reaction in the step 4 is 80 DEG C, and mixing speed 3000r/min is filtered while hot
Temperature is 80 DEG C.
The temperature of distilled water constant temp in the step 4 is 80 DEG C.
Embodiment 6
A kind of preparation method of high-efficiency composite photocatalyst, includes the following steps：
Step 1, low temperature is added into absolute ethyl alcohol in chloroplatinic acid to stir to being completely dissolved, it is equal that dispersant stirring is then added
Even formation chloroplatinic acid dispersion liquid；
Step 2, oxalic acid is slowly added dropwise into chloroplatinic acid dispersion liquid until being completely dissolved, then ultrasonic reaction 2h is added
Titanous chloride sealed thermostat reacts 3h, and sealed thermostat is added percarbonic acid ammonium isothermal reaction 3h, obtains reaction solution after reaction；Institute
The addition for stating percarbonic acid ammonium is the 4% of chloroplatinic acid quality, and the temperature of the isothermal reaction is 35 DEG C；
Step 3, distilled water is added and is stirred evenly into reaction solution, it is mixed to obtain platinum-titanium dioxide by vacuum distillation reaction 3h
Close liquid；
Step 4, platinum-titanium dioxide mixed liquor heating stirring is reacted into 50min, platinum-titanium dioxide is then obtained by filtration while hot
Titanium precipitates, and platinum-titanium dioxide optical catalyst is obtained after distilled water constant temp.
A concentration of 30g/L of the chloroplatinic acid in absolute ethyl alcohol in the step 1, the dispersant is using high substitution hydroxypropyl
Base cellulose, the addition of the Hydroxypropylcelliloxe are the 30% of chloroplatinic acid quality.
The temperature of low temperature stirring in the step 1 is 25 DEG C, mixing speed 800r/min, it is described stir evenly stir
It is 1500r/min to mix speed.
Oxalic acid addition in the step 2 is the 60% of chloroplatinic acid quality, and the rate of addition being slowly added dropwise is 4mL/
The temperature of min, the ultrasonic reaction are 40 DEG C, supersonic frequency 30kHz.
The addition of titanous chloride in the step 2 is the 40% of chloroplatinic acid quality, the temperature of the sealed thermostat reaction
Degree is 80 DEG C.
Distilled water addition in the step 3 is the 110% of absolute ethyl alcohol volume, and the pressure for being evaporated under reduced pressure reaction is big
The 70% of air pressure, temperature are 75 DEG C.
The temperature of heating stirring reaction in the step 4 is 75 DEG C, and mixing speed 2500r/min is filtered while hot
Temperature is 75 DEG C.
The temperature of distilled water constant temp in the step 4 is 70 DEG C.
Performance detection
In conclusion the present invention has the following advantages：
1. the present invention solves the problems, such as that prior art platinum activity declines and platinum-titanium dioxide binding force is bad, pass through chlorine
The reduction reaction for changing titanous and chloroplatinic acid promotes catalyst and combines inner, while platinum particles activity is big, is passed with the electronics of titanium dioxide
Defeated property is good, and photocatalysis performance is good.
2. the present invention is using solving the problems, such as that titanous ionic oxide formation is incomplete, percarbonic acid ammonium promotes the oxygen of titanous ion
Change, stabilized chlorine titanium can be formed, and reaction is decomposed to form gaseous state after percarbonic acid ammonium excess, residual is not present in a solvent.
3. the photocatalytic of the present invention is good, good stability, anti-toxicity is good.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
Technical solution described in inventive embodiments.It will be understood by those of ordinary skill in the art that still can be carried out to the present invention
Modification or equivalent replacement, to reach identical technique effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of preparation method of high-efficiency composite photocatalyst, which is characterized in that include the following steps：
Step 1, low temperature is added into absolute ethyl alcohol in chloroplatinic acid to stir to being completely dissolved, dispersant is then added and stirs evenly shape
At chloroplatinic acid dispersion liquid；
Step 2, oxalic acid is slowly added dropwise into chloroplatinic acid dispersion liquid until being completely dissolved, then chlorine is added in ultrasonic reaction 1-2h
Change titanous sealed thermostat and react 2-4h, obtains reaction solution；
Step 3, distilled water is added and is stirred evenly into reaction solution, vacuum distillation reaction 2-4h obtains platinum-titanium dioxide mixing
Liquid；
Step 4, platinum-titanium dioxide mixed liquor heating stirring is reacted into 30-60min, platinum-titanium dioxide is then obtained by filtration while hot
It precipitates, platinum-titanium dioxide optical catalyst is obtained after distilled water constant temp.
2. a kind of preparation method of high-efficiency composite photocatalyst according to claim 1, it is characterised in that：The step 1
In a concentration of 20-40g/L of the chloroplatinic acid in absolute ethyl alcohol, the dispersant uses Hydroxypropylcelliloxe, described
The addition of Hydroxypropylcelliloxe is the 20-40% of chloroplatinic acid quality.
3. a kind of preparation method of high-efficiency composite photocatalyst according to claim 1, it is characterised in that：The step 1
In the temperature of low temperature stirring be 20-30 DEG C, mixing speed 500-1000r/min, the mixing speed stirred evenly is
1000-2000r/min。
4. a kind of preparation method of high-efficiency composite photocatalyst according to claim 1, it is characterised in that：The step 2
In oxalic acid addition be chloroplatinic acid quality 40-70%, the rate of addition being slowly added dropwise is 2-5mL/min, and the ultrasound is anti-
The temperature answered is 30-50 DEG C, supersonic frequency 20-50kHz.
5. a kind of preparation method of high-efficiency composite photocatalyst according to claim 1, it is characterised in that：The step 2
In titanous chloride addition be chloroplatinic acid quality 20-50%, the temperature of sealed thermostat reaction is 60-90 DEG C.
6. a kind of preparation method of high-efficiency composite photocatalyst according to claim 1, it is characterised in that：The step 2
Percarbonic acid ammonium isothermal reaction 2-4h is added in middle sealed thermostat after reaction, obtains the reaction solution described in step 2.
7. a kind of preparation method of high-efficiency composite photocatalyst according to claim 6, it is characterised in that：The percarbonic acid
The addition of ammonium is the 2-6% of chloroplatinic acid quality, and the temperature of the isothermal reaction is 30-40 DEG C.
8. a kind of preparation method of high-efficiency composite photocatalyst according to claim 1, it is characterised in that：The step 3
In distilled water addition be absolute ethyl alcohol volume 80-120%, be evaporated under reduced pressure reaction pressure be atmospheric pressure 70-80%,
Temperature is 70-80 DEG C.
9. a kind of preparation method of high-efficiency composite photocatalyst according to claim 1, it is characterised in that：The step 4
In heating stirring reaction temperature be 70-80 DEG C, mixing speed 2000-3000r/min, the temperature filtered while hot be 70-
80℃。
10. a kind of preparation method of high-efficiency composite photocatalyst according to claim 1, it is characterised in that：The step 4
In distilled water constant temp temperature be 60-80 DEG C.
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Application publication date: 20181026 |