CN109331822A - A kind of photocatalysis benzyl alcohol oxidation Au-Pd alloy catalyst and the preparation method and application thereof - Google Patents
A kind of photocatalysis benzyl alcohol oxidation Au-Pd alloy catalyst and the preparation method and application thereof Download PDFInfo
- Publication number
- CN109331822A CN109331822A CN201811365696.2A CN201811365696A CN109331822A CN 109331822 A CN109331822 A CN 109331822A CN 201811365696 A CN201811365696 A CN 201811365696A CN 109331822 A CN109331822 A CN 109331822A
- Authority
- CN
- China
- Prior art keywords
- tio
- catalyst
- photochemical catalyst
- added
- benzyl alcohol
- 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.)
- Pending
Links
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000003054 catalyst Substances 0.000 title claims abstract description 52
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 42
- 239000000956 alloy Substances 0.000 title claims abstract description 42
- 229910002710 Au-Pd Inorganic materials 0.000 title claims abstract description 31
- 235000019445 benzyl alcohol Nutrition 0.000 title claims abstract description 22
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 16
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 16
- 238000007254 oxidation reaction Methods 0.000 title abstract description 18
- 230000003647 oxidation Effects 0.000 title abstract description 15
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000002070 nanowire Substances 0.000 claims abstract description 42
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 26
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims abstract description 15
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 19
- 238000006555 catalytic reaction Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 13
- 239000010931 gold Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 241000218636 Thuja Species 0.000 claims description 7
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 235000008109 Thuja occidentalis Nutrition 0.000 claims description 4
- 229910052736 halogen Inorganic materials 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 2
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 2
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 238000005406 washing Methods 0.000 description 13
- 238000001027 hydrothermal synthesis Methods 0.000 description 10
- 229910052737 gold Inorganic materials 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 229910052763 palladium Inorganic materials 0.000 description 5
- 238000005554 pickling Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 235000012149 noodles Nutrition 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000002407 reforming Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910002708 Au–Cu Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000002153 concerted effect Effects 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 150000002940 palladium Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
-
- 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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/37—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups
- C07C45/38—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups being a primary hydroxyl group
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of Au-Pd/TiO2Nanowire alloys photochemical catalyst and the preparation method and application thereof, Au-Pd alloy is loaded to TiO by the present invention2Nanowire surface, Au-Pd/TiO obtained2Catalyst shows higher activity in the reaction that the solvent-free liquid phase oxidation of photocatalysis benzyl alcohol prepares benzaldehyde.
Description
(1) technical field
The present invention relates to a kind of Au-Pd alloy catalysts, prepare more particularly, to one kind for photocatalysis benzyl alcohol oxidation
The Au-Pd alloy modification TiO of benzaldehyde2Nano-wire catalyst and preparation method thereof.
(2) background technique
Bimetal nanostructure often has any one list better than its composition because possessing peculiar electronic structure
The concerted catalysis of metal and light reaction catalytic performance.There are many kinds of structure, common structures alloy knot for bimetal nano material
Structure, core-shell structure, metal nanometre cluster etc., these bimetal nano materials can be formed different by control preparation method
Heterojunction structure.The bimetal nano catalyst of alloy structure because surface atom composition and sequence, particle radius etc. it is numerous because
The influence of element, so physics, the performances such as chemistry can all have nothing in common with each other.The catalyst of general bimetallic alloy structure and reactant
There is many differences compared with its single-metal reforming catalyst for mode of action when effect.Because of bimetal nano alloy structure
Metal between have stronger active force, this will improve mode of the catalyst surface in conjunction with reactant, therefore bimetallic is received
Rice alloy structure can effectively promote going on smoothly for reaction.For example, Au-Ag bimetallic catalyst (Journal of
Catalysis 2013,301,217-226.), Au-Cu bimetallic catalyst (Journal of Materials Chemistry
A 2014,2,16292-16298.) in the presence of oxygen catalysis oxidation benzyl alcohol oxidation reaction in conversion ratio and choosing
Selecting property is all higher than any one single-metal reforming catalyst for constituting its composition.
Compared with powder nanometer catalysis material, one dimension semiconductor nano-photocatalyst material have great aspect ratio and
Quite high electronics rate travel, therefore it can express high light catalytic performance (Nanoscale 2014,7,209-217).
The present invention utilizes the one-dimensional TiO of Au-Pd alloy modification2Nanowire semiconductor material prepares Au-Pd/TiO2Nanowire alloys photocatalysis
Agent, and benzaldehyde is prepared for solvent-free photocatalysis benzyl alcohol oxidation.Currently, having no Au-Pd alloy modification TiO2Nano wire is simultaneously
The report of benzaldehyde is prepared for solvent-free photochemical catalytic oxidation benzyl alcohol.
(3) summary of the invention
The present invention is intended to provide a kind of Au-Pd alloy modification TiO for preparing benzaldehyde for photocatalysis benzyl alcohol oxidation2It receives
Rice noodles catalyst and preparation method thereof.
Technical scheme is as follows:
A kind of Au-Pd/TiO2Nanowire alloys photochemical catalyst is prepared as follows to obtain:
(1) by TiO2(P25) powder is added in the NaOH aqueous solution of 30~50wt%, is stirred evenly, it is warming up to 180~
280 DEG C of 20~70h of reaction, are down to room temperature (20~30 DEG C) to reaction system later, and filtering, filter cake passes through (0.1mol/L) HCl/water
Solution washing, deionized water washing, (60 DEG C) vacuum drying, then by obtained solid powder in air atmosphere, 250~650 DEG C
2~6h of lower roasting, obtains one-dimensional TiO2Nano wire；
The volumetric usage of the NaOH aqueous solution is with TiO2The quality of powder is calculated as 50~100mL/g；
(2) after the leaf of arbor-vitae plant (C.Platycladi) being dried, crushed, add by feed liquid mass ratio 1:50~200
Into deionized water, 1~4h is stirred, filtering obtains arbor-vitae filtrate, and Pd presoma, Au forerunner are added into gained arbor-vitae filtrate
Body, obtain Pd content 0.0001~0.0003g/mL, Au content 0.0001~0.003g/mL mixed liquor, then by institute
It obtains mixed liquor and is warming up to 60~100 DEG C of 1~3h of stirring, obtain alloy solution；
The Pd presoma preferably soluble palladium salt, such as palladium chloride, palladium nitrate etc.；
Described Au presoma such as gold chloride etc.；
(3) by one-dimensional TiO obtained by step (1)2Nano wire is added in alloy solution obtained by step (2), stirs 1~3h,
Filtering, filter cake obtain powdered Au-Pd/TiO through washing, (60 DEG C) vacuum drying2Nanowire alloys photochemical catalyst；
The volumetric usage of the alloy solution is with one-dimensional TiO2The quality of nano wire is calculated as 50~200mL/g.
Au-Pd/TiO produced by the present invention2Nanowire alloys photochemical catalyst alloy load capacity is 0.5~2wt%.
Au-Pd/TiO produced by the present invention2Nanowire alloys photochemical catalyst can be applied to the solvent-free liquid of photocatalysis benzyl alcohol
Phase oxidation is prepared in the reaction of benzaldehyde.Specifically, the method for the application are as follows:
The catalyst is added in benzyl alcohol, 90 DEG C of preheating 5min simultaneously flow back (75~110 DEG C), with the speed of 90mL/min
Degree is passed through oxygen, and the gold-halogen lamp light source for opening simultaneously 150W carries out light-catalyzed reaction, and HPLC is monitored to fully reacting；
The quality dosage of the catalyst is calculated as 0.005~0.015g/mL with the volume of benzyl alcohol.
Compared with prior art, the beneficial effects of the present invention are: Au-Pd alloy is loaded to TiO by the present invention2Nano wire
Surface, Au-Pd/TiO obtained2Catalyst shows in the reaction that the solvent-free liquid phase oxidation of photocatalysis benzyl alcohol prepares benzaldehyde
Higher activity out.
(4) Detailed description of the invention
Fig. 1 is Au-Pd/TiO prepared by embodiment 52The STEM of nanowire alloys photochemical catalyst schemes (a), and Au member vegetarian noodles is swept
Figure (b) and Pd member vegetarian noodles sweep figure (c).
(5) specific embodiment
Below by specific embodiment, the invention will be further described, but protection scope of the present invention is not limited in
This.
Embodiment 1
By the TiO of 1.5g2(P25 creates Degussa EVONIK-DEGUSSA purchased from winning) powder is added to 100mL 40wt%
In NaOH aqueous solution, 30min is sufficiently stirred, and transfers the solution into the hydrothermal reaction kettle of 200mL, under conditions of 200 DEG C
Hydro-thermal reaction 48h is down to room temperature later, filtering, and filter cake is by 0.1mol/L HCl pickling, deionized water washing, 60 DEG C of vacuum
It is dry, and by obtained powder in air atmosphere 250 DEG C of roasting 4h, one-dimensional TiO can be obtained2- 250 nano wires.
Arbor-vitae plant leaves are dried, are crushed, 2g is taken to add 200mL water, is filtered after stirring 2h, is obtained filtrate A, take 30mL's
Filtrate A and 30mL deionized water, it is 49mM that palladium nitrate aqueous solution that 765 μ L concentration are 74mM and 622 μ L concentration are added after mixing
Aqueous solution of chloraurate, stir 1.0h under conditions of 90 DEG C, obtain solution B, by 0.6g TiO2- 250 nano wires are added to solution
In B, making the load capacity of Au and Pd is all 1wt%, and filtering, washing, 60 DEG C of vacuum drying after 1h are sufficiently stirred, obtain powdered
Au-Pd/TiO2- 250 nanowire alloys photochemical catalyst A.
Benzyl alcohol oxidation reaction: being added 0.1g catalyst A, and 10mL benzyl alcohol be added in 50mL three-necked flask, later will
Three-necked flask, which is placed in 90 DEG C of oil bath pans, to be preheated 5min and flows back, and is passed through the oxygen of 90mL/min later, is opened the golden halogen of 150W
Lamp source starts light-catalyzed reaction, after reacting 4h, sampling analysis.Catalysis reaction result is shown in Table 1.
Embodiment 2
Catalyst A is prepared according to the method for embodiment 1, and is reacted for photocatalysis benzyl alcohol oxidation, 50mL three-necked flask
Middle addition 0.1g catalyst A, and 10mL benzyl alcohol is added, three-necked flask is placed in 90 DEG C of oil bath pans later and preheats 5min and returns
Stream, is passed through the oxygen of 90mL/min later, and the gold-halogen lamp light source for opening 150W starts light-catalyzed reaction, after reacting 6h, sampling point
Analysis.Catalysis reaction result is shown in Table 1.
Embodiment 3
By the TiO of 1.5g2(P25) powder is added in 100mL 40wt%NaOH aqueous solution, and 30min is sufficiently stirred, and
It transferring the solution into the hydrothermal reaction kettle of 200mL, hydro-thermal reaction 48h under conditions of 200 DEG C is down to room temperature later, filtering,
Filter cake is dried in vacuo by 0.1mol/L HCl pickling, deionized water washing, 60 DEG C, and by obtained powder in air atmosphere
350 DEG C of roasting 4h, can be obtained one-dimensional TiO2- 350 nano wires.
Filtrate A and the 30mL deionized water for taking 30mL, be added after mixing 765 μ L concentration be 74mM palladium nitrate aqueous solution and
622 μ L concentration are the aqueous solution of chloraurate of 49mM, stir 1.0h under conditions of 90 DEG C, obtain solution B, by 0.6g TiO2-350
Nano wire is added in solution B, and making the load capacity of Au and Pd is all 1wt%, and filtering, washing, 60 DEG C of vacuum after 1h is sufficiently stirred
It is dry, obtain powdered Au-Pd/TiO2- 350 nanowire alloys photochemical catalyst B.Evaluating catalyst condition is the same as embodiment 1, catalysis
Reaction result is shown in Table 1.
Embodiment 4
Catalyst B is prepared according to the method for embodiment 3, and is reacted for photocatalysis benzyl alcohol oxidation, evaluating catalyst item
Part is catalyzed reaction result and is shown in Table 1 with embodiment 2.
Embodiment 5
By the TiO of 1.5g2(P25) powder is added in 100mL 40wt%NaOH aqueous solution, and 30min is sufficiently stirred, and
It transferring the solution into the hydrothermal reaction kettle of 200mL, hydro-thermal reaction 48h under conditions of 200 DEG C is down to room temperature later, filtering,
Filter cake is dried in vacuo by 0.1mol/L HCl pickling, deionized water washing, 60 DEG C, and by obtained powder in air atmosphere
450 DEG C of roasting 4h, can be obtained one-dimensional TiO2- 450 nano wires.
Filtrate A and the 30mL deionized water for taking 30mL, be added after mixing 765 μ L concentration be 74mM palladium nitrate aqueous solution and
622 μ L concentration are the aqueous solution of chloraurate of 49mM, stir 1.0h under conditions of 90 DEG C, obtain solution B, by 0.6g TiO2-450
Nano wire is added in solution B, and making the load capacity of Au and Pd is all 1wt%, and filtering, washing, 60 DEG C of vacuum after 1h is sufficiently stirred
It is dry, obtain powdered Au-Pd/TiO2- 450 nanowire alloys photochemical catalyst C.Evaluating catalyst condition is the same as embodiment 1, catalysis
Reaction result is shown in Table 1.
Embodiment 6
Catalyst C is prepared according to the method for embodiment 5, and is reacted for photocatalysis benzyl alcohol oxidation, evaluating catalyst item
Part is catalyzed reaction result and is shown in Table 1 with embodiment 2.
Embodiment 7
By the TiO of 1.5g2(P25) powder is added in 100mL 40wt%NaOH aqueous solution, and 30min is sufficiently stirred, and
It transferring the solution into the hydrothermal reaction kettle of 200mL, hydro-thermal reaction 48h under conditions of 200 DEG C is down to room temperature later, filtering,
Filter cake is dried in vacuo by 0.1mol/L HCl pickling, deionized water washing, 60 DEG C, and by obtained powder in air atmosphere
550 DEG C of roasting 4h, can be obtained one-dimensional TiO2- 550 nano wires.
Filtrate A and the 30mL deionized water for taking 30mL, be added after mixing 765 μ L concentration be 74mM palladium nitrate aqueous solution and
622 μ L concentration are the aqueous solution of chloraurate of 49mM, stir 1.0h under conditions of 90 DEG C, obtain solution B, by 0.6g TiO2-550
Nano wire is added in solution B, and making the load capacity of Au and Pd is all 1wt%, and filtering, washing, 60 DEG C of vacuum after 1h is sufficiently stirred
It is dry, obtain powdered Au-Pd/TiO2- 550 nanowire alloys photochemical catalyst D.Evaluating catalyst condition is the same as embodiment 1, catalysis
Reaction result is shown in Table 1.
Embodiment 8
Catalyst D is prepared according to the method for embodiment 7, and is reacted for photocatalysis benzyl alcohol oxidation, evaluating catalyst item
Part is catalyzed reaction result and is shown in Table 1 with embodiment 2.
Embodiment 9
By the TiO of 1.5g2(P25) powder is added in 100mL 40wt%NaOH aqueous solution, and 30min is sufficiently stirred, and
It transferring the solution into the hydrothermal reaction kettle of 200mL, hydro-thermal reaction 48h under conditions of 200 DEG C is down to room temperature later, filtering,
Filter cake is dried in vacuo by 0.1mol/L HCl pickling, deionized water washing, 60 DEG C, and by obtained powder in air atmosphere
650 DEG C of roasting 4h, can be obtained one-dimensional TiO2- 650 nano wires.
Filtrate A and the 30mL deionized water for taking 30mL, be added after mixing 765 μ L concentration be 74mM palladium nitrate aqueous solution and
622 μ L concentration are the aqueous solution of chloraurate of 49mM, stir 1.0h under conditions of 90 DEG C, obtain solution B, by 0.6g TiO2-650
Nano wire is added in solution B, and making the load capacity of Au and Pd is all 1wt%, and filtering, washing, 60 DEG C of vacuum after 1h is sufficiently stirred
It is dry, obtain powdered Au-Pd/TiO2- 650 nanowire alloys photochemical catalyst E.Evaluating catalyst condition is the same as embodiment 1, catalysis
Reaction result is shown in Table 1.
Embodiment 10
Catalyst E is prepared according to the method for embodiment 9, and is reacted for photocatalysis benzyl alcohol oxidation, evaluating catalyst item
Part is catalyzed reaction result and is shown in Table 1 with embodiment 2.
Table 1Au-Pd/TiO2Nanowire alloys catalyst photocatalysis benzyl alcohol oxidation reactivity worth
Claims (8)
1. a kind of Au-Pd/TiO2Nanowire alloys photochemical catalyst, which is characterized in that be prepared as follows to obtain:
(1) by TiO2Powder is added in the NaOH aqueous solution of 30~50wt%, is stirred evenly, and 180~280 DEG C of reactions are warming up to
20~70h is down to room temperature to reaction system later, filtering, and filter cake is washed through HCL aqueous solution, deionized water is washed, and vacuum is dry
It is dry, then obtained solid powder is roasted to 2~6h in air atmosphere, at 250~650 DEG C, obtain one-dimensional TiO2Nano wire；
(2) it after the leaf of arbor-vitae plant being dried, crushed, is added in deionized water by feed liquid mass ratio 1:50~200, stirring 1
~4h, filtering, obtains arbor-vitae filtrate, and Pd presoma, Au presoma are added into gained arbor-vitae filtrate, obtains Pd content and exists
Gained mixed liquor is then warming up to 60 in the mixed liquor of 0.0001~0.003g/mL by 0.0001~0.0003g/mL, Au content
~100 DEG C of 1~3h of stirring, obtain alloy solution；
(3) by one-dimensional TiO obtained by step (1)2Nano wire is added in alloy solution obtained by step (2), stirs 1~3h, is filtered,
Filter cake is washed, is dried in vacuo, and powdered Au-Pd/TiO is obtained2Nanowire alloys photochemical catalyst.
2. Au-Pd/TiO as described in claim 12Nanowire alloys photochemical catalyst, which is characterized in that described in step (1)
TiO2Powder is titanium dioxide P25 powder.
3. Au-Pd/TiO as described in claim 12Nanowire alloys photochemical catalyst, which is characterized in that described in step (1)
The volumetric usage of NaOH aqueous solution is with TiO2The quality of powder is calculated as 50~100mL/g.
4. Au-Pd/TiO as described in claim 12Nanowire alloys photochemical catalyst, which is characterized in that described in step (2)
Pd presoma is palladium chloride or palladium nitrate.
5. Au-Pd/TiO as described in claim 12Nanowire alloys photochemical catalyst, which is characterized in that described in step (2)
Au presoma is gold chloride.
6. Au-Pd/TiO as described in claim 12Nanowire alloys photochemical catalyst, which is characterized in that described in step (3)
The volumetric usage of alloy solution is with one-dimensional TiO2The quality of nano wire is calculated as 50~200mL/g.
7. Au-Pd/TiO as described in claim 12Nanowire alloys photochemical catalyst is in the solvent-free Oxygen in Liquid of photocatalysis benzyl alcohol
Change prepares the application in the reaction of benzaldehyde.
8. the use as claimed in claim 7, which is characterized in that the method for the application are as follows:
The catalyst is added in benzyl alcohol, 90 DEG C of preheating 5min simultaneously flow back, and are passed through oxygen with the speed of 90mL/min, simultaneously
The gold-halogen lamp light source for opening 150W carries out light-catalyzed reaction, and HPLC is monitored to fully reacting；
The quality dosage of the catalyst is calculated as 0.005~0.015g/mL with the volume of benzyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811365696.2A CN109331822A (en) | 2018-11-16 | 2018-11-16 | A kind of photocatalysis benzyl alcohol oxidation Au-Pd alloy catalyst and the preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811365696.2A CN109331822A (en) | 2018-11-16 | 2018-11-16 | A kind of photocatalysis benzyl alcohol oxidation Au-Pd alloy catalyst and the preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109331822A true CN109331822A (en) | 2019-02-15 |
Family
ID=65315702
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811365696.2A Pending CN109331822A (en) | 2018-11-16 | 2018-11-16 | A kind of photocatalysis benzyl alcohol oxidation Au-Pd alloy catalyst and the preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109331822A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109876843A (en) * | 2019-03-08 | 2019-06-14 | 北京化工大学 | Copper alloy modified titanic oxide/carbonitride heterojunction photocatalyst and preparation method |
| CN111185199A (en) * | 2020-01-22 | 2020-05-22 | 天津理工大学 | Z-type heterojunction photocatalyst and preparation method and application thereof |
| CN111359670A (en) * | 2020-03-10 | 2020-07-03 | 浙江工业大学 | Au-Pd/NH2-MIL-101(Cr) catalyst and preparation and application thereof |
| CN114272947A (en) * | 2022-01-05 | 2022-04-05 | 陕西科技大学 | Catalyst for preparing benzaldehyde by solvent-free benzyl alcohol oxidation and preparation method and application thereof |
| CN114425332A (en) * | 2022-02-24 | 2022-05-03 | 河南科技大学 | Preparation method and application of Au-Pd micro-flowers constructed by ultrathin nanosheets |
| CN114588897A (en) * | 2022-03-25 | 2022-06-07 | 安徽工程大学 | Composite porous photocatalyst material and preparation method and application thereof |
| CN114733520A (en) * | 2022-04-02 | 2022-07-12 | 烟台大学 | Preparation method and application of supported nano-gold catalyst |
| CN115121262A (en) * | 2022-07-08 | 2022-09-30 | 太原工业学院 | Method for preparing cinnamaldehyde by oxidizing hydrotalcite-supported Au-Co alloy photocatalytic cinnamyl alcohol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105536779A (en) * | 2015-12-31 | 2016-05-04 | 浙江工业大学 | Preparation method of Pd/TiO2 nanowire catalyst, prepared catalyst and application thereof |
| CN106892482A (en) * | 2017-01-04 | 2017-06-27 | 浙江工业大学 | A kind of black TiO2Nano material and preparation method and application |
| CN107890867A (en) * | 2017-12-15 | 2018-04-10 | 浙江工业大学 | A kind of grey Pd/TiO2Nano wire photochemical catalyst and its preparation method and application |
-
2018
- 2018-11-16 CN CN201811365696.2A patent/CN109331822A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105536779A (en) * | 2015-12-31 | 2016-05-04 | 浙江工业大学 | Preparation method of Pd/TiO2 nanowire catalyst, prepared catalyst and application thereof |
| CN106892482A (en) * | 2017-01-04 | 2017-06-27 | 浙江工业大学 | A kind of black TiO2Nano material and preparation method and application |
| CN107890867A (en) * | 2017-12-15 | 2018-04-10 | 浙江工业大学 | A kind of grey Pd/TiO2Nano wire photochemical catalyst and its preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| 刘明明: "纳米Pd负载TiO2纳米线的制备及其苯甲醇氧化反应", 《道客巴巴》 * |
| 姜彤彤: "Au-Pd双金属催化剂的制备及其催化性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109876843A (en) * | 2019-03-08 | 2019-06-14 | 北京化工大学 | Copper alloy modified titanic oxide/carbonitride heterojunction photocatalyst and preparation method |
| CN111185199A (en) * | 2020-01-22 | 2020-05-22 | 天津理工大学 | Z-type heterojunction photocatalyst and preparation method and application thereof |
| CN111359670A (en) * | 2020-03-10 | 2020-07-03 | 浙江工业大学 | Au-Pd/NH2-MIL-101(Cr) catalyst and preparation and application thereof |
| CN114272947A (en) * | 2022-01-05 | 2022-04-05 | 陕西科技大学 | Catalyst for preparing benzaldehyde by solvent-free benzyl alcohol oxidation and preparation method and application thereof |
| CN114425332A (en) * | 2022-02-24 | 2022-05-03 | 河南科技大学 | Preparation method and application of Au-Pd micro-flowers constructed by ultrathin nanosheets |
| CN114588897A (en) * | 2022-03-25 | 2022-06-07 | 安徽工程大学 | Composite porous photocatalyst material and preparation method and application thereof |
| CN114733520A (en) * | 2022-04-02 | 2022-07-12 | 烟台大学 | Preparation method and application of supported nano-gold catalyst |
| CN114733520B (en) * | 2022-04-02 | 2023-11-21 | 烟台大学 | Preparation method and application of supported nano gold catalyst |
| CN115121262A (en) * | 2022-07-08 | 2022-09-30 | 太原工业学院 | Method for preparing cinnamaldehyde by oxidizing hydrotalcite-supported Au-Co alloy photocatalytic cinnamyl alcohol |
| CN115121262B (en) * | 2022-07-08 | 2024-02-02 | 太原工业学院 | Method for preparing cinnamaldehyde by photocatalytic cinnamyl alcohol oxidation of water-skid-supported Au-Co alloy |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109331822A (en) | A kind of photocatalysis benzyl alcohol oxidation Au-Pd alloy catalyst and the preparation method and application thereof | |
| CN103209765B (en) | Sinter stable heterogeneous catalyst | |
| CN102883809B (en) | Preparation has the method for the catalyst of the noble metal nano particles being deposited on carrier | |
| CN104549368B (en) | A kind of supported bi-metallic type Cu Pt/TiO2The preparation method of NBs catalyst and application | |
| CN106732567B (en) | A kind of metal composite oxide supported active metals catalyst and preparation method thereof | |
| CN107855133B (en) | Method for preparing supported small-particle gold catalyst | |
| CN105536779B (en) | A kind of preparation method of Pd/TiO2 nano-wire catalyst, catalyst obtained and its application | |
| CN100471558C (en) | Compound having a pyrochlore-structure and its use as a catalyst carrier in water gas shift reaction | |
| CN109939693B (en) | CoMn2O4Bimetallic oxide catalyst, preparation method and application | |
| CN107812520A (en) | A kind of loading type silver catalyst preparation method for purifying formaldehyde | |
| CN107890867A (en) | A kind of grey Pd/TiO2Nano wire photochemical catalyst and its preparation method and application | |
| CN103691434B (en) | A kind of metallic catalyst and preparation method and application | |
| JP2005509515A (en) | Heterogeneous catalysts constituting aggregates of metal-coated nanoparticles | |
| CN110252298B (en) | Catalyst for preparing DHA (docosahexaenoic acid) by efficiently catalyzing glycerol through metal oxide supported gold and preparation method thereof | |
| CN108889303A (en) | The support type high dispersive copper-based catalysts and preparation method of carbon dioxide methanol and application | |
| CN109174092B (en) | Zinc oxide/platinum composite material microsphere and preparation method and application thereof | |
| JP5269892B2 (en) | Process for the preparation of cobalt-zinc oxide Fischer-Tropsch catalyst | |
| CN107915255A (en) | The preparation method of nano zircite and its nano zircite of preparation | |
| CN109331819A (en) | Titanium dioxide load-type Pt-Pd bimetallic photochemical catalyst and the preparation method and application thereof | |
| JP5822349B2 (en) | Oxidation catalyst for organic sulfur compounds | |
| CN110339844A (en) | Fe nanometer rods and Pt@Fe Nanorods Catalyst and synthesis and application | |
| CN111359670A (en) | Au-Pd/NH2-MIL-101(Cr) catalyst and preparation and application thereof | |
| CN106994342A (en) | A kind of preparation method of photochemical catalyst | |
| CN114425333B (en) | Catalyst for methane catalytic combustion and preparation method thereof | |
| JP6086622B2 (en) | Oxidation catalyst for organic sulfur compound, method for producing oxidation catalyst for organic sulfur compound, method for selectively oxidizing organic sulfur compound |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190215 |
|
| RJ01 | Rejection of invention patent application after publication |