CN108906077A - A kind of zinc oxide synthetic method of Pd-Cu modification - Google Patents
A kind of zinc oxide synthetic method of Pd-Cu modification Download PDFInfo
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- CN108906077A CN108906077A CN201810749573.2A CN201810749573A CN108906077A CN 108906077 A CN108906077 A CN 108906077A CN 201810749573 A CN201810749573 A CN 201810749573A CN 108906077 A CN108906077 A CN 108906077A
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- Prior art keywords
- zinc
- zinc oxide
- modification
- aqueous solution
- synthetic method
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910002668 Pd-Cu Inorganic materials 0.000 title claims abstract description 20
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 18
- 230000004048 modification Effects 0.000 title claims abstract description 14
- 238000012986 modification Methods 0.000 title claims abstract description 14
- 238000010189 synthetic method Methods 0.000 title claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims abstract description 14
- 230000001376 precipitating effect Effects 0.000 claims abstract description 10
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 9
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 9
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229960004011 methenamine Drugs 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 150000003751 zinc Chemical class 0.000 claims abstract description 5
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- ZPEJZWGMHAKWNL-UHFFFAOYSA-L zinc;oxalate Chemical compound [Zn+2].[O-]C(=O)C([O-])=O ZPEJZWGMHAKWNL-UHFFFAOYSA-L 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000000446 fuel Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- GJCXHYNLSNVSQZ-UHFFFAOYSA-L [Cu](Cl)Cl.Cl Chemical compound [Cu](Cl)Cl.Cl GJCXHYNLSNVSQZ-UHFFFAOYSA-L 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8953—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
-
- 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
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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 present invention provides a kind of zinc oxide synthetic method of Pd-Cu modification, which is characterized in that includes the following steps：(1) zinc salt is added in the strong alkali aqueous solution of 8~10mol/L, methenamine is added, is put into 50~70 DEG C of baking ovens and reacts 4~6 hours, precipitating is obtained by filtration.(2) by precipitating ultrasonic disperse into the aqueous solution containing copper chloride and palladium chloride, and it is stirred continuously until that solvent is evaporated naturally；(3) residue after being evaporated is put into 200~300 DEG C of Muffle furnaces and is calcined 4~6 hours, obtain the zinc oxide that load has Pd-Cu.Synthesis technology of the present invention is simple, and the zinc oxide intensity of the Pd-Cu modification of synthesis is high, activity stabilized longer, can be widely used for the fields such as environmental protection, sensor, fuel cell.
Description
Technical field
The invention belongs to material chemistry technical fields, are related to a kind of zinc oxide synthetic method of Pd-Cu modification.
Background technique
Palladium chloride and palladium chloride-copper chloride system are the catalyst systems haveing excellent performance, environmental protection, fuel cell,
Many fields such as sensor can be used for the room-temperature catalytic oxidation of carbon monoxide.Aluminium oxide, titanium oxide, the active carbon of micron or nanometer
It is all common catalytic carrier, catalyst active component, which loads to, improves utilization efficiency on carrier.Zinc oxide is that one kind generally makes
Catalysis material, the present invention propose a kind of synthetic method of Pd-Cu modification ZnO submicron material catalyst system.
Summary of the invention
The purpose of the present invention is to provide a kind of zinc oxide synthetic methods of Pd-Cu modification, which is characterized in that including as follows
Step：
(1) zinc salt is added in the strong alkali aqueous solution of 8~10mol/L, methenamine is added, is put into 50~70 DEG C of baking ovens
Reaction 4~6 hours, is obtained by filtration precipitating.
(2) by precipitating ultrasonic disperse into the aqueous solution containing copper chloride and palladium chloride, and it is stirred continuously until solvent certainly
So it is evaporated；
(3) residue after being evaporated is put into 200~300 DEG C of Muffle furnaces and is calcined 4~6 hours, obtaining load has Pd-Cu
Zinc oxide.
The zinc salt includes one of zinc chloride, zinc acetate, zinc oxalate, zinc nitrate or combinations thereof, and concentration 0.1~
0.5mol/L；0.1~0.2mol/L of methenamine concentration.
Palladium chloride concentration is 0.5~2gL in the aqueous solution-1, chlorination copper mass be 1~4 times of palladium chloride quality, dispersion
Precipitophore quality is palladium chloride and 4~8 times of copper chloride gross mass in aqueous solution.
Synthesis technology of the present invention is simple, and the zinc oxide intensity of the Pd-Cu modification of synthesis is high, activity stabilized longer, can be extensive
For fields such as environmental protection, sensor, fuel cells.
The contents of the present invention and feature have revealed that as above, however the present invention that describes of front only briefly or pertains only to this
The specific part of invention, feature of the invention may be more than what content disclosed herein was related to.Therefore, protection model of the invention
The revealed content of embodiment should be not limited to by enclosing, and should include the combination of all the elements embodied in different piece, with
And it is various without departing substantially from replacement and modification of the invention, and covered by claims of the present invention.
Detailed description of the invention
The zinc oxide scanning electron microscope pattern that Fig. 1 is modified using (embodiment 1) of the invention synthesis Pd-Cu.
Specific embodiment
Embodiment 1
(1) 0.1mol/L zinc chloride is added in the strong alkali aqueous solution of 8~10mol/L, 0.1mol/L methenamine is added,
It is put into 50~70 DEG C of baking ovens and reacts 4~6 hours, precipitating is obtained by filtration.
(2) by 20gL-1Precipitating ultrasonic disperse is to containing 2gL-1Copper chloride and 0.5gL-1In the aqueous solution of palladium chloride, and hold
Continuous stirring is until solvent is evaporated naturally；
(3) residue after being evaporated is put into 250 DEG C of Muffle furnaces and is calcined 4 hours, obtaining loading as shown in Figure 1 has Pd-
The zinc oxide of Cu.
Embodiment 2
(1) 0.5mol/L zinc acetate is added in the strong alkali aqueous solution of 8~10mol/L, 0.2mol/L methenamine is added,
It is put into 50~70 DEG C of baking ovens and reacts 4~6 hours, precipitating is obtained by filtration.
(2) by 16gL-1Precipitating ultrasonic disperse is to containing 2gL-1Copper chloride and 2gL-1In the aqueous solution of palladium chloride, and continue
Stirring is until solvent is evaporated naturally；
(3) residue after being evaporated is put into 200 DEG C of Muffle furnaces and is calcined 6 hours, obtain the oxidation that load has Pd-Cu
Zinc.
Embodiment 3
(1) 0.2mol/L zinc oxalate is added in the strong alkali aqueous solution of 8~10mol/L, 0.1mol/L methenamine is added,
It is put into 50~70 DEG C of baking ovens and reacts 4~6 hours, precipitating is obtained by filtration.
(2) by 16gL-1Precipitating ultrasonic disperse is to containing 1gL-1Copper chloride and 1gL-1In the aqueous solution of palladium chloride, and continue
Stirring is until solvent is evaporated naturally；
(3) residue after being evaporated is put into 300 DEG C of Muffle furnaces and is calcined 5 hours, obtain the oxidation that load has Pd-Cu
Zinc.
Embodiment 4
(1) 0.4mol/L zinc nitrate is added in the strong alkali aqueous solution of 8~10mol/L, 0.2mol/L methenamine is added,
It is put into 50~70 DEG C of baking ovens and reacts 4~6 hours, precipitating is obtained by filtration.
(2) by 12gL-1Precipitating ultrasonic disperse is to containing 2gL-1Copper chloride and 1gL-1In the aqueous solution of palladium chloride, and continue
Stirring is until solvent is evaporated naturally；
(3) residue after being evaporated is put into 300 DEG C of Muffle furnaces and is calcined 4 hours, obtain the oxidation that load has Pd-Cu
Zinc.
Claims (4)
1. a kind of zinc oxide synthetic method of Pd-Cu modification, which is characterized in that include the following steps：
(1) zinc salt is added in the strong alkali aqueous solution of 8~10mol/L, methenamine is added, is put into 50~70 DEG C of baking ovens and reacts
4~6 hours, precipitating is obtained by filtration.
(2) by precipitating ultrasonic disperse into the aqueous solution containing copper chloride and palladium chloride, and it is stirred continuously until that solvent steams naturally
It is dry；
(3) residue after being evaporated is put into 200~300 DEG C of Muffle furnaces and is calcined 4~6 hours, obtain the oxygen that load has Pd-Cu
Change zinc.
2. a kind of zinc oxide synthetic method of Pd-Cu modification according to claim 1, it is characterised in that：The zinc salt includes
One of zinc chloride, zinc acetate, zinc oxalate, zinc nitrate or combinations thereof, 0.1~0.5mol/L of concentration；Methenamine concentration 0.1
~0.2mol/L.
3. a kind of zinc oxide synthetic method of Pd-Cu modification according to claim 1, it is characterised in that：The aqueous solution
Middle palladium chloride concentration is 0.5~2gL-1, chlorination copper mass be 1~4 times of palladium chloride quality, dispersion precipitophore matter in aqueous solution
Amount is palladium chloride and 4~8 times of copper chloride gross mass.
4. Pd-Cu prepared by a kind of zinc oxide synthetic method of the Pd-Cu modification as described in claims 1 to 3 any one
The zinc oxide of modification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810749573.2A CN108906077A (en) | 2018-07-02 | 2018-07-02 | A kind of zinc oxide synthetic method of Pd-Cu modification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810749573.2A CN108906077A (en) | 2018-07-02 | 2018-07-02 | A kind of zinc oxide synthetic method of Pd-Cu modification |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108906077A true CN108906077A (en) | 2018-11-30 |
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ID=64412293
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810749573.2A Withdrawn CN108906077A (en) | 2018-07-02 | 2018-07-02 | A kind of zinc oxide synthetic method of Pd-Cu modification |
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| Country | Link |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103837517A (en) * | 2014-03-25 | 2014-06-04 | 哈尔滨工业大学 | Preparation method of metal film/zinc oxide (ZnO) nanorod array fluorescence enhancement material |
| CN104237464A (en) * | 2014-09-09 | 2014-12-24 | 上海纳米技术及应用国家工程研究中心有限公司 | Gas-sensitive sensing material with nano-zinc oxide supported palladium-copper porous structure and preparation method of gas-sensitive sensing material |
| CN106268801A (en) * | 2016-07-20 | 2017-01-04 | 方亚鹏 | High efficiency photocatalysis composite and preparation method thereof |
| CN106423154A (en) * | 2016-09-22 | 2017-02-22 | 华中科技大学 | 3D flexible electrode or 3D flexible catalyst as well as preparation method and application thereof |
-
2018
- 2018-07-02 CN CN201810749573.2A patent/CN108906077A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103837517A (en) * | 2014-03-25 | 2014-06-04 | 哈尔滨工业大学 | Preparation method of metal film/zinc oxide (ZnO) nanorod array fluorescence enhancement material |
| CN104237464A (en) * | 2014-09-09 | 2014-12-24 | 上海纳米技术及应用国家工程研究中心有限公司 | Gas-sensitive sensing material with nano-zinc oxide supported palladium-copper porous structure and preparation method of gas-sensitive sensing material |
| CN106268801A (en) * | 2016-07-20 | 2017-01-04 | 方亚鹏 | High efficiency photocatalysis composite and preparation method thereof |
| CN106423154A (en) * | 2016-09-22 | 2017-02-22 | 华中科技大学 | 3D flexible electrode or 3D flexible catalyst as well as preparation method and application thereof |
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| PB01 | Publication | ||
| PB01 | Publication | ||
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20181130 |
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| WW01 | Invention patent application withdrawn after publication |