CN113181911A - Preparation method of noble metal platinum modified silicotungstic acid supported cerium dioxide catalyst - Google Patents
Preparation method of noble metal platinum modified silicotungstic acid supported cerium dioxide catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 43
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 title claims abstract description 27
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 23
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 22
- -1 platinum modified silicotungstic acid Chemical class 0.000 title claims description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 17
- 230000003647 oxidation Effects 0.000 claims abstract description 16
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 16
- CGFYHILWFSGVJS-UHFFFAOYSA-N silicic acid;trioxotungsten Chemical class O[Si](O)(O)O.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 CGFYHILWFSGVJS-UHFFFAOYSA-N 0.000 claims abstract description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 239000010970 precious metal Substances 0.000 claims abstract 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- MUMZUERVLWJKNR-UHFFFAOYSA-N oxoplatinum Chemical compound [Pt]=O MUMZUERVLWJKNR-UHFFFAOYSA-N 0.000 claims description 7
- 229910003446 platinum oxide Inorganic materials 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 4
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 abstract description 40
- 230000003197 catalytic effect Effects 0.000 abstract description 18
- 238000012216 screening Methods 0.000 abstract description 2
- 239000012693 ceria precursor Substances 0.000 abstract 2
- 239000002245 particle Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 10
- 238000001914 filtration Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000011964 heteropoly acid Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000007084 catalytic combustion reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 125000006414 CCl Chemical group ClC* 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910002621 H2PtCl6 Inorganic materials 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- RCJVRSBWZCNNQT-UHFFFAOYSA-N dichloridooxygen Chemical compound ClOCl RCJVRSBWZCNNQT-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 231100000171 higher toxicity Toxicity 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 231100000683 possible toxicity Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J23/6527—Tungsten
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- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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Abstract
一种贵金属铂改性硅钨酸负载二氧化铈催化剂制备方法，涉及一种贵金属铂改性硅钨酸负载二氧化铈催化剂制备方法，该制备方法为以下步骤：步骤一，将适量的醋酸铈、适量的尿素、一定量的硅钨酸、不同质量分数的氯铂酸溶液充分溶解在溶剂中，得到贵金属铂改性硅钨酸负载二氧化铈前体溶液；步骤二，将贵金属铂改性硅钨酸负载二氧化铈前体溶液置于水热反应釜中，经水热反应后得到产物；步骤三，将产物烘干后进行高温煅烧，通过筛选最终得到粒径为40‑60目的贵金属铂改性硅钨酸负载二氧化铈催化剂。本发明用于催化氧化氯苯，具有催化活性高、制备过程简单等优点，为工业化应用提供新思路。A preparation method of a noble metal platinum-modified silicotungstic acid supported ceria catalyst relates to a preparation method of a noble metal platinum-modified silicotungstic acid supported ceria catalyst. The preparation method comprises the following steps: Step 1, adding an appropriate amount of cerium acetate , an appropriate amount of urea, a certain amount of silicotungstic acid, and chloroplatinic acid solutions of different mass fractions are fully dissolved in the solvent to obtain a precious metal platinum-modified silicotungstic acid-supported ceria precursor solution; step 2, the precious metal platinum is modified The silicotungstic acid-supported ceria precursor solution is placed in a hydrothermal reaction kettle, and a product is obtained after hydrothermal reaction; step 3, the product is dried and then calcined at high temperature, and the precious metal with a particle size of 40-60 mesh is finally obtained through screening Platinum-modified silicotungstic acid supported ceria catalyst. The invention is used for catalytic oxidation of chlorobenzene, has the advantages of high catalytic activity, simple preparation process and the like, and provides a new idea for industrial application.
Description
Technical Field
The invention relates to a preparation method of a catalyst, in particular to a preparation method of a noble metal platinum modified silicotungstic acid loaded cerium dioxide catalyst.
Background
In industrial production, halogenated organic volatile matters frequently emitted by industries such as medicine, pesticide, light industry, packaging industry and the like are in wide concern due to the durability and potential toxicity of the halogenated organic volatile matters in the environment. In which the chlorinated radicals have a higher toxicity
Volatile Organic Compounds (CVOCs) not only destroy the atmosphere, but also have a persistent and cumulative impact on human health and ecosystem. Chlorobenzene has been a chlorinated organic volatile gas of great interest to researchers due to its properties of being difficult to degrade and toxic.
With the development of science and technology, various methods are adopted at home and abroad to treat chlorobenzene pollution, such as biodegradation, absorption/adsorption, membrane separation technology, photocatalysis, ozone oxidation, thermal combustion, catalytic combustion and the like; of these technologies, catalytic combustion is a promising treatment because it reduces the temperature and energy consumption during oxidation and converts chlorobenzene to H2O, HCl, CO2, etc. end products at lower temperatures, and thus is considered an environmentally friendly, green, efficient chlorobenzene treatment. At present, the key research of catalytic oxidation of chlorobenzene at home and abroad mainly focuses on screening and optimizing catalytic materials. The noble metal has obvious effect of improving the performance of catalytic oxidation of chlorobenzene. CeO2 is modified by heteropoly acid, so that the heteropoly acid has good oxidation-reduction capability and more surface acid sites. In the process of catalytic oxidation of chlorobenzene, CeO2 is modified by heteropoly acid, so that the catalytic activity and stability of the CeO2 catalyst in the catalytic oxidation of chlorobenzene are improved. More surface acidity can dissociate C-Cl of chlorobenzene, and stronger redox ability can continuously crack benzene rings and further deeply oxidize the benzene rings into short-chain intermediate products, so that the chlorobenzene is subjected to harmless treatment.
Disclosure of Invention
The invention aims to provide a preparation method of a noble metal platinum modified silicotungstic acid supported cerium dioxide catalyst, the oxidation-reduction performance and the surface acidity of the noble metal platinum modified silicotungstic acid supported cerium dioxide catalyst are obviously improved compared with those of the silicotungstic acid modified cerium dioxide catalyst, and the catalytic oxidation of chlorobenzene is proved to have excellent catalytic performance by an activity test, and the preparation method is simple and economic and has great significance in industrial application.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a noble metal platinum modified silicotungstic acid loaded cerium dioxide catalyst comprises the following preparation processes:
1) putting 8-10 mmol of cerium acetate and 15-30 mmol of urea in 25-50 mL of solvent, adding 0.08-0.14 mmol of silicotungstic acid and 7.7mmol/L of chloroplatinic acid solution after full dissolution, and stirring for 0.5-2 hours;
2) placing the obtained solution in a hydrothermal reaction kettle, and keeping the hydrothermal temperature of 80-170 ℃ for 6-42 hours;
3) washing and filtering a product obtained through the hydrothermal reaction, and moving the product into a drying oven with the temperature of 50-100 ℃ for 12-48 hours;
4) and (3) transferring the dried solid to a muffle furnace, firstly heating to 250-350 ℃ from room temperature through a program of 1-5 ℃ per minute, keeping the temperature for 1-2 hours, then heating to 500-700 ℃ through a program of 1-5 ℃ per minute, and keeping the temperature for 2-4 hours.
According to the preparation method of the noble metal platinum modified silicotungstic acid supported cerium dioxide catalyst, the solvent used in the step 1) is water, glycol, ethanol and methanol.
In the preparation method of the noble metal platinum modified silicotungstic acid supported cerium dioxide catalyst, the chloroplatinic acid solution in the step 1) is prepared by respectively adding 4mL of H with the concentration of 7.7mmol/L2PtCl6·6H2O, the mass fraction of the platinum oxide after roasting accounts for 0.5 percent of the catalyst; 8mL of H with a concentration of 7.7mmol/L was added2PtCl6·6H2O, the mass fraction of the platinum oxide after roasting accounts for 1 percent of the catalyst; 12mL of H with a concentration of 7.7mmol/L was added2PtCl6·6H2O, the mass fraction of the platinum oxide after roasting accounts for 1.5 percent of the catalyst; add 16mL of concentrateDegree of 7.7 mmol/L2% H2PtCl6·6H2And O, wherein the mass fraction of the platinum oxide after roasting accounts for 2 percent of the catalyst.
According to the preparation method of the noble metal platinum modified silicotungstic acid supported cerium dioxide catalyst, the hydrothermal temperature in the step 2) is 80-170 ℃, and the hydrothermal time is 6-42 hours.
According to the preparation method of the noble metal platinum modified silicotungstic acid supported cerium dioxide catalyst, the dried solid is calcined in the following two stages:
(1) the temperature is programmed to be increased from room temperature to 250-350 ℃ at 1-5 ℃ per min, and the temperature is kept for 1-2 hours;
(2) and (4) continuing programming at 1-5 ℃ per min until the temperature reaches 500-700 ℃, and keeping the temperature for 2-4 hours.
The preparation method of the noble metal platinum modified silicotungstic acid supported cerium dioxide catalyst comprises the step of preparing the catalyst with the specific surface area of 30.023-95.475 m2The pore diameter is 1.67-8.35 nm.
The invention has the advantages and effects that:
1. the heteropoly acid HSiW is used for the reaction of CeO2The modification can simultaneously improve the oxidation performance, the surface acidity and the catalytic activity and the stability in the catalytic oxidation of chlorobenzene.
2. The catalyst of the invention has low preparation cost and simple and convenient preparation method, and is suitable for large-scale production and utilization.
3. The high stability and excellent anti-carbon deposition capability of the catalyst show that the catalyst has the ideal effect of preventing chlorine adsorption from forming oxychloride on the surface and poisoning and degrading chlorobenzene pollution in the process of continuously catalyzing chlorobenzene for a long time.
4. The catalytic performance of the catalyst is further improved after the catalyst is doped with noble metal.
Drawings
FIG. 1 is an X-ray diffraction pattern (XRD) of silicotungstic acid modified ceria loaded with different mass fractions of platinum in the examples according to the invention;
FIG. 2 shows the conversion of a silicotungstic acid modified ceria catalyst loaded with different mass fractions of platinum for catalytic oxidation of chlorobenzene in the examples of the present invention.
Detailed Description
The present invention will be described in detail with reference to the embodiments shown in the drawings.
Example one
A preparation method of a noble metal platinum modified silicotungstic acid loaded cerium dioxide catalyst for catalytic oxidation of chlorobenzene comprises the following steps:
1) completely dissolving 8mmol of cerium acetate and 15mmol of urea in 25mL of ethylene glycol, and then adding 0.08mmol of silicotungstic acid and 4mL of H with the concentration of 7.7mmol/L2PtCl6·6H2O, and stirring for 1 hour;
2) placing the obtained solution in a hydrothermal reaction kettle, keeping the hydrothermal temperature of 180 ℃, and carrying out hydrothermal reaction for 12 hours;
3) washing and filtering a product obtained through the hydrothermal reaction, and moving the product into a drying oven with the temperature of 105 ℃ for 12 hours;
4) and transferring the dried solid to a muffle furnace, firstly raising the temperature from room temperature to 350 ℃ through a 2 ℃ C/min program, keeping the temperature for 2 hours, and then raising the temperature to 550 ℃ through a 2 ℃ C/min program, and keeping the temperature for 3 hours.
Example two
A preparation method of a noble metal platinum modified silicotungstic acid loaded cerium dioxide catalyst for catalytic oxidation of chlorobenzene comprises the following steps:
1) completely dissolving 8mmol of cerium acetate and 15mmol of urea in 25mL of ethylene glycol, and then adding 0.08mmol of silicotungstic acid and 8mL of H with the concentration of 7.7mmol/L2PtCl6·6H2O, and stirring for 1 hour;
2) placing the obtained solution in a hydrothermal reaction kettle, keeping the hydrothermal temperature of 180 ℃, and carrying out hydrothermal reaction for 12 hours;
3) washing and filtering a product obtained through the hydrothermal reaction, and moving the product into a drying oven with the temperature of 105 ℃ for 12 hours;
4) and transferring the dried solid to a muffle furnace, firstly raising the temperature from room temperature to 350 ℃ through a 2 ℃ C/min program, keeping the temperature for 2 hours, and then raising the temperature to 550 ℃ through a 2 ℃ C/min program, and keeping the temperature for 3 hours.
EXAMPLE III
A preparation method of a noble metal platinum modified silicotungstic acid loaded cerium dioxide catalyst for catalytic oxidation of chlorobenzene comprises the following steps:
1) completely dissolving 8mmol of cerium acetate and 15mmol of urea in 25mL of ethylene glycol, and then adding 0.08mmol of silicotungstic acid and 12mL of H with the concentration of 7.7mmol/L2PtCl6·6H2O, and stirring for 1 hour;
2) placing the obtained solution in a hydrothermal reaction kettle, keeping the hydrothermal temperature of 180 ℃ and carrying out hydrothermal reaction for 12 hours;
3) washing and filtering a product obtained through the hydrothermal reaction, and moving the product into a drying oven with the temperature of 105 ℃ for 12 hours;
4) and transferring the dried solid to a muffle furnace, firstly raising the temperature from room temperature to 350 ℃ through a 2 ℃ C/min program, keeping the temperature for 2 hours, and then raising the temperature to 550 ℃ through a 2 ℃ C/min program, and keeping the temperature for 3 hours.
Example four
A preparation method of a noble metal platinum modified silicotungstic acid loaded cerium dioxide catalyst for catalytic oxidation of chlorobenzene comprises the following steps:
1) completely dissolving 8mmol of cerium acetate and 15mmol of urea in 25mL of ethylene glycol, and then adding 0.08mmol of silicotungstic acid and 16mL of H with the concentration of 7.7mmol/L2PtCl6·6H2O, and stirring for 1 hour;
2) placing the obtained solution in a hydrothermal reaction kettle, keeping the hydrothermal temperature of 180 ℃ and carrying out hydrothermal reaction for 12 hours;
3) washing and filtering a product obtained through the hydrothermal reaction, and moving the product into a drying oven with the temperature of 105 ℃ for 12 hours;
4) and transferring the dried solid to a muffle furnace, firstly raising the temperature from room temperature to 350 ℃ through a 2 ℃ C/min program, keeping the temperature for 2 hours, and then raising the temperature to 550 ℃ through a 2 ℃ C/min program, and keeping the temperature for 3 hours.
The preferred embodiments of the present invention are shown above, but the embodiments are not limited to the examples, and the protection scope of the present invention includes: various modifications, changes, combinations, substitutions, etc. can be made in the embodiments without departing from the spirit and scope of the claims.
Claims (6)
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