CN108295844A - A kind of palladium dopen Nano TiO2The preparation method of powder - Google Patents
A kind of palladium dopen Nano TiO2The preparation method of powder Download PDFInfo
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- CN108295844A CN108295844A CN201810095034.1A CN201810095034A CN108295844A CN 108295844 A CN108295844 A CN 108295844A CN 201810095034 A CN201810095034 A CN 201810095034A CN 108295844 A CN108295844 A CN 108295844A
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- dopen nano
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 46
- 239000000843 powder Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 45
- 239000010439 graphite Substances 0.000 claims abstract description 45
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000084 colloidal system Substances 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 9
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 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 6
- 238000013019 agitation Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 22
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 206010037660 Pyrexia Diseases 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 235000013339 cereals Nutrition 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 238000005245 sintering Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 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
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000007790 scraping Methods 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 10
- 230000000694 effects Effects 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 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 description 5
- 235000019441 ethanol Nutrition 0.000 description 4
- 125000005909 ethyl alcohol group Chemical group 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 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
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—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
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- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
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- 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
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- 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
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- 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
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Abstract
A kind of palladium dopen Nano TiO2The preparation method of powder, belongs to field of material technology.This method includes：Palladium acetylacetonate is added in absolute ethyl alcohol, stirs evenly, obtains mixed liquor；Under agitation by 70~80ml isopropyl titanates, it is added drop-wise in mixed liquor, after being added dropwise, continues 0.5~1h of stirring, obtain colloidal sol；Graphite cake is submerged into colloidal sol bottom, after being aged 10~12h, is placed in 60~80 DEG C of dry 20~22h, obtain the graphite cake that colloid is covered with to surface, 500~600A, 15~25min of direct current are passed through, the sintered colloid adhered on graphite cake, scraping, grinding are obtained, obtain palladium dopen Nano TiO2Powder.This method synthesis technology is simple, and reaction condition is mild, and sample sintering time greatly shortens, and sample morphology is more preferable after sintering, and structure is more stable, while greatly lowering production cost, favorable repeatability, and the palladium of preparation adulterates TiO2Photochemical catalyst significantly improves the degradation rate of methylene blue.
Description
Technical field
The invention belongs to field of material technology, more particularly to a kind of palladium dopen Nano TiO2The preparation method of powder.
Background technology
TiO2Photochemical catalyst, because it is controllable, nontoxic with stable chemical performance, manufacturing cost, and using sunlight,
The advantages that non-secondary pollution, has a extensive future in terms of the processing of pollutant effluents.But pure TiO2When being used as photochemical catalyst, because
Greater band gap can only absorb the long photon less than 387nm, and light induced electron-hole-recombination rate is high, cause quantum yield it is low,
Photocatalysis efficiency is low, strongly limits its practical ranges, therefore must be frequently with metal ion mixing, anion doped, different
The methods of semiconductors coupling, noble metal decorated improve TiO2Photocatalytic activity.By doping, it can effectively inhibit photoproduction electric
Son-hole-recombination, in TiO2Defective bit is introduced in lattice, changes and extend its spectral response range, improves photocatalysis efficiency.
Currently, preparing palladium doping TiO2Using resistance furnace sintering process, this method needs gradient increased temperature, and sintering time is long, sample morphology compared with
Difference.
Invention content
Palladium dopen Nano TiO is prepared for existing sintering process2, a kind of palladium of present invention offer, which adulterates, to be received
Rice TiO2The preparation method of powder, this method prepare work by graphite surface depositing colloidal, then carrying out electric heating sintering, simplifying
While skill, the palladium dopen Nano TiO of function admirable can be prepared by2Powder.
A kind of palladium dopen Nano TiO of the present invention2The preparation method of powder, includes the following steps：
Step 1, palladium acetylacetonate is added in absolute ethyl alcohol, stirs evenly, obtains the mixed liquor of water white transparency；Wherein,
By solid-to-liquid ratio, palladium acetylacetonate：Absolute ethyl alcohol=(0.2~0.3) g：(30~40) mL；
Step 2, under agitation by 70~80mL isopropyl titanates (IOPT), it is added drop-wise in mixed liquor, is added dropwise
Afterwards, continue 0.5~1h of stirring, obtain the colloidal sol of semi-transparent clear；
Step 3, graphite cake is submerged into colloidal sol bottom, after being aged 10~12h, is placed in 60~80 DEG C of dry 20~22h, obtains
The graphite cake of colloid is covered with to surface；
Step 4, it is covered with to surface in the graphite cake of colloid and is passed through direct current, control electrical current is 500~600A, is led to
The colloid for being covered in graphite plate surface is sintered using graphite cake fever, obtains adhering on graphite cake by electric 15~25min of time
Sintered colloid；
Step 5, sintered colloid is wiped off from graphite cake, the material being scraped is ground, and as palladium is mixed
Miscellaneous nano-TiO2Powder.
The palladium dopen Nano TiO2In the preparation method of powder, the palladium dopen Nano TiO of preparation2The average grain diameter of powder is
100~150nm, photocatalytic activity are 80~95%.
The palladium dopen Nano TiO2In the preparation method of powder, the graphite cake is the stone of purity >=99.9wt.%
Plank made of ink, thickness are preferably 1.5cm.The graphite cake, by polishing, obtains smooth graphite cake using preceding.
In the step 1, the stirring, speed of agitator is 600~1000rpm, and mixing time is at least 10min.
In the step 2, the stirring, speed of agitator is 5~15rpm.
In the step 2, the dropwise addition, time for adding is 10~15min, and drop rate is 4.5~8mL/min.
In the step 3, the surface is covered in the graphite cake of colloid, the thickness of the colloid covered on graphite cake
For 2~3mm.
In the step 3, the ageing process is process of the sol deposition in graphite plate surface.
In the step 5, the grinding, milling time is 10~20min, and it acts as receive the palladium doping of caking
Rice TiO2Powder grind into powder.
A kind of palladium dopen Nano TiO of the present invention2The preparation method of powder, compared with the prior art, advantage is：
The method synthesis technology of the present invention is simple, and reaction condition is mild, and sample sintering time greatly shortens, sample after sintering
Form is more preferable, and structure is more stable, while greatly lowering production cost, favorable repeatability, and the palladium of preparation adulterates TiO2Photochemical catalyst
The degradation rate of methylene blue is significantly improved；In TiO2Middle doping palladium ion can inhibit the compound of light induced electron and hole, this
It is, to improve the separative efficiency of photo-generate electron-hole pair, significantly to be carried since metal ion can effectively capture light induced electron
Height enhances TiO in the absorbent properties of visible region2Photocatalytic activity.
Description of the drawings
Fig. 1 is palladium dopen Nano TiO made from the embodiment of the present invention 12The SEM of powder schemes.
Fig. 2 is palladium dopen Nano TiO made from the embodiment of the present invention 12The XRD diagram of powder.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail.
In following embodiment, the equipment that SEM observations use is JSM-7500F cold field emission scanning electron microscope.
In following embodiment, palladium acetylacetonate, absolute ethyl alcohol and the isopropyl titanate used is market analytical pure reagents.
In following embodiment, graphite cake material is the graphite of purity >=99.9%.
In following embodiment, graphite cake is polished flat using preceding process.
In following embodiment, the thickness of the graphite cake surface colloid after drying is 2~3mm.
In following embodiment, when being added dropwise, it is 10~15min to control whole time for adding.
In following embodiment, by the material being scraped 10~20min of mortar grinder, whole materials is made to form powder.
In following embodiment, voltage is 5~10V when being passed through direct current.
In following embodiment, carries out photocatalytic degradation test method and use GB/T23762-2009《Catalysis material is water-soluble
Liquid system purifying property test method》.
Below in conjunction with the content that example further illustrates the present invention, as known by the technical knowledge, the present invention also can be by other
The scheme that does not depart from the technology of the present invention feature describe, therefore it is all within the scope of the present invention or in the equivalent scope of the invention
Change is included in the invention.
Embodiment 1
A kind of palladium dopen Nano TiO2The preparation method of powder, includes the following steps：
Step 1,0.2g palladium acetylacetonates are added in 30mL absolute ethyl alcohols, are then 600rpm stirring conditions in rotating speed
Lower stirring 25min, obtains the mixed liquor of water white transparency；
Step 2, under agitation by 70mL isopropyl titanates, it is added drop-wise in mixed liquor, after being added dropwise, continues to stir
0.5h obtains the colloidal sol of semi-transparent clear；Wherein, control isopropyl titanate time for adding is 10min；The stirring, stirring
Rotating speed is 5rpm；
Step 3, graphite cake is immersed in colloidal sol bottom, after being aged 10h, is placed in 60 DEG C of dry 22h, obtains to surface and be covered with
The graphite cake of colloid；Wherein, the thickness of the colloid of graphite plate surface covering is 2mm；
Step 4, the graphite cake that colloid is covered with to surface is passed through direct current, and control electrical current is 500A, conduction time
The colloid for being covered in graphite plate surface is sintered using graphite cake fever, obtains adhering on graphite cake sintered by 25min
Colloid；
Step 5, sintered colloid to be wiped off from graphite cake, the material being scraped is ground to powdered,
As palladium dopen Nano TiO2Powder.
To palladium dopen Nano TiO manufactured in the present embodiment2Powder uses electron microscope observation, SEM figures as shown in Figure 1；
It will be seen from figure 1 that the dopen Nano TiO prepared2Powder pattern is uniform.
To palladium dopen Nano TiO manufactured in the present embodiment2Powder carries out XRD analysis, and XRD diagram is shown in Fig. 2, can be with from Fig. 2
Find out, palladium dopen Nano TiO manufactured in the present embodiment2Powder is Detitanium-ore-type TiO2(characteristic peak is at 25.3 °), the Detitanium-ore-type
TiO2Belong to tetragonal crystal system, structure is stablized relatively, with excellent photocatalytic.
Using the method for GB/T23762-2009 standards, to palladium dopen Nano TiO manufactured in the present embodiment2Powder carries out light and urges
Change degradation test to test.It is tested by the test of real photocatalytic degradation, adulterates the product photocatalysis effect after palladium and obviously compare pure titinium dioxide
Effect is good, and when undoped, photocatalytic activity is 25% or so, and after adulterating palladium element, photocatalytic activity is improved up to 95%
In the absorbent properties of visible region, TiO is enhanced2Photocatalytic activity.
Embodiment 2
A kind of palladium dopen Nano TiO2The preparation method of powder, with embodiment 1, difference is：
(1) 0.3g palladium acetylacetonates are added in 40mL absolute ethyl alcohols, then in the case where rotating speed is 700rpm stirring conditions
Stir 10min；
(2) 75mL isopropyl titanates are added drop-wise in mixed liquor, isopropyl titanate whole time for adding is 12min；Stirring
Rotating speed is 15rpm；
(3) it is aged 11h, then in 70 DEG C of dry 21h, the thickness of graphite cake surface colloid is 2.4mm；
(4) electrical current is 550A, conduction time 20min；
(5) it is tested by the test of real photocatalytic degradation, photocatalytic activity is up to 80%.
Embodiment 3
A kind of palladium dopen Nano TiO2The preparation method of powder, with embodiment 1, difference is：
(1) 0.2g palladium acetylacetonates are added in 35mL absolute ethyl alcohols, then in the case where rotating speed is 800rpm stirring conditions
Stir 15min；
(2) 78mL isopropyl titanates are added drop-wise in mixed liquor, isopropyl titanate whole time for adding is 14min；
(3) it is aged 12h, then in 75 DEG C of dry 20h, the thickness of graphite cake surface colloid is 2.8mm；
(4) electrical current is 560A, conduction time 18min；
(5) it is tested by the test of real photocatalytic degradation, photocatalytic activity is up to 85%.
Embodiment 4
A kind of palladium dopen Nano TiO2The preparation method of powder, with embodiment 1, difference is：
(1) 0.2g palladium acetylacetonates are added in 30mL absolute ethyl alcohols, then in the case where rotating speed is 1000rpm stirring conditions
Stir 20min；
(2) 80mL isopropyl titanates are added drop-wise in mixed liquor, isopropyl titanate whole time for adding is 15min, is added dropwise
After, stir 1h；
(3) it is aged 12h, then in 80 DEG C of dry 20h, the thickness of graphite cake surface colloid is 3mm；
(4) electrical current is 600A, conduction time 15min；
(5) it is tested by the test of real photocatalytic degradation, photocatalytic activity is up to 90%.
Claims (8)
1. a kind of palladium dopen Nano TiO2The preparation method of powder, which is characterized in that include the following steps：
Step 1, palladium acetylacetonate is added in absolute ethyl alcohol, stirs evenly, obtains the mixed liquor of water white transparency；Wherein, it presses solid
Liquor ratio, palladium acetylacetonate：Absolute ethyl alcohol=(0.2~0.3) g：(30~40) mL；
Step 2, under agitation by 70~80mL isopropyl titanates, it is added drop-wise in mixed liquor, after being added dropwise, continues to stir
0.5~1h obtains the colloidal sol of semi-transparent clear；
Step 3, graphite cake is submerged into colloidal sol bottom, after being aged 10~12h, is placed in 60~80 DEG C of dry 20~22h, obtains table
Face is covered with the graphite cake of colloid；
Step 4, it is covered with to surface in the graphite cake of colloid and is passed through direct current, control electrical current is 500~600A, when energization
Between 15~25min, using graphite cake fever will be covered in graphite plate surface colloid be sintered, obtain the burning adhered on graphite cake
Colloid after knot；
Step 5, sintered colloid is wiped off from graphite cake, the material being scraped is ground, and as palladium doping is received
Rice TiO2Powder.
2. palladium dopen Nano TiO as described in claim 12The preparation method of powder, which is characterized in that the palladium adulterates TiO2
In the preparation method of powder, the palladium dopen Nano TiO of preparation2The average grain diameter of powder is 100~150nm.
3. palladium dopen Nano TiO as described in claim 12The preparation method of powder, which is characterized in that the palladium adulterates TiO2
In the preparation method of powder, the graphite cake is plank made of the graphite of purity >=99.9wt.%；The graphite cake uses
It is preceding to pass through polishing, obtain smooth graphite cake.
4. palladium dopen Nano TiO as described in claim 12The preparation method of powder, which is characterized in that in the step 1, institute
The stirring stated, speed of agitator are 600~1000rpm, and mixing time is at least 10min.
5. palladium dopen Nano TiO as described in claim 12The preparation method of powder, which is characterized in that in the step 2, institute
The stirring stated, speed of agitator are 5~15rpm.
6. palladium dopen Nano TiO as described in claim 12The preparation method of powder, which is characterized in that in the step 2, institute
The dropwise addition stated, time for adding are 10~15min, and drop rate is 4.5~8mL/min.
7. palladium dopen Nano TiO as described in claim 12The preparation method of powder, which is characterized in that in the step 3, institute
The surface stated is covered in the graphite cake of colloid, and the thickness of the colloid covered on graphite cake is 2~3mm.
8. palladium dopen Nano TiO as described in claim 12The preparation method of powder, which is characterized in that in the step 5, institute
The grinding stated, milling time are 10~20min.
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