CN107233922B - A kind of stone-like C2O7Ti2·3H2O photochemical catalyst and preparation method thereof - Google Patents
A kind of stone-like C2O7Ti2·3H2O photochemical catalyst and preparation method thereof Download PDFInfo
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- CN107233922B CN107233922B CN201710462044.XA CN201710462044A CN107233922B CN 107233922 B CN107233922 B CN 107233922B CN 201710462044 A CN201710462044 A CN 201710462044A CN 107233922 B CN107233922 B CN 107233922B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- 239000010936 titanium Substances 0.000 claims abstract description 62
- 230000001699 photocatalysis Effects 0.000 claims abstract description 52
- 238000007146 photocatalysis Methods 0.000 claims abstract description 50
- 239000000843 powder Substances 0.000 claims abstract description 47
- 239000007787 solid Substances 0.000 claims abstract description 28
- 230000001376 precipitating effect Effects 0.000 claims abstract description 27
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 22
- HHDOORYZQSEMGM-UHFFFAOYSA-L potassium;oxalate;titanium(4+) Chemical compound [K+].[Ti+4].[O-]C(=O)C([O-])=O HHDOORYZQSEMGM-UHFFFAOYSA-L 0.000 claims abstract description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 210000000232 gallbladder Anatomy 0.000 claims 1
- BBJSDUUHGVDNKL-UHFFFAOYSA-J oxalate;titanium(4+) Chemical compound [Ti+4].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O BBJSDUUHGVDNKL-UHFFFAOYSA-J 0.000 claims 1
- -1 polytetrafluoroethylene Polymers 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 239000005416 organic matter Substances 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 18
- 239000007788 liquid Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000002045 lasting effect Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002254 LaCoO3 Inorganic materials 0.000 description 1
- 241000403354 Microplus Species 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000161 silver phosphate Inorganic materials 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
- B01J31/223—At least two oxygen atoms present in one at least bidentate or bridging ligand
- B01J31/2239—Bridging ligands, e.g. OAc in Cr2(OAc)4, Pt4(OAc)8 or dicarboxylate ligands
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The present invention provides a kind of stone-like C2O7Ti2·3H2O photochemical catalyst and preparation method thereof.Stone-like C2O7Ti2·3H2The preparation method of O photocatalysis powder is the following steps are included: (1) prepares titanium potassium oxalate solution；(2) concentrated hydrochloric acid is added into titanium potassium oxalate solution, mixed solution is made, solid precipitating is made through hydro-thermal reaction；(3) obtained solid precipitating washed using deionized water and dehydrated alcohol, dried, novel stone-like C is made2O7Ti2·3H2O photocatalysis powder.The present invention passes through to stone-like C2O7Ti2·3H2The preparation method and preparation condition of O photocatalysis powder are defined, and realize prepare stone-like C using hydrothermal reaction at low temperature for the first time2O7Ti2·3H2O photocatalysis powder simplifies stone-like C2O7Ti2·3H2The preparation process of O photocatalysis powder reduces preparation cost.There is preferable photocatalysis performance using photochemical catalyst prepared by preparation method of the invention, can under ultraviolet or visible light effective decomposing organic matter, achieve the purpose that the depollution of environment.
Description
Technical field
The present invention relates to photocatalysis technology field, especially a kind of stone-like C2O7Ti2·3H2O photochemical catalyst and its preparation
Method.
Background technique
Environmental pollution and energy shortage are the common issues that the current whole world is faced, therefore effective use solar energy etc. is natural
Resource solves the problems, such as environmental pollution and energy shortage is one of research hotspot of the world today.1970s, because
Fujishima and Houda has found by light activated TiO2It can be photocatalysis after hydrogen and oxygen water decomposition on electrode
Oxidation technology comes into being.With further going deep into for research, it has been found that remove TiO2In addition, many semiconductor materials such as ZnO2、
W2O3Deng also with photocatalysis performance.In recent years, some novel photochemical catalysts are also constantly reported, including Was Used compound
CdS、Bi2O3、g-C3N4, three element compound L aFeO3、LaCoO3、Ag3PO4、BiPO4, BiOX (X=Cl, Br, I),
Bi2O2CO3、 Bi2WO6、FeVO4And four element compound Bi1.5ZnTa1.5O7(α-BZT)、Bi2Zn2/3Ta4/3O7(β-BZT)
Deng, but influenced by actual production efficiency and cost, existing photochemical catalyst is not widely used.Therefore, such as
What provides a kind of high production efficiency, photochemical catalyst at low cost and with highlight catalytic active becomes grinding for photocatalysis technology field
Study carefully emphasis.
In view of this, it is necessory to be improved to existing photochemical catalyst, to solve the above problems.
Summary of the invention
In view of the above problems, the purpose of the present invention is to provide a kind of novel stone-like C2O7Ti2·3H2O light
It is catalyzed powder, the novel stone-like C2O7Ti2·3H2The high and low cost of the photocatalytic activity of O photocatalysis powder and can be through simple side
One step of method is made.
The technical scheme is that a kind of stone-like C2O7Ti2·3H2The preparation method of O photochemical catalyst, including it is following
Step:
(1) with titanium potassium oxalate [K2TiO(C2O4)2] it is titanium source, deionized water is solvent, prepares titanium potassium oxalate solution；
(2) concentrated hydrochloric acid is added in the titanium potassium oxalate solution prepared in Xiang Suoshu step (1), mixed solution is made, and will mix
Conjunction solution, which is transferred in reaction kettle, to be heated, and solid precipitating is made through hydro-thermal reaction；
(3) the solid precipitating in the step (2) is washed, and the solid precipitating after washing is dried, with
Novel stone-like C is made2O7Ti2·3H2O photocatalysis powder.
Further, the step (1) specifically: titanium potassium oxalate is add to deionized water, through 30-40 DEG C it is micro- plus
Heat stirs 20-40min, and the titanium potassium oxalate solution that concentration is 0.10-0.20mol/L is made.
Further, the step (2) specifically:
(2.1) concentrated hydrochloric acid that concentration is 37% is added dropwise in Xiang Suoshu step (1) in titanium potassium oxalate solution obtained, knot is added dropwise
Shu Hou stirs 25-35min, mixed solution is made；
(2.2) in step (2.1) mixed solution carry out it is still aging, and will be still aging after mixed solution transfer
Hydro-thermal reaction is carried out, into reaction kettle solid precipitating is made.
Further, the still aging 6-24h under closed environment of the mixed solution in the step (2.2), is then shifted
It is heated into the hydrothermal reaction kettle with polytetrafluoroethylliner liner.
Further, in the step (2.2), the hydrothermal reaction kettle for being contained with mixed solution is transferred in baking oven
Hydro-thermal reaction is carried out, the hydrothermal temperature for controlling the hydro-thermal reaction is 120 DEG C -150 DEG C, and the hydro-thermal time is 10h-18h, with
Solid precipitating is made.
Further, the step (3) specifically:
(3.1) solid obtained in the step (2) precipitating is washed, and the solid precipitating after washing is divided again
From；
(3.2) the solid precipitating in the step (3.1) is dried, produces stone-like C2O7Ti2·3H2O light is urged
Change powder.
Further, in the step (3.1), solid precipitating is washed using deionized water, to cleaning solution
The pH value of supernatant liquor when being neutral, washing terminates.
Further, the step (3.1) washs solid precipitating using deionized water, to the upper of cleaning solution
When the pH value of layer clear liquid is neutral, solid precipitating wash 3-5 times again using dehydrated alcohol.
Further, in the step (3.2), the temperature for controlling the drying is 75 DEG C -85 DEG C, to prevent the stone
Shape C2O7Ti2·3H2The pattern of O photocatalysis powder changes.
For achieving the above object, the present invention provides a kind of photochemical catalyst, the main component of aforementioned photochemical catalyst is
C2O7Ti2·3H2O photocatalysis powder, wherein the stone-like C2O7Ti2·3H2O photocatalysis powder is through aforementioned stone-like
C2O7Ti2·3H2The preparation method of O photocatalysis powder is prepared.
Compared with prior art, the beneficial effects of the present invention are: the present invention passes through to stone-like C2O7Ti2·3H2O light is urged
Change raw powder's production technology and preparation condition is defined, this substance is used in photocatalysis for the first time, is realized for the first time using low temperature
Hydro-thermal method prepares stone-like C2O7Ti2·3H2O photocatalysis powder, and Post isothermal treatment is not necessarily in preparation process, simplify stone-like
C2O7Ti2·3H2The preparation process of O photocatalysis powder reduces preparation cost.Use stone-like C of the invention2O7Ti2·3H2O light
The photochemical catalyst for being catalyzed raw powder's production technology preparation has preferable photocatalysis performance, can effectively divide under ultraviolet or visible light
Organic matter is solved, achievees the purpose that the depollution of environment.
Detailed description of the invention
Fig. 1 is stone-like C prepared by the embodiment of the present invention 12O7Ti2·3H2The low power SEM photo of O photocatalysis powder.
Fig. 2 is stone-like C prepared by the embodiment of the present invention 12O7Ti2·3H2The high power SEM photo of O photocatalysis powder.
Fig. 3 is stone-like C prepared by the embodiment of the present invention 12O7Ti2·3H2The XRD spectra of O photocatalysis powder.
Fig. 4 is the photochemical catalyst of the preparation of the embodiment of the present invention 1 under ultraviolet light to the degradation curve figure of methyl orange solution.
Fig. 5 is the photochemical catalyst of the preparation of the embodiment of the present invention 1 under visible light to the degradation curve figure of methyl orange solution.
Fig. 6 is stone-like C prepared by the embodiment of the present invention 22O7Ti2·3H2The low power SEM photo of O photocatalysis powder.
Fig. 7 is stone-like C prepared by the embodiment of the present invention 22O7Ti2·3H2The high power SEM photo of O photocatalysis powder.
Fig. 8 is stone-like C prepared by the embodiment of the present invention 22O7Ti2·3H2The XRD spectra of O photocatalysis powder.
Fig. 9 is the photochemical catalyst of the preparation of the embodiment of the present invention 2 under ultraviolet light to the degradation curve figure of methyl orange solution.
Stone-like C prepared by Figure 10 embodiment of the present invention 22O7Ti2·3H2The surface photovoltaic spectroscopy of O photocatalysis powder.
Figure 11 is stone-like C prepared by the embodiment of the present invention 42O7Ti2·3H2The low power SEM photo of O photocatalysis powder.
Figure 12 is stone-like C prepared by the embodiment of the present invention 42O7Ti2·3H2The high power of bulky grain in O photocatalysis powder
SEM photograph.
Figure 13 is stone-like C prepared by the embodiment of the present invention 42O7Ti2·3H2The high power of O photocatalysis powder small particles
SEM photograph.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples.
Embodiment 1
1.58g titanium potassium oxalate is taken, 30ml deionized water is added, it is molten to configure titanium potassium oxalate by 35 DEG C of micro- heating stirring 25mim
Liquid, concentration 0.15mol/L.Continue to stir after dissolution, the concentrated hydrochloric acid that 4.5mL concentration is 37% is added dropwise while stirring, continues
Closed standing 10h after stirring 30min, is then transferred into the hydrothermal reaction kettle containing polytetrafluoroethylliner liner, carries out hydro-thermal reaction
12h, hydrothermal temperature are 120 DEG C.It is cooled to room temperature after the completion of hydro-thermal reaction and solid precipitating is taken to be washed with deionized to cleaning solution
After the pH of supernatant liquor is neutral, is precipitated 3-5 times using dehydrated alcohol washing solid, finally dry, can be obtained at 80 DEG C
Stone-like C2O7Ti2·3H2O photocatalysis powder.
Shown in Fig. 1 to Fig. 2, for the stone-like C of the preparation of the embodiment of the present invention 12O7Ti2·3H2The surface of O photocatalysis powder
Pattern schematic diagram, the stone-like C prepared using the embodiment of the present invention 12O7Ti2·3H2O photocatalysis powder is that stratiform stack forms
Stone-like bulky grain.
Shown in Fig. 3, for the stone-like C of the preparation of the embodiment of the present invention 12O7Ti2·3H2The XRD spectrogram of O photocatalysis powder,
The stone-like C prepared using the embodiment of the present invention 12O7Ti2·3H2O photocatalysis powder mainly includes C2O7Ti2·3H2O。
As shown in figure 4, the degradation curve figure of the methyl orange solution for photochemical catalyst provided by the invention.Specifically, originally
The photochemical catalyst main component of invention is stone-like C2O7Ti2·3H2O photocatalysis powder, and stone-like C2O7Ti2·3H2O light is urged
Change the preparation method of powder through the invention to be prepared.Compared with traditional photochemical catalyst, preparation method system of the invention is used
Standby stone-like C2O7Ti2·3H2O photocatalysis powder has higher photocatalytic activity, the lower 2 hours catalytic efficiencies of ultraviolet light
Reach 92.1%, it is seen that the lower 5 hours catalytic efficiencies of light reach 82.5%.
Embodiment 2
3.16g titanium potassium oxalate is taken, 60ml deionized water is added, micro- heating stirring 35mim configures titanium potassium oxalate solution,
Concentration is 0.15mol/L.Continue to stir after dissolution, the concentrated hydrochloric acid that 3mL concentration is 37% is added dropwise while stirring, it is lasting to stir
Closed standing 10h, is then transferred into the hydrothermal reaction kettle containing polytetrafluoroethylliner liner after 30min, carries out hydro-thermal reaction 12h,
Hydrothermal temperature is 120 DEG C.It is cooled to room temperature that take solid precipitating to be washed with deionized upper to cleaning solution after the completion of hydro-thermal reaction
The pH of layer clear liquid is neutrality, finally dries at 80 DEG C, stone-like C can be obtained2O7Ti2·3H2O photocatalysis powder.
Embodiment 3
1.58g titanium potassium oxalate is taken, 30ml deionized water is added, micro- heating stirring 25mim configures titanium potassium oxalate solution,
Concentration is 0.15mol/L.Continue to stir after dissolution, the concentrated hydrochloric acid that 4.5mL concentration is 37% is added dropwise while stirring, it is lasting to stir
Closed standing 10h, is then transferred into the hydrothermal reaction kettle containing polytetrafluoroethylliner liner after 30min, carries out hydro-thermal reaction 12h,
Hydrothermal temperature is 150 DEG C.It is cooled to room temperature that take solid precipitating to be washed with deionized upper to cleaning solution after the completion of hydro-thermal reaction
The pH of layer clear liquid is neutrality, finally dries at 80 DEG C, stone-like C can be obtained2O7Ti2·3H2O photocatalysis powder.
Embodiment 4
3.16g titanium potassium oxalate is taken, 60ml deionized water is added, micro- heating stirring 25mim configures titanium potassium oxalate solution,
Concentration is 0.15mol/L.Continue to stir after dissolution, the concentrated hydrochloric acid that 3mL concentration is 37% is added dropwise while stirring, it is lasting to stir
Closed standing 10h, is then transferred into the hydrothermal reaction kettle containing polytetrafluoroethylliner liner after 30min, carries out hydro-thermal reaction 12h,
Hydrothermal temperature is 150 DEG C.It is cooled to room temperature that take solid precipitating to be washed with deionized upper to cleaning solution after the completion of hydro-thermal reaction
The pH of layer clear liquid is neutrality, finally dries at 80 DEG C, stone-like C can be obtained2O7Ti2·3H2O photocatalysis powder.
The present invention passes through to stone-like C2O7Ti2·3H2O photocatalysis powder prepare raw material and preparation method is selected,
On the one hand, it is ensured that stone-like C2O7Ti2·3H2The photocatalysis effect of O photocatalysis powder；On the other hand, stone-like is reduced
C2O7Ti2·3H2The production cost of O photocatalysis powder simplifies stone-like C2O7Ti2·3H2The synthesis of O photocatalysis powder walks
Suddenly, be conducive to improve stone-like C2O7Ti2·3H2The use scope of O photocatalysis powder.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (9)
1. a kind of stone-like C2O7Ti2·3H2The preparation method of O photochemical catalyst, which comprises the following steps:
(1) with titanium potassium oxalate [K2TiO(C2O4)2] it is titanium source, deionized water is solvent, prepares the titanium oxalate of 0.10-0.20mol/L
Potassium solution；
(2) 37% concentrated hydrochloric acid is added in the titanium potassium oxalate solution prepared in Xiang Suoshu step (1), mixed solution is made, and will
Mixed solution still aging 6-24h under closed environment, is transferred in reaction kettle, 120 DEG C of -150 DEG C of hydro-thermal reaction 10-18h, warp
Solid precipitating is made in hydro-thermal reaction；
(3) the solid precipitating in the step (2) is washed, and the solid precipitating after washing is dried, to be made
Stone-like C2O7Ti2·3H2O photocatalysis powder.
2. a kind of stone-like C according to claim 12O7Ti2·3H2The preparation method of O photochemical catalyst, which is characterized in that
The step (1) specifically: titanium potassium oxalate is add to deionized water, heating temperature is 30-40 DEG C, 20-40min is stirred,
The titanium potassium oxalate solution that concentration is 0.10-0.20mol/L is made.
3. a kind of stone-like C according to claim 12O7Ti2·3H2The preparation method of O photochemical catalyst, which is characterized in that
The step (2) specifically:
(2.1) concentrated hydrochloric acid that concentration is 37% is added dropwise in Xiang Suoshu step (1) in titanium potassium oxalate solution obtained, after completion of dropwise addition
25-35min is stirred, mixed solution is made；
(2.2) in step (2.1) mixed solution carry out it is still aging, and will be still aging after mixed solution be transferred to instead
It answers and carries out hydro-thermal reaction in kettle, solid precipitating is made.
4. a kind of stone-like C according to claim 32O7Ti2·3H2The preparation method of O photochemical catalyst, which is characterized in that
Mixed solution in the step (2.2) the still aging 6-24h under closed environment, is then transferred into in polytetrafluoroethylene (PTFE)
It is heated in the hydrothermal reaction kettle of gallbladder.
5. a kind of stone-like C according to claim 12O7Ti2·3H2The preparation method of O photochemical catalyst, which is characterized in that
The step (3) specifically:
(3.1) solid obtained in the step (2) precipitating is washed, and the solid precipitating after washing is separated again；
(3.2) the solid precipitating in the step (3.1) is dried, produces stone-like C2O7Ti2·3H2O photocatalysis powder.
6. a kind of stone-like C according to claim 52O7Ti2·3H2The preparation method of O photochemical catalyst, which is characterized in that
In the step (3.1), solid precipitating is washed using deionized water, the pH value of the supernatant liquor to cleaning solution is
When neutral, washing terminates.
7. a kind of stone-like C according to claim 52O7Ti2·3H2The preparation method of O photochemical catalyst, which is characterized in that
The step (3.1) washs solid precipitating using deionized water, during the pH value of the supernatant liquor to cleaning solution is
Property when, using dehydrated alcohol to the solid precipitating carry out again wash 3-5 times.
8. a kind of stone-like C according to claim 52O7Ti2·3H2The preparation method of O photochemical catalyst, which is characterized in that
In the step (3.2), the temperature for controlling the drying is 75 DEG C -85 DEG C.
9. a kind of photochemical catalyst, which is characterized in that the main component of the photochemical catalyst is stone-like C2O7Ti2·3H2O photocatalysis
Powder, the stone-like C2O7Ti2·3H2O photocatalysis powder is through the described in any item stone-like C of claim 1~62O7Ti2·
3H2The preparation method of O photochemical catalyst is prepared.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710462044.XA CN107233922B (en) | 2017-06-19 | 2017-06-19 | A kind of stone-like C2O7Ti2·3H2O photochemical catalyst and preparation method thereof |
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