CN105664940B - A kind of preparation method of magnetic oxygenated palladium pucherite compounded visible light photocatalyst - Google Patents
A kind of preparation method of magnetic oxygenated palladium pucherite compounded visible light photocatalyst Download PDFInfo
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- CN105664940B CN105664940B CN201610009752.3A CN201610009752A CN105664940B CN 105664940 B CN105664940 B CN 105664940B CN 201610009752 A CN201610009752 A CN 201610009752A CN 105664940 B CN105664940 B CN 105664940B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 27
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 22
- 239000012153 distilled water Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims abstract description 10
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 6
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000002045 lasting effect Effects 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 45
- 238000005406 washing Methods 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 13
- 229910000474 mercury oxide Inorganic materials 0.000 claims description 11
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 claims description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 7
- 239000000428 dust Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 4
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 238000000643 oven drying Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims description 2
- 238000013517 stratification Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000000227 grinding Methods 0.000 abstract description 7
- 238000004064 recycling Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 206010013786 Dry skin Diseases 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 7
- 229910002915 BiVO4 Inorganic materials 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 5
- 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 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001802 infusion Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- DPSWNBLFKLUQTP-UHFFFAOYSA-N bismuth vanadium Chemical compound [V].[Bi] DPSWNBLFKLUQTP-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010959 steel 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
-
- 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
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/648—Vanadium, niobium or tantalum or polonium
- B01J23/6482—Vanadium
-
- 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
- B01J35/33—Electric or magnetic 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
- B01J35/39—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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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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 discloses a kind of preparation method of magnetic oxygenated palladium pucherite compounded visible light photocatalyst, comprise the following steps：Pucherite is made using bismuth nitrate and ammonium vanadate as raw material in a；Magnetic iron oxide is made using iron oxide and sodium hydroxide as raw material in b；Palladium bichloride is dissolved in distilled water by c, lasting stirring, adds concentrated hydrochloric acid, is completely dissolved to obtain palladium chloride solution；D sequentially adds pucherite, palladium chloride solution and magnetic iron oxide in crucible, being stirred continuously with glass bar makes it well mixed, it is placed in drying box, in 100 110 DEG C of dryings, take out, be placed in Muffle furnace, 0.5h is calcined in 400 DEG C, calcined product grinding is taken out, obtains magnetic oxygenated palladium pucherite compounded visible light photocatalyst.Catalyst produced by the present invention has magnetic action, it is facilitated follow-up recycling while catalyst activity is kept.
Description
Technical field
The present invention relates to a kind of preparation method of visible-light photocatalyst, concretely relate to a kind of magnetic oxygenated palladium-
The preparation method of pucherite compounded visible light photocatalyst.
Background technology
At present, known active oxidation palladium-composite bismuth vanadium photocatalyst is with bismuth nitrate, ammonium vanadate, palladium bichloride and ammonia
Water is prepared for raw material.The catalyst has certain catalytic action, it can be difficult to recycling, causes the wasting of resources.In order to
Facilitate the recovery of catalyst, it is conventional resolving ideas that catalyst is combined with the magnetic material of tool.But for inhomogeneity
The catalyst of type, used specific solution but differ greatly.At present, there has been no palladium oxide-pucherite complex light is urged
Agent is assigned to magnetic, to solve the relevant report of the catalyst effective recycling.
The content of the invention
It is an object of the invention to provide a kind of preparation side of magnetic oxygenated palladium-pucherite compounded visible light photocatalyst
Method, the catalyst obtained by this method introduces magnetisable material, not only with preferable catalytic effect, and conveniently recycles,
It is cost-effective.
The adopted technical solution is that：
A kind of preparation method of magnetic oxygenated palladium-pucherite compounded visible light photocatalyst, comprises the following steps：
Bismuth nitrate is dissolved in dust technology by a, is heated to 50-70 DEG C, obtains solution one；Ammonium vanadate is dissolved in deionized water
In, 50-70 DEG C is heated to, obtains solution two；Solution one and solution two are mixed while stirring, obtain mixed solution, to mixing
Ammoniacal liquor is added in solution, pH to 6.5-7.5 is adjusted, stratification, pours out supernatant liquor and obtain yellow mercury oxide, with distillation water washing
Yellow mercury oxide；Yellow mercury oxide after washing is diluted with distilled water into suspension, is placed in the closed stainless of polytetrafluoroethyllining lining
It is heat-treated in steel reactor, temperature is 180-200 DEG C, time 6h；After being disposed, heat-treated products are cooled down dry
It is dry, obtain pucherite；
Iron oxide is dissolved in distilled water by b, then adds polyethylene glycol, obtains solution three；Sodium hydroxide is dissolved in distillation
In water, polyethylene glycol is then added, obtains solution four；Solution four is poured into rapidly in solution three, stirs 30-45min, subsequent mistake
Filter, oven drying is placed in after much filtrate is washed, oven temperature is 70-100 DEG C, drying time 5-7h, will after the completion of drying
Much filtrate is placed in Muffle furnace and calcined, and calcining heat is 300 DEG C, calcination time 1h, by calcined product after the completion of calcining
Take out, be down to room temperature, be ground, obtain magnetic iron oxide；
Palladium bichloride is dissolved in distilled water by c, lasting stirring, is heated to 50-70 DEG C, then adds concentrated hydrochloric acid, be completely dissolved
Obtain palladium chloride solution；
Pucherite made from step a is placed in crucible by d, and palladium chloride solution made from step c is then added into crucible,
Magnetic iron oxide made from step b is added, being stirred continuously with glass bar makes it well mixed, is subsequently placed in drying box and does
Dry, drying box temperature is 100-110 DEG C, takes out dried object after the completion of drying, is subsequently placed in Muffle furnace and is calcined, and is calcined
Temperature is 400 DEG C, calcination time 0.5h, takes out calcined product after the completion of calcining and grinds, obtains magnetic oxygenated palladium-pucherite
Compounded visible light photocatalyst.
In step a：The mass ratio of bismuth nitrate and ammonium vanadate is preferably 4-6: 1-1.5.
In step a：The concentration of the dust technology is preferably 0.6mol/L；The concentration of the ammoniacal liquor is preferably 3mol/L, institute
The number for stating distillation water washing yellow mercury oxide is preferably 5-8 times.
In step b：The mass ratio of iron chloride and sodium hydroxide is preferably 5-6: 2-3；The solution three and solution four are matched somebody with somebody
During system, the addition of polyethylene glycol is both preferably 4-5ml.
In step c：It is preferred that add palladium bichloride 0.08-0.1g in per 100ml distilled water.
In step c：The mass fraction of the concentrated hydrochloric acid is preferably 36%-38%, and the addition of concentrated hydrochloric acid is preferably 0.5-
1ml。
In step d：The amount ratio of pucherite and palladium chloride solution is preferably 1g: 1-4ml.
In step d：The mass ratio of pucherite and magnetic iron oxide is preferably 1: 0.01-0.5.
The method have the benefit that：
Magnetic oxygenated palladium-pucherite compounded visible light photocatalyst produced by the present invention has magnetic action, makes it can be with
While catalyst activity is kept, facilitate follow-up recycling, greatly reduce cost.
Brief description of the drawings
Fig. 1 is the XRD spectra of magnetic oxygenated palladium-pucherite compounded visible light photocatalyst produced by the present invention.
Embodiment
Below by specific embodiment, the invention will be further described.
Embodiment 1
4.9g bismuth nitrates are weighed, 1.16g ammonium vanadate is dissolved in dust technology with obtaining clear solution in deionized water respectively, by two
Kind solution mixing, 3mol/L ammoniacal liquor regulation pH=7.00 is added while stirring, stands 15min, centrifugation.By yellow mercury oxide
It is multiple with distillation water washing, suspension is diluted with distilled water into after the completion of washing.Suspension is placed in the white of stainless steel
The closed reactor of polytetrafluoroethyllining lining is heat-treated, and reacts 6h at 180 DEG C.Sample after processing through cool drying,
Pucherite is produced after grinding.
PdO-BiVO is prepared using infusion process4Composite photo-catalyst：Weigh the above-mentioned samples of 1.0g to be placed in crucible, instill
4mlPdCl2Solution, being stirred continuously with glass bar makes it well mixed, and dries.Dried sample is in Muffle furnace through 400
DEG C heat treatment 0.5h, take out grinding, be made PdO-BiVO4Composite photo-catalyst.
Weigh iron chloride 5.44g and sodium hydroxide 2.81g is dissolved in distilled water respectively, each add polyethylene glycol 4ml, stirring
Mix under state, sodium hydroxide solution is poured into rapidly 30min is stirred in ferric chloride solution, filter, fully after washing, be placed in baking oven
Dry.Then in 300 DEG C of calcining 1h of Muffle furnace, grinding is taken out, magnetic iron oxide is made.
By PdO-BiVO4Suspension is made with magnetic iron oxide in composite photo-catalyst, calcines 0.5h in 400 DEG C, obtains magnetic
Property palladium oxide-pucherite compounded visible light photocatalyst finished product.
Embodiment 2
Weigh 4.9g bismuth nitrates to be dissolved in 0.6mol/L dust technology at room temperature, be stirred and heated to 70 DEG C, obtain molten
Liquid one.Weigh 1.16g ammonium vanadate to be dissolved in deionized water at room temperature, be stirred and heated to 70 DEG C, obtain solution two.By solution
One and solution two mix while stirring, obtain mixed solution, into mixed solution add 3mol/L ammoniacal liquor, adjust pH to 7.05,
15min is stood, supernatant liquor is poured out and obtains yellow mercury oxide.It is multiple with distillation water washing yellow mercury oxide.Yellow after washing is sunk
Form sediment with 450ml distilled water dilutings into suspension, be placed in the closed reactor of white polytetrafluoroethylpipe liner of stainless steel
6h is reacted in 180 DEG C.By heat-treated products cool drying, pucherite is obtained.
At room temperature, weigh 5.44g iron oxide to be dissolved in 20ml distilled water, add 4ml polyethylene glycol, obtain solution three.Claim
Take 2.81g sodium hydroxides to be dissolved in 20ml distilled water, 4ml polyethylene glycol is added dropwise, obtains solution four., will be molten under stirring
Liquid four is poured into rapidly in solution three, is stirred 30min, room temperature filtering, much filtrate is fully washed, is placed in 100 DEG C of oven drying 6h.
Then 300 DEG C of calcining 1h in Muffle furnace.Post-calcination sample is ground, obtains magnetic iron oxide.
At room temperature, 0.089g palladium bichlorides are weighed to be dissolved in 100ml distilled water, lasting stirring, are heated to 70 DEG C, while stirring
The concentrated hydrochloric acid 0.8ml that mass fraction is 36%-38% is added, is completely dissolved to obtain palladium chloride solution.
At room temperature, 1.0g pucherites are weighed to be placed in crucible, 4ml palladium chloride solutions is added and magnetic iron oxide is a little, use
Glass bar, which is stirred continuously, makes it well mixed, is subsequently placed in drying box and dries, and drying box temperature is 105 DEG C, is placed in Muffle furnace
In in 400 DEG C calcine 0.5h, calcined product take out grinding, obtain magnetic oxygenated palladium-pucherite compounded visible light photocatalyst.
Fig. 1 is the XRD spectra of magnetic oxygenated palladium-pucherite compounded visible light photocatalyst.As shown in Figure 1, γ-Fe2O3-
Pd-BiVO4There are obvious γ-Fe 2 θ=36.5 ° and 63 ° in compounded visible light photocatalyst2O3Characteristic peak, 2 θ=
28.6 °, 30.5 °, 35.2 °, 39.7 ° and 53.1 ° there is monoclinic phase BiVO4Characteristic peak.Because Pd contents are few, do not occur its diffraction spy
Levy peak.But Pd doping substantially increases degradation efficiency of the catalyst to methylene blue.
Comparative example
4.9g bismuth nitrates are weighed, 1.16g ammonium vanadate is dissolved in dust technology with obtaining clear solution in deionized water respectively, by two
Kind solution mixing, 3mol/L ammoniacal liquor regulation pH=7.00 is added while stirring, stands 15min, centrifugation.By yellow mercury oxide
It is multiple with distillation water washing, suspension is diluted with distilled water into after the completion of washing.Suspension is placed in the white of stainless steel
The closed reactor of polytetrafluoroethyllining lining is heat-treated, and reacts 6h at 180 DEG C.Sample after processing through cool drying,
Pucherite is produced after grinding.
PdO-BiVO is prepared using infusion process4Composite photo-catalyst：Weigh the above-mentioned samples of 1.0g to be placed in crucible, instill
4mlPdCl2Solution, being stirred continuously with glass bar makes it well mixed, and dries.Dried sample is in Muffle furnace through 400
DEG C heat treatment 0.5h, take out grinding, be made PdO-BiVO4Compounded visible light photocatalyst.
Embodiment 1, embodiment 2 and compounded visible light photocatalyst 0.5g made from comparative example, catalytic degradation are weighed respectively
30ml mass concentrations are 5g/ml methylene blue 2.5h, and temperature is 20 DEG C, and 1 is shown in Table to the clearance of methylene blue.
Table 1
| Embodiment 1 | Embodiment 2 | Comparative example | |
| Clearance (%) | 98.42% | 98.39% | 98.42% |
As shown in Table 1, the magnetic PdO/BiVO that prepared by embodiment 1 and embodiment 24Composite visible light catalyst is in experiment bar
There is higher degradation rate under part to methylene blue, be provided simultaneously with advantage capable of magnetic separating.Pass through the ratio of embodiment 1,2 and comparative example
Compared with it can also be seen that using the inventive method to PdO/BiVO4, can't be to catalyst when composite visible light catalyst assigns magnetic
Activity impact.
Embodiments of the invention are the foregoing is only, are not thereby limited the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent process that bright specification is made exchange, or are directly or indirectly used in other association areas, similarly wrap
Include in the protection protection domain of the present invention.
Claims (5)
1. a kind of preparation method of magnetic oxygenated palladium-pucherite compounded visible light photocatalyst, it is characterised in that including following step
Suddenly：
Bismuth nitrate is dissolved in dust technology by a, is heated to 50-70 DEG C, obtains solution one；Ammonium vanadate is dissolved in deionized water, added
Heat obtains solution two to 50-70 DEG C；Solution one and solution two are mixed while stirring, obtain mixed solution, into mixed solution
Ammoniacal liquor is added, pH to 6.5-7.5 is adjusted, stratification, pours out supernatant liquor and obtain yellow mercury oxide, is sunk with distillation water washing yellow
Form sediment；Yellow mercury oxide after washing is diluted with distilled water into suspension, is placed in the closed stainless steel reaction of polytetrafluoroethyllining lining
It is heat-treated in kettle, temperature is 180-200 DEG C, time 6h；After being disposed, heat-treated products cool drying obtains
Pucherite；
Iron chloride is dissolved in distilled water by b, then adds polyethylene glycol, obtains solution three；Sodium hydroxide is dissolved in distilled water,
Then polyethylene glycol is added, obtains solution four；Solution four is poured into rapidly in solution three, stirs 30-45min, then filtering, will
Oven drying is placed in after much filtrate washing, oven temperature is 70-100 DEG C, drying time 5-7h, after the completion of drying, will be filtered out
Thing is placed in Muffle furnace and calcined, and calcining heat is 300 DEG C, time 1h, takes out calcined product after the completion of calcining, is down to
Room temperature, it is ground, obtains magnetic iron oxide；
Palladium bichloride is dissolved in distilled water by c, lasting stirring, is heated to 50-70 DEG C, then adds concentrated hydrochloric acid, be completely dissolved to obtain
Palladium chloride solution；
Pucherite made from step a is placed in crucible by d, palladium chloride solution made from step c is then added into crucible, then add
Enter magnetic iron oxide made from step b, being stirred continuously with glass bar makes it well mixed, is subsequently placed in drying box and dries, and does
Dry box temperature degree is 100-110 DEG C, takes out dried object after the completion of drying, is placed in Muffle furnace and is calcined, calcining heat 400
DEG C, calcination time 0.5h, calcined product is taken out after the completion of calcining and ground, it is compound visible to obtain magnetic oxygenated palladium-pucherite
Light photochemical catalyst；
In step b：The mass ratio of iron chloride and sodium hydroxide is 5-6: 2-3；In the process for preparation of the solution three and solution four,
The addition of polyethylene glycol is 4-5ml；
In step d：The amount ratio of pucherite and palladium chloride solution is 1g: 1-4ml；The mass ratio of pucherite and magnetic iron oxide is
1∶0.01-0.5。
2. a kind of preparation method of magnetic oxygenated palladium-pucherite compounded visible light photocatalyst according to claim 1, its
It is characterised by, in step a：The mass ratio of bismuth nitrate and ammonium vanadate is 4-6: 1-1.5.
3. a kind of preparation method of magnetic oxygenated palladium-pucherite compounded visible light photocatalyst according to claim 1, its
It is characterised by, in step a：The concentration of the dust technology is 0.6mol/L；The concentration of the ammoniacal liquor is 3mol/L, the distilled water
The number for washing yellow mercury oxide is 5-8 times.
4. a kind of preparation method of magnetic oxygenated palladium-pucherite compounded visible light photocatalyst according to claim 1, its
It is characterised by, in step c：Palladium bichloride 0.08-0.1g is added in per 100ml distilled water.
5. a kind of preparation method of magnetic oxygenated palladium-pucherite compounded visible light photocatalyst according to claim 1, its
It is characterised by, in step c：The mass fraction of the concentrated hydrochloric acid is 36%-38%, and the addition of concentrated hydrochloric acid is 0.5-1ml.
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| CN107899570A (en) * | 2017-11-28 | 2018-04-13 | 秦皇岛天大环保研究院有限公司 | Integral catalyzer for super low concentration methyl hydride combustion and preparation method thereof |
| CN108543536A (en) * | 2018-03-14 | 2018-09-18 | 西安建筑科技大学 | A kind of pucherite-calcium ferrite composite photo-catalyst, preparation method and applications |
| CN113351222A (en) * | 2021-06-23 | 2021-09-07 | 湖北民族大学 | Bismuth vanadate and manganese dioxide magnetic composite photocatalysis-oxidizing agent and preparation method thereof |
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