CN108295844B - Palladium-doped nano TiO2Method for preparing powder - Google Patents
Palladium-doped nano TiO2Method for preparing powder Download PDFInfo
- Publication number
- CN108295844B CN108295844B CN201810095034.1A CN201810095034A CN108295844B CN 108295844 B CN108295844 B CN 108295844B CN 201810095034 A CN201810095034 A CN 201810095034A CN 108295844 B CN108295844 B CN 108295844B
- Authority
- CN
- China
- Prior art keywords
- palladium
- graphite plate
- powder
- doped nano
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000843 powder Substances 0.000 title claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 47
- 239000010439 graphite Substances 0.000 claims abstract description 47
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 30
- 239000000084 colloidal system Substances 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000010298 pulverizing process Methods 0.000 claims abstract description 5
- 238000007790 scraping Methods 0.000 claims abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 241000733322 Platea Species 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 13
- 239000011941 photocatalyst Substances 0.000 abstract description 6
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 12
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 11
- 229910052763 palladium Inorganic materials 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- -1 palladium ions Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
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
- B01J23/44—Palladium
-
- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/033—Using Hydrolysis
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/038—Precipitation; Co-precipitation to form slurries or suspensions, e.g. a washcoat
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/342—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electric, magnetic or electromagnetic fields, e.g. for magnetic separation
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Electromagnetism (AREA)
- Optics & Photonics (AREA)
- Plasma & Fusion (AREA)
- Catalysts (AREA)
Abstract
Palladium-doped nano TiO2A preparation method of powder, belonging to the technical field of materials. The method comprises the following steps: adding palladium acetylacetonate into absolute ethyl alcohol, and uniformly stirring to obtain a mixed solution; dropwise adding 70-80 ml of isopropyl titanate into the mixed solution under the stirring condition, and continuously stirring for 0.5-1 h after dropwise adding is finished to obtain sol; immersing a graphite plate into the bottom of the sol, aging for 10-12 h, drying at 60-80 ℃ for 20-22 h to obtain a graphite plate with the surface covered with colloid, introducing 500-600A direct current for 15-25 min to obtain sintered colloid attached to the graphite plate, scraping, grinding to obtain palladium-doped nano TiO2And (3) pulverizing. The method has the advantages of simple synthesis process, mild reaction conditions, greatly shortened sample sintering time, better sintered sample shape, more stable structure, greatly reduced production cost, good repeatability and capability of preparing the palladium-doped TiO2The degradation rate of the photocatalyst to methylene blue is obviously improved.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to palladium-doped nano TiO2A method for preparing powder.
Background
TiO2The photocatalyst has the advantages of stable chemical performance, controllable preparation cost, no toxicity, utilization of sunlight, no secondary pollution and the like, and has wide application prospect in the treatment of polluted wastewater. But pure TiO2When the photocatalyst is used as a photocatalyst, the band gap is wide, only photons with the length less than 387nm can be absorbed, and the photogenerated electron-hole recombination rate is high, so that the quantum yield is low, the photocatalytic efficiency is low, and the practical application range of the photocatalyst is greatly limited, so that the methods of metal ion doping, anion doping, different semiconductor compounding, noble metal modification and the like are frequently adopted to improve TiO2Photocatalytic activity of (1). Tong (Chinese character of 'tong')Over-doping can effectively inhibit photogenerated electron-hole recombination in TiO2Defect sites are introduced into the crystal lattices, the spectral response range of the crystal lattices is changed and expanded, and the photocatalytic efficiency is improved. Currently, palladium doped TiO is prepared2The resistance furnace sintering method is adopted, and the method needs gradient temperature rise, has long sintering time and poor sample form.
Disclosure of Invention
Aiming at the existing sintering method for preparing palladium-doped nano TiO2The invention provides palladium-doped nano TiO2The preparation method of the powder is characterized in that colloid is deposited on the surface of graphite, and then electric heating sintering is carried out, so that the palladium-doped nano TiO with excellent performance can be prepared while the preparation process is simplified2And (3) pulverizing.
The invention relates to palladium-doped nano TiO2The preparation method of the powder comprises the following steps:
step 1, adding palladium acetylacetonate into absolute ethyl alcohol, and uniformly stirring to obtain a colorless and transparent mixed solution; wherein, according to the solid-to-liquid ratio, the ratio of palladium acetylacetonate: absolute ethyl alcohol (0.2 to 0.3) g: (30-40) mL;
step 2, dropwise adding 70-80 mL of isopropyl titanate (IOPT) into the mixed solution under the stirring condition, and continuously stirring for 0.5-1 h after dropwise adding is finished to obtain colorless and semitransparent sol;
step 3, immersing the graphite plate into the bottom of the sol, aging for 10-12 h, and drying at 60-80 ℃ for 20-22 h to obtain the graphite plate with the surface covered with the colloid;
step 4, introducing direct current into the graphite plate with the surface covered with the colloid, controlling the current to be 500-600A, electrifying for 15-25 min, sintering the colloid covered on the surface of the graphite plate by utilizing the heating of the graphite plate, and obtaining sintered colloid attached to the graphite plate;
step 5, scraping the sintered colloid from the graphite plate to obtain a scraped material, and grinding the scraped material to obtain the palladium-doped nano TiO2And (3) pulverizing.
The palladium-doped nano TiO2In the preparation method of the powder, the prepared palladium-doped nano TiO2The average particle size of the powder is 100 to150nm, and the photocatalytic degradation rate is 80-95%.
The palladium-doped nano TiO2In the preparation method of the powder, the graphite plate is a plate made of graphite with the purity of more than or equal to 99.9 wt.%, and the thickness is preferably 1.5 cm. The graphite plate is polished before use to obtain a smooth graphite plate.
In the step 1, the stirring is carried out at a stirring speed of 600-1000 rpm for at least 10 min.
In the step 2, the stirring is carried out at a stirring speed of 5-15 rpm.
In the step 2, the dripping time is 10-15 min, and the dripping speed is 4.5-8 mL/min.
In the step 3, the thickness of the colloid covered on the graphite plate is 2-3 mm in the graphite plate with the surface covered with the colloid.
In the step 3, the aging process is a process of depositing the sol on the surface of the graphite plate.
In the step 5, the grinding is carried out for 10-20 min, and the grinding is used for doping agglomerated palladium with nano TiO2Grinding the powder into powder.
The invention relates to palladium-doped nano TiO2Compared with the prior art, the preparation method of the powder has the beneficial effects that:
the method has the advantages of simple synthesis process, mild reaction conditions, greatly shortened sample sintering time, better sintered sample shape, more stable structure, greatly reduced production cost, good repeatability and capability of preparing the palladium-doped TiO2The degradation rate of the photocatalyst to methylene blue is obviously improved; in TiO2The palladium ions doped in the composite material can inhibit the recombination of photo-generated electrons and holes, and the metal ions can effectively capture the photo-generated electrons, so that the separation efficiency of photo-generated electron-hole pairs is improved, the absorption performance in a visible light region is obviously improved, and TiO (TiO) is enhanced2Photocatalytic activity of (1).
Drawings
FIG. 1 shows Pd-doped nano TiO material prepared in example 1 of the present invention2SEM image of powder.
FIG. 2 shows Pd-doped nano TiO compound prepared in example 1 of the present invention2XRD pattern of powder.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the following examples, the SEM observation was performed using a JSM-7500F cold field emission scanning electron microscope.
In the following examples, palladium acetylacetonate, absolute ethanol and isopropyl titanate were used as commercially available analytical reagents.
In the following examples, the graphite plate is made of graphite with a purity of not less than 99.9%.
In the following examples, graphite plates were polished flat prior to use.
In the following examples, the thickness of the colloid on the surface of the dried graphite plate is 2 to 3 mm.
In the following examples, the total dropping time was controlled to 10 to 15min when the dropping was carried out.
In the following examples, the scraped materials were ground in a mortar for 10 to 20min to form a powder of the whole materials.
In the following embodiments, the voltage is 5-10V when the DC is applied.
In the following examples, the photocatalytic degradation test method was performed using GB/T23762-2009 "photocatalytic material aqueous solution system purification performance test method".
The present invention will be further described with reference to the following examples, which are intended to illustrate the technical common general knowledge that the present invention can be described by other means without departing from the technical features of the present invention, and therefore all changes within the scope of the present invention or the equivalent scope of the present invention are intended to be embraced by the present invention.
Example 1
Palladium-doped nano TiO2The preparation method of the powder comprises the following steps:
step 1, adding 0.2g of palladium acetylacetonate into 30mL of absolute ethyl alcohol, and stirring for 25min under the stirring condition of the rotating speed of 600rpm to obtain a colorless and transparent mixed solution;
step 2, dropwise adding 70mL of isopropyl titanate into the mixed solution under the stirring condition, and continuously stirring for 0.5h after dropwise adding is finished to obtain colorless and semitransparent sol; wherein the dripping time of the isopropyl titanate is controlled to be 10 min; the stirring speed is 5 rpm;
step 3, immersing the graphite plate at the bottom of the sol, aging for 10h, and drying at 60 ℃ for 22h to obtain the graphite plate with the surface covered with the colloid; wherein the thickness of the colloid covered on the surface of the graphite plate is 2 mm;
step 4, introducing direct current to the graphite plate with the surface covered with the colloid, controlling the current to be 500A, conducting for 25min, sintering the colloid covered on the surface of the graphite plate by utilizing the heating of the graphite plate, and obtaining sintered colloid attached to the graphite plate;
step 5, scraping the sintered colloid from the graphite plate to obtain a scraped material, and grinding the scraped material into powder, namely the palladium-doped nano TiO2And (3) pulverizing.
For the palladium-doped nano TiO prepared in this example2Observing the powder by using an electron microscope, wherein an SEM image is shown in figure 1; as can be seen from FIG. 1, the prepared doped nano TiO2The powder has uniform appearance.
For the palladium-doped nano TiO prepared in this example2XRD analysis of the powder was carried out, and its XRD pattern is shown in FIG. 2. from FIG. 2, it can be seen that the palladium-doped nano TiO prepared in this example2The powder is anatase type TiO2(characteristic peak at 25.3 degree), the anatase type TiO2Belongs to a tetragonal system, has relatively stable structure and excellent photocatalysis.
The palladium-doped nano TiO prepared in the embodiment is subjected to the method of GB/T23762-2009 standard2The powder was subjected to photocatalytic degradation testing. Through a real photocatalytic degradation test, the product doped with palladium has a better photocatalytic effect than pure titanium dioxide, the photocatalytic degradation rate is about 25% when the product is not doped, and the photocatalytic degradation rate reaches 95% after the product is doped with palladium, so that the absorption performance in a visible light region is improved, and the TiO is enhanced2Photocatalytic activity of (1).
Example 2
Palladium dopingNano TiO 22The powder preparation method is the same as example 1, except that:
(1) adding 0.3g of palladium acetylacetonate into 40mL of absolute ethyl alcohol, and stirring for 10min under the stirring condition of the rotating speed of 700 rpm;
(2) dropwise adding 75mL of isopropyl titanate into the mixed solution, wherein the total dropwise adding time of the isopropyl titanate is 12 min; the stirring speed is 15 rpm;
(3) aging for 11h, and drying at 70 deg.C for 21h to obtain graphite plate surface colloid with thickness of 2.4 mm;
(4) the electrifying current is 550A, and the electrifying time is 20 min;
(5) through a real photocatalytic degradation test, the photocatalytic degradation rate reaches 80%.
Example 3
Palladium-doped nano TiO2The powder preparation method is the same as example 1, except that:
(1) adding 0.2g of palladium acetylacetonate into 35mL of absolute ethyl alcohol, and stirring for 15min under the stirring condition of the rotating speed of 800 rpm;
(2) dropwise adding 78mL of isopropyl titanate into the mixed solution, wherein the total dropwise adding time of the isopropyl titanate is 14 min;
(3) aging for 12h, and drying at 75 deg.C for 20h to obtain graphite plate surface colloid with thickness of 2.8 mm;
(4) the electrifying current is 560A, and the electrifying time is 18 min;
(5) through a real photocatalytic degradation test, the photocatalytic degradation rate reaches 85%.
Example 4
Palladium-doped nano TiO2The powder preparation method is the same as example 1, except that:
(1) adding 0.2g of palladium acetylacetonate into 30mL of absolute ethyl alcohol, and stirring for 20min under the stirring condition of the rotating speed of 1000 rpm;
(2) dropwise adding 80mL of isopropyl titanate into the mixed solution, wherein the total dropwise adding time of the isopropyl titanate is 15min, and stirring for 1h after the dropwise adding is finished;
(3) aging for 12h, and drying at 80 deg.C for 20h to obtain graphite plate surface colloid with thickness of 3 mm;
(4) the electrifying current is 600A, and the electrifying time is 15 min;
(5) through a real photocatalytic degradation test, the photocatalytic degradation rate reaches 90%.
Claims (8)
1. Palladium-doped nano TiO2The preparation method of the powder is characterized by comprising the following steps:
step 1, adding palladium acetylacetonate into absolute ethyl alcohol, and uniformly stirring to obtain a colorless and transparent mixed solution; wherein, according to the solid-to-liquid ratio, the ratio of palladium acetylacetonate: absolute ethyl alcohol (0.2 to 0.3) g: (30-40) mL;
step 2, dropwise adding 70-80 mL of isopropyl titanate into the mixed solution under the stirring condition, and after dropwise adding, continuously stirring for 0.5-1 h to obtain colorless and semitransparent sol;
step 3, immersing the graphite plate into the bottom of the sol, aging for 10-12 h, and drying at 60-80 ℃ for 20-22 h to obtain the graphite plate with the surface covered with the colloid;
step 4, introducing direct current into the graphite plate with the surface covered with the colloid, controlling the current to be 500-600A, electrifying for 15-25 min, sintering the colloid covered on the surface of the graphite plate by utilizing the heating of the graphite plate, and obtaining sintered colloid attached to the graphite plate;
step 5, scraping the sintered colloid from the graphite plate to obtain a scraped material, and grinding the scraped material to obtain the palladium-doped nano TiO2And (3) pulverizing.
2. The palladium-doped nano TiO of claim 12The preparation method of the powder is characterized in that the palladium-doped TiO2In the preparation method of the powder, the prepared palladium-doped nano TiO2The average particle size of the powder is 100-150 nm.
3. The palladium-doped nano TiO of claim 12The preparation method of the powder is characterized in that the palladium-doped TiO2In the preparation method of the powder, the graphite plate is a plate made of graphite with the purity of more than or equal to 99.9 wt.%; the graphite plate is polished before use to obtain a smooth graphite plateA graphite plate.
4. The palladium-doped nano TiO of claim 12The preparation method of the powder is characterized in that in the step 1, the stirring is carried out at a stirring speed of 600-1000 rpm for at least 10 min.
5. The palladium-doped nano TiO of claim 12The preparation method of the powder is characterized in that in the step 2, the stirring is carried out at the stirring speed of 5-15 rpm.
6. The palladium-doped nano TiO of claim 12The preparation method of the powder is characterized in that in the step 2, the dripping time is 10-15 min, and the dripping speed is 4.5-8 mL/min.
7. The palladium-doped nano TiO of claim 12The preparation method of the powder is characterized in that in the step 3, the thickness of the colloid covered on the graphite plate is 2-3 mm in the graphite plate with the surface covered with the colloid.
8. The palladium-doped nano TiO of claim 12The preparation method of the powder is characterized in that in the step 5, the grinding is carried out for 10-20 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810095034.1A CN108295844B (en) | 2018-01-31 | 2018-01-31 | Palladium-doped nano TiO2Method for preparing powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810095034.1A CN108295844B (en) | 2018-01-31 | 2018-01-31 | Palladium-doped nano TiO2Method for preparing powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108295844A CN108295844A (en) | 2018-07-20 |
| CN108295844B true CN108295844B (en) | 2020-03-31 |
Family
ID=62867285
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810095034.1A Active CN108295844B (en) | 2018-01-31 | 2018-01-31 | Palladium-doped nano TiO2Method for preparing powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108295844B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1734260A (en) * | 2004-08-03 | 2006-02-15 | 上海奉泰电子电器元件有限公司 | Method for preparing carrier catalytic element for gas detection in coal mine |
| CN101059467A (en) * | 2007-06-07 | 2007-10-24 | 上海交通大学 | Catalytic combustion type sensor sensitive body self-assembled molding method |
| CN101785479A (en) * | 2010-03-03 | 2010-07-28 | 曲阜师范大学 | Palladium-doped nano titanium dioxide anti-bacterial agent and preparation method and application thereof |
| CN103100386A (en) * | 2013-01-15 | 2013-05-15 | 汕头大学 | Preparation method of monolithic catalyst for degrading VOCS (Volatile Organic Compounds) |
| CN104138756A (en) * | 2014-08-02 | 2014-11-12 | 孙超 | Supported catalyzer for low-temperature catalytic combustion of VOCs and method for preparing supported catalyzer for low-temperature catalytic combustion of VOCs |
-
2018
- 2018-01-31 CN CN201810095034.1A patent/CN108295844B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1734260A (en) * | 2004-08-03 | 2006-02-15 | 上海奉泰电子电器元件有限公司 | Method for preparing carrier catalytic element for gas detection in coal mine |
| CN101059467A (en) * | 2007-06-07 | 2007-10-24 | 上海交通大学 | Catalytic combustion type sensor sensitive body self-assembled molding method |
| CN101785479A (en) * | 2010-03-03 | 2010-07-28 | 曲阜师范大学 | Palladium-doped nano titanium dioxide anti-bacterial agent and preparation method and application thereof |
| CN103100386A (en) * | 2013-01-15 | 2013-05-15 | 汕头大学 | Preparation method of monolithic catalyst for degrading VOCS (Volatile Organic Compounds) |
| CN104138756A (en) * | 2014-08-02 | 2014-11-12 | 孙超 | Supported catalyzer for low-temperature catalytic combustion of VOCs and method for preparing supported catalyzer for low-temperature catalytic combustion of VOCs |
Non-Patent Citations (1)
| Title |
|---|
| Time effects on the stability of the induced defects in TiO2 nanoparticles doped by different nitrogen sources;F. Spadavecchia et al.;《J Nanopart Res》;20121231;第14卷;全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108295844A (en) | 2018-07-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109569684B (en) | Plasma modified metal oxide and g-carbon nitride co-modified titanium dioxide nanorod composite photocatalyst as well as preparation method and application thereof | |
| CN105126886B (en) | A kind of TiO2/WO3/g-C3N4The preparation method of full meso-porous nano fiber | |
| CN110152711A (en) | A kind of CeO2@MoS2/g-C3N4Three-element composite photocatalyst and preparation method thereof | |
| CN112310377B (en) | Battery negative electrode material and preparation method thereof | |
| CN106732358B (en) | A kind of biomass carbonization microballoon loading iron oxide and its preparation and application | |
| CN109126758B (en) | Preparation method and application of blue titanium dioxide | |
| CN108067281A (en) | Porous g-C3N4Photochemical catalyst and its preparation method and application | |
| CN103101972A (en) | Preparation method of three-dimensional mesoporous titanium dioxide photocatalyst by means of biological template method | |
| CN114618537A (en) | Red phosphorus/strontium titanate heterojunction photocatalyst and preparation method and application thereof | |
| CN105002599A (en) | Preparation method of high-purity N-doped TiO2 mesoporous nanofiber | |
| CN108579775B (en) | Silver phosphate/silver/titanium dioxide nanoflower composite material and preparation method and application thereof | |
| CN108295844B (en) | Palladium-doped nano TiO2Method for preparing powder | |
| CN108246335B (en) | Nitrogen-silver doped nano TiO2Method for preparing powder | |
| CN113385213B (en) | Preparation method of adsorption type piezoelectric photocatalysis composite fiber material | |
| CN105126892B (en) | A kind of TiO2/WO3/g-C3N4Full application of the meso-porous nano fiber in high efficiency photocatalyst | |
| CN105148965B (en) | A kind of TiO2/WO3/g-C3N4Full meso-porous nano fiber | |
| CN107497458B (en) | Bismuth fluorotellurate photocatalytic material, preparation method and application thereof | |
| CN107497427B (en) | Preparation method of silver/graphene/zinc oxide composite material capable of degrading formaldehyde | |
| WO2021103478A1 (en) | Preparation method for bismuth acid copper film | |
| CN102586741A (en) | Preparation method of doped zinc oxide film | |
| CN109778352B (en) | Ti prepared by electrostatic spinning in-situ reduction4O7Nanofibers and methods thereof | |
| CN110935441A (en) | Titanium-based composite catalytic net for efficiently degrading formaldehyde and preparation method thereof | |
| CN107670681B (en) | Nitrogen-doped TiO2Method for preparing powder | |
| CN104998676A (en) | High-purity N-doped TiO2 full-mesoporous nanofiber | |
| CN109985652B (en) | Photocatalyst and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |