CN113600183A - Preparation method and application of Pd-based catalyst - Google Patents
Preparation method and application of Pd-based catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title abstract description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 151
- 239000002105 nanoparticle Substances 0.000 claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 62
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 29
- 238000011068 loading method Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000003223 protective agent Substances 0.000 claims abstract description 7
- 238000009903 catalytic hydrogenation reaction Methods 0.000 claims abstract description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract 10
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract 5
- 229960005070 ascorbic acid Drugs 0.000 claims abstract 5
- 239000011668 ascorbic acid Substances 0.000 claims abstract 5
- 239000003638 chemical reducing agent Substances 0.000 claims abstract 4
- 239000003344 environmental pollutant Substances 0.000 claims abstract 2
- 231100000719 pollutant Toxicity 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 83
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 42
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 40
- 239000008367 deionised water Substances 0.000 claims description 37
- 229910021641 deionized water Inorganic materials 0.000 claims description 37
- 238000005406 washing Methods 0.000 claims description 36
- 238000006722 reduction reaction Methods 0.000 claims description 23
- 238000003760 magnetic stirring Methods 0.000 claims description 22
- 239000011734 sodium Substances 0.000 claims description 21
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 20
- 235000019253 formic acid Nutrition 0.000 claims description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000012696 Pd precursors Substances 0.000 claims 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims 2
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims 1
- STESGJHDBJZDRY-UHFFFAOYSA-N 1-hexadecyl-3-methyl-1,2-dihydroimidazol-1-ium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[NH+]1CN(C)C=C1 STESGJHDBJZDRY-UHFFFAOYSA-N 0.000 claims 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims 1
- DVBJBNKEBPCGSY-UHFFFAOYSA-M cetylpyridinium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+]1=CC=CC=C1 DVBJBNKEBPCGSY-UHFFFAOYSA-M 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000004132 cross linking Methods 0.000 claims 1
- 239000008103 glucose Substances 0.000 claims 1
- 231100000086 high toxicity Toxicity 0.000 claims 1
- 231100000053 low toxicity Toxicity 0.000 claims 1
- 239000002808 molecular sieve Substances 0.000 claims 1
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims 1
- 239000012279 sodium borohydride Substances 0.000 claims 1
- 229910000033 sodium borohydride Inorganic materials 0.000 claims 1
- ABKQFSYGIHQQLS-UHFFFAOYSA-J sodium tetrachloropalladate Chemical compound [Na+].[Na+].Cl[Pd+2](Cl)(Cl)Cl ABKQFSYGIHQQLS-UHFFFAOYSA-J 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 1
- 238000010531 catalytic reduction reaction Methods 0.000 abstract description 22
- 229910052763 palladium Inorganic materials 0.000 abstract description 13
- 229910003244 Na2PdCl4 Inorganic materials 0.000 abstract description 2
- 239000011651 chromium Substances 0.000 abstract 2
- 238000004523 catalytic cracking Methods 0.000 abstract 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 abstract 1
- 230000000593 degrading effect Effects 0.000 abstract 1
- 238000005984 hydrogenation reaction Methods 0.000 abstract 1
- 239000003208 petroleum Substances 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 140
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 42
- 239000007974 sodium acetate buffer Substances 0.000 description 20
- 238000005070 sampling Methods 0.000 description 19
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 19
- 230000003197 catalytic effect Effects 0.000 description 10
- 239000002086 nanomaterial Substances 0.000 description 10
- 239000000084 colloidal system Substances 0.000 description 9
- 229960004756 ethanol Drugs 0.000 description 9
- 235000019441 ethanol Nutrition 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000000527 sonication Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000005641 tunneling Effects 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of a catalyst containing Pd nano particles and a method for reducing Cr by catalytic hydrogenation of the catalyst in water6+The use of (1). The method uses Cetyl Trimethyl Ammonium Bromide (CTAB) as a protective agent and Na2PdCl4Preparing palladium nano-particles by using Ascorbic Acid (AA) as a reducing agent as a precursor under the condition of kinetic control, and loading the palladium nano-particles to Al calcined at 600 DEG C2O3On the carrier, the influence of different kinetic control preparation conditions, namely reaction temperature, time and CTAB dosage on the structure and morphology of the Pd nano-particles after loading is inspected. Then the catalyst is applied to catalytic reduction for degrading the pollutant Cr in water6+. The catalyst has relatively simple preparation process and strong catalytic hydrogenation performance, and can be applied to the catalytic reduction of hexavalent chromium and the hydrogenation of phenolReaction, automobile tail gas exhaust, catalytic cracking of petroleum and other aspects.
Description
Technical Field
The invention belongs to the field of catalytic materials, and particularly relates to a preparation method of a Pd-based catalyst and application of the Pd-based catalyst in catalytic hydrogenation reduction of Cr (VI) in water.
Background
The palladium nano material has quantum size effect, volume effect, surface effect, macroscopic quantum tunneling effect and the like
Basic characteristics, such as unique optical, electrical, catalytic properties, phase transition, particle transport and the like,
so that the palladium nano material can be used in automobile exhaust treatment, hydrogen storage material, fuel cell catalytic electrode and organic-inorganic catalysis
The Pd nano material has high catalytic activity, so the Pd nano material serving as the catalyst is widely applied to the fields of fuel cells, sensors, petroleum cracking, tail gas treatment and the like.
Since Pd metal is expensive and rare, it is important to reduce the amount of Pd by improving its catalytic performance. A great deal of research shows that the morphology of the Pd nano-material has great influence on the catalytic performance of the Pd nano-material, so that the preparation of the Pd nano-material with a specific morphology is one of the focuses in the field of Pd catalysis in the last decade.
The noble metal nanoparticles with specific morphology can well improve the catalytic performance of the noble metal nanoparticles, but the controllable synthesis of the morphology of the nanoparticles is influenced by many factors, such as pH value, temperature, solvent, concentration, pressure, quantity ratio of reactant substances, heating rate, cooling rate, reaction raw materials and the like, the experimental conditions are not easy to control, the experimental reproducibility is not high, and some problems still remain to be solved. How to reasonably control the growth of the nano material and further realize the regulation and control of the size, the dimensionality, the composition and the crystal structure of the nano material is a key point of the later research and has profound significance. In addition, the research on the application of the precious metal nano material is still a focus of the scientists, and the research and development of novel nano products which are easier to industrialize and meet the market demand are greatly concerned by research and development personnel, and new findings and inventions are believed to be continuously emerged.
Disclosure of Invention
The invention aims to regulate and control the appearance of the Pd-based catalyst by controlling certain conditions, such as the amount of a protective agent, reaction time, temperature, removal of redundant protective agent and the like, so as to improve the catalytic performance of the Pd-based catalyst and more efficiently catalyze and reduce Cr (VI).
In order to achieve the purpose, the invention adopts the following technical scheme.
Pd/Al2O3The preparation method comprises the following steps:
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and a certain amount of CTAB protective agent solution of 0.1mol/L are evenly mixed for 10min under magnetic stirring and preheated to the reaction temperature. Then adding 2.5mL of 0.1mol/L AA solution, after a certain time of reduction reaction, centrifuging the obtained solution (11000 rpm, 15 min), alternately washing the solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano-particles, ultrasonically dispersing the obtained nano-particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano-particles dispersed in the absolute ethyl alcohol into 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
Providing a preferred scheme:
the Pd/Al2O3(5wt%) catalyst preparation, CTAB 0.5ml, AA 2.5ml, at 60 ℃ reaction for 5min, it has better catalytic activity.
The invention has the beneficial effects that: the Pd-containing catalyst prepared by the invention has better catalytic reduction effect on Cr (VI) in water, and the method is simple and easy to operate and endows the catalyst with better catalytic performance.
Detailed Description
In order to explain the present invention in detail, some specific examples are given below, but the present invention is not limited to these examples.
Example 1
Preparing a solution: 0.1mol/L AA solution, 0.1mol/L CTAB solution, 0.01mol/L Na2PdCl4The solution, 0.1mg/ml potassium dichromate solution, 0.05mg/ml potassium dichromate solution, and acetic acid-sodium acetate buffer solution with pH of 3.60.
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml of 0.1mol/L CTAB solution were mixed homogeneously for 10min with magnetic stirring and preheated to 60 ℃. Then adding 2.5ml of 0.1mol/L AA solution, after 5min of reduction reaction, centrifuging the obtained solution (11000 rpm, 15 min), alternately washing with absolute ethyl alcohol and deionized water for three times to obtain Pd nano-particles, and drying the Pd nano-particles to obtain the Pd nano-particlesThe obtained nanoparticles were ultrasonically dispersed in 8mL of anhydrous ethanol, and then the Pd nanoparticles dispersed in the dehydrated ethanol were added to a solution containing 0.1g of Al2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 2
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml of 0.1mol/L CTAB solution were mixed homogeneously for 10min with magnetic stirring and preheated to 60 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after 5min of reduction reaction, centrifuging the obtained solution (11000 rpm, 15 min), alternately washing the obtained solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano particles, ultrasonically dispersing the obtained nano particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano particles dispersed in the absolute ethyl alcohol into 0.5312gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 1wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 3
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml of 0.1mol/L CTAB solution were mixed homogeneously for 10min with magnetic stirring and preheated to 60 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after 5min of reduction reaction, centrifuging the obtained solution (11000 rpm, 15 min), alternately washing the obtained solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano particles, ultrasonically dispersing the obtained nano particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano particles dispersed in the absolute ethyl alcohol into 0.2656gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 2wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 4
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml of 0.1mol/L CTAB solution were mixed homogeneously for 10min with magnetic stirring and preheated to 60 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after 5min of reduction reaction, centrifuging the obtained solution (11000 rpm, 15 min), alternately washing the obtained solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano particles, ultrasonically dispersing the obtained nano particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano particles dispersed in the absolute ethyl alcohol into 0.0759gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical load of 7wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Is arranged atStirring in a 50ml beaker in a 25 ℃ water bath for 30min, adding 2ml formic acid, sampling at different time periods, and analyzing the sample with an ultraviolet-visible spectrophotometer.
Example 5
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.25mL0.1mol/L CTAB solution were mixed homogeneously for 10min with magnetic stirring and preheated to 60 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after 1h and 30min of reduction reaction, centrifuging the obtained solution (11000 rpm and 15 min), alternately washing the solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano particles, ultrasonically dispersing the obtained nano particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano particles dispersed in the absolute ethyl alcohol into 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 6
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml0.1mol/L CTAB solution, under magnetic stirring uniformly mixed for 10min, and preheated to 60 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after 1h and 30min of reduction reaction, centrifuging the obtained solution (11000 rpm and 15 min), alternately washing the solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano particles, ultrasonically dispersing the obtained nano particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano particles dispersed in the absolute ethyl alcohol into 0.1gAl2O3The carrier was stirred in a 50ml beaker at room temperature for 15h, then washed with acetone three times and dried at 180 ℃For 3 hours, Pd/Al with the theoretical loading of 5wt percent is obtained2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 7
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 1mL0.1mol/L CTAB solution, under magnetic stirring uniform mixing for 10min, and preheating to 60 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after 1h and 30min of reduction reaction, centrifuging the obtained solution (11000 rpm and 15 min), alternately washing the solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano particles, ultrasonically dispersing the obtained nano particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano particles dispersed in the absolute ethyl alcohol into 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 8
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 1.5ml of 0.1mol/L CTAB solution were mixed homogeneously for 10min with magnetic stirring and preheated to 60 ℃. Then adding 2.5ml of 0.1mol/L AA solution, after reduction reaction for 1h30min, centrifuging the obtained solution (11000 rpm, 15 min), and separating with anhydrous ethanolWashing with water for three times alternately to obtain Pd nanoparticles, ultrasonically dispersing the obtained nanoparticles in 8mL of absolute ethyl alcohol, and adding the Pd nanoparticles dispersed in the absolute ethyl alcohol into the solution containing 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 9
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml0.1mol/L CTAB solution, under magnetic stirring uniformly mixed for 10min, and preheated to 40 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after 1h and 30min of reduction reaction, centrifuging the obtained solution (11000 rpm and 15 min), alternately washing the solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano particles, ultrasonically dispersing the obtained nano particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano particles dispersed in the absolute ethyl alcohol into 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 10
20mL of deionized water was addedIn a 100mL flask, 5mL of 0.01mol/L Na was added2PdC14The solution and 0.5ml0.1mol/L CTAB solution, under magnetic stirring uniformly mixed for 10min, and preheated to 50 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after 1h and 30min of reduction reaction, centrifuging the obtained solution (11000 rpm and 15 min), alternately washing the solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano particles, ultrasonically dispersing the obtained nano particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano particles dispersed in the absolute ethyl alcohol into 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 11
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml0.1mol/L CTAB solution, under magnetic stirring uniformly mixed for 10min, and preheated to 70 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after 1h and 30min of reduction reaction, centrifuging the obtained solution (11000 rpm and 15 min), alternately washing the solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano particles, ultrasonically dispersing the obtained nano particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano particles dispersed in the absolute ethyl alcohol into 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken and added with 10ml of sodium acetate buffer with pH value of 3.6Weighing 0.0080gPd/Al2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 12
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml0.1mol/L CTAB solution, under magnetic stirring uniformly mixed for 10min, and preheated to 60 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after 5min of reduction reaction, centrifuging the obtained solution (11000 rpm, 15 min), alternately washing the solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano-particles, ultrasonically dispersing the obtained nano-particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano-particles dispersed in the absolute ethyl alcohol into 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 13
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml0.1mol/L CTAB solution, under magnetic stirring uniformly mixed for 10min, and preheated to 60 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after 1h of reduction reaction, centrifuging the obtained solution (11000 rpm, 15 min), alternately washing the solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano-particles, ultrasonically dispersing the obtained nano-particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano-particles dispersed in the absolute ethyl alcohol into 0.1gAl2O3The carrier was stirred at room temperature for 15 hours in a 50ml beaker,then acetone is washed and separated for three times, and the mixture is dried for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical load of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 14
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml0.1mol/L CTAB solution, under magnetic stirring uniformly mixed for 10min, and preheated to 60 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after reduction reaction for 3h, centrifuging the obtained solution (11000 rpm, 15 min), alternately washing the solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano-particles, ultrasonically dispersing the obtained nano-particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano-particles dispersed in the absolute ethyl alcohol into 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 15
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml0.1mol/L CTAB solution, under magnetic stirring uniformly mixed for 10min, and preheated to 60 ℃. Then 2.5ml of 0.1mol/L AA solution is added, after 6 hours of reduction reaction, the obtained solution is centrifuged(11000 rpm, 15 min), washing the nano particles with absolute ethyl alcohol and deionized water alternately for three times to obtain Pd nano particles, ultrasonically dispersing the obtained nano particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano particles dispersed in the absolute ethyl alcohol into 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 16
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml0.1mol/L CTAB solution, under magnetic stirring uniformly mixed for 10min, and preheated to 60 ℃. Then adding 2.5mL of 0.1mol/L AA solution, after reduction reaction for 9h, centrifuging the obtained solution (11000 rpm, 15 min), alternately washing the solution with absolute ethyl alcohol and deionized water for three times to obtain Pd nano-particles, ultrasonically dispersing the obtained nano-particles in 8mL of absolute ethyl alcohol, and then adding the Pd nano-particles dispersed in the absolute ethyl alcohol into 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0080g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 17
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml0.1mol/L CTAB solution, under magnetic stirring uniformly mixed for 10min, and preheated to 60 ℃. Then 2.5ml of 0.1mol/L AA solution is added, and after reduction reaction for 5min, palladium colloid is obtained. Ethanol was added to the prepared palladium colloid in a volume ratio of 2 (ethanol) to 1 (colloid), and the mixture was stirred for about 2 hours. When the palladium nanoparticles started to precipitate, the stirring was stopped and the mixture was allowed to stand at room temperature overnight. The black precipitate was separated by centrifugation (11000 rpm, 15 minutes) and redispersed in ethanol by sonication for 20 min. Then adding Pd nano particles dispersed in dehydrated alcohol to the solution containing 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution with the concentration of 0.05mg/ml is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0060g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 18
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml0.1mol/L CTAB solution, under magnetic stirring uniformly mixed for 10min, and preheated to 60 ℃. Then 2.5ml of 0.1mol/L AA solution is added, and after reduction reaction for 5min, palladium colloid is obtained. Ethanol was added to the prepared palladium colloid in a volume ratio of 1 (ethanol): 1 (colloid), and the mixture was stirred for about 2 hours. When the palladium nanoparticles started to precipitate, the stirring was stopped and the mixture was allowed to stand at room temperature overnight. The black precipitate was separated by centrifugation (11000 rpm, 15 minutes) and redispersed in ethanol by sonication for 20 min. Then adding Pd nano particles dispersed in dehydrated alcohol to the solution containing 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution with the concentration of 0.05mg/ml is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0060g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Example 19
20mL of deionized water was taken in a 100mL flask, and 5mL of 0.01mol/L Na was added thereto2PdC14The solution and 0.5ml0.1mol/L CTAB solution, under magnetic stirring uniformly mixed for 10min, and preheated to 60 ℃. Then 2.5ml of 0.1mol/L AA solution is added, and after reduction reaction for 5min, palladium colloid is obtained. Ethanol was added to the prepared palladium colloid in a volume ratio of 4 (ethanol): 1 (colloid), and the mixture was stirred for about 2 hours. When the palladium nanoparticles started to precipitate, the stirring was stopped and the mixture was allowed to stand at room temperature overnight. The black precipitate was separated by centrifugation (11000 rpm, 15 minutes) and redispersed in ethanol by sonication for 20 min. Then adding Pd nano particles dispersed in dehydrated alcohol to the solution containing 0.1gAl2O3Stirring the carrier in a 50ml beaker for 15 hours at room temperature, washing and separating the carrier by acetone for three times, and drying the carrier for 3 hours at 180 ℃ to obtain Pd/Al with the theoretical loading of 5wt%2O3A catalyst.
The prepared Pd-based catalyst is used for the catalytic reduction of Cr (VI), 40ml of prepared potassium dichromate solution with the concentration of 0.05mg/ml is taken, 10ml of sodium acetate buffer solution with the pH value of 3.6 is added, and 0.0060g of Pd/Al is weighed2O3Stirring in a water bath at 25 deg.C for 30min in a 50ml beaker, adding 2ml formic acid, sampling at different time periods, and analyzing with an ultraviolet-visible spectrophotometer.
Claims (5)
1. One kind containsReduction of Cr by Pd catalyst catalytic hydrogenation6+The method for preparing (1), characterized in that:
under the condition of magnetic stirring, mixing the Pd precursor solution with a reducing agent, and carrying out high-temperature reaction in the presence of a protective agent to prepare a supported catalyst with a certain morphology, wherein the supported catalyst is applied to pollutants Cr in water6+Catalytic hydrogenation reduction of (3).
2. The method of claim 1, wherein:
the Pd precursor can be a Pd source such as chloropalladate, palladium acetate, sodium tetrachloropalladate and the like;
the reducing agent can be Ascorbic Acid (AA), sodium borohydride, glucose and the like;
the protective agent can be polyvinylpyrrolidone (PVP), Cetyl Trimethyl Ammonium Bromide (CTAB), cetyl pyridine bromide (HDPB), 1-hexadecyl-3-methylimidazole bromide (HMIB) or oleylamine and other compounds;
the carrier has Al2O3、TiO2Molecular sieves, P25And the like.
3. The method of claim 1, wherein:
the dosage of CTAB in the Pd catalyst is 0.25-1.5;
the reaction temperature T in the Pd catalyst is 40-70 ℃;
the reaction time t in the Pd catalyst is 5 min-9 h;
the load amount in the Pd catalyst is 1-7 wt%.
4. The method of claim 1, wherein:
the Pd-based catalyst is prepared by putting deionized water into a flask, and adding Na into the flask2PdC14Uniformly mixing the solution and a certain amount of CTAB protective agent solution under magnetic stirring for a period of time, preheating to reaction temperature, adding AA solution, carrying out reduction reaction for a period of time, centrifuging the obtained solution, and carrying out cross-linking on absolute ethyl alcohol and deionized waterAfter washing, obtaining Pd nano-particles, ultrasonically dispersing the obtained nano-particles in absolute ethyl alcohol, and then adding the Pd nano-particles dispersed in the absolute ethyl alcohol into Al2O3Stirring the carrier in a beaker at room temperature for a certain time, washing and separating the carrier by using acetone, and drying the carrier for 3 hours to obtain Pd/Al with the theoretical loading of 5wt percent2O3A catalyst.
5. The method of claim 1, wherein:
the Pd-based catalyst can efficiently catalyze and reduce Cr (VI) with high toxicity into Cr (III) with low toxicity by using a reducing agent formic acid.
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| CN106391000A (en) * | 2016-10-10 | 2017-02-15 | 中国科学院福建物质结构研究所 | Pd(111)/gamma-Al2O3 catalyst for CO dehydrogenation purification reaction and preparation method thereof |
| CN109248680A (en) * | 2018-09-28 | 2019-01-22 | 浙江理工大学 | Low-energy-consumption chemical field-driven organic pollutant degradation catalyst and application thereof |
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| CN106391000A (en) * | 2016-10-10 | 2017-02-15 | 中国科学院福建物质结构研究所 | Pd(111)/gamma-Al2O3 catalyst for CO dehydrogenation purification reaction and preparation method thereof |
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| CN115814789A (en) * | 2022-11-25 | 2023-03-21 | 安徽师范大学 | Coated Pd-based catalyst, preparation method thereof and method for treating hexavalent chromium in water body |
| CN115814789B (en) * | 2022-11-25 | 2024-03-29 | 安徽师范大学 | Coated Pd-based catalyst, preparation method thereof and method for treating hexavalent chromium in water body |
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