CN108607547B - Preparation method of nano platinum oxide catalyst - Google Patents
Preparation method of nano platinum oxide catalyst Download PDFInfo
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- CN108607547B CN108607547B CN201810598111.5A CN201810598111A CN108607547B CN 108607547 B CN108607547 B CN 108607547B CN 201810598111 A CN201810598111 A CN 201810598111A CN 108607547 B CN108607547 B CN 108607547B
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- MUMZUERVLWJKNR-UHFFFAOYSA-N oxoplatinum Chemical compound [Pt]=O MUMZUERVLWJKNR-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910003446 platinum oxide Inorganic materials 0.000 title claims abstract description 38
- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- NFOHLBHARAZXFQ-UHFFFAOYSA-L platinum(2+);dihydroxide Chemical compound O[Pt]O NFOHLBHARAZXFQ-UHFFFAOYSA-L 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 34
- 238000005406 washing Methods 0.000 claims abstract description 28
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims abstract description 26
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims abstract description 26
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003513 alkali Substances 0.000 claims abstract description 18
- 239000012153 distilled water Substances 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000002244 precipitate Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 15
- 238000004821 distillation Methods 0.000 claims abstract description 13
- 239000003292 glue Substances 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000002245 particle Substances 0.000 abstract description 16
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 229910000510 noble metal Inorganic materials 0.000 description 9
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 150000004706 metal oxides Chemical class 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001248 thermal gelation Methods 0.000 description 2
- 239000002341 toxic gas Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- 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
- B01J23/42—Platinum
-
- 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
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/004—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/02—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation
- C07C5/08—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of carbon-to-carbon triple bonds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/02—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation
- C07C5/08—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of carbon-to-carbon triple bonds
- C07C5/09—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of carbon-to-carbon triple bonds to carbon-to-carbon double bonds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
- C07C2523/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals
- C07C2523/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals of the platinum group metals
- C07C2523/42—Platinum
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The invention belongs to the field of catalysis, and particularly relates to a preparation method of a nano platinum oxide catalyst, which comprises the following steps: step 1, adding chloroplatinic acid into an alkali solution, filtering, washing and drying to obtain a white platinum hydroxide precipitate; step 2, adding the white platinum hydroxide precipitate into distilled water, stirring, adding the high-substituted hydroxypropyl cellulose, and uniformly stirring at a low temperature to obtain a suspension; step 3, putting the suspension into a reaction kettle, slowly heating, stirring and reacting for 2-5 hours, standing for 1-2 hours at constant temperature, and filtering to obtain gel; step 4, putting the gel into reduced pressure distilled water for reduced pressure distillation reaction for 1-3h to obtain mixed dry glue; and 5, putting the dry glue into absolute ethyl alcohol, ultrasonically washing for 20-40min, filtering, and drying to obtain the nano platinum oxide catalyst. The invention solves the problem of larger particle size distribution of the existing platinum oxide process, can form nano platinum oxide by utilizing the dispersibility and the coating property of the high-substituted hydroxypropyl cellulose, and has strong particle size controllability.
Description
Technical Field
The invention belongs to the field of catalysis, and particularly relates to a preparation method of a nano platinum oxide catalyst.
Background
The noble metal oxide catalyst has extremely important position in the fields of petroleum, chemical industry, medicine, pesticide, energy and the like because of no replaceable catalytic performance and selectivity. Particularly, in recent years, the national economy is rapidly developed, the highway network is comprehensively constructed, the living standard is greatly improved, automobiles are gradually integrated into the daily life of people, the automobiles bring rapidness and convenience to the society, and meanwhile, a series of social problems are brought, for example, the emission of automobile exhaust causes serious pollution to the environment, the national economy development is restricted to a certain extent, and the harm to the health of the public becomes an important factor influencing the stability and harmony of the society. Under the new situation that environmental problems are increasingly prominent and people pay more attention to environmental protection, the problem of automobile exhaust emission is more and more attracting social attention, so that the noble metal oxide is adopted as a catalyst to purify the automobile exhaust, reduce the emission of toxic gases, protect the health of people and promote the social harmony development, which is very important. Platinum oxide, a typical noble metal oxide catalyst, has excellent catalytic performance, can reduce toxic gases in automobile exhaust emission to a great extent, draws increasing attention, and becomes an indispensable material in automobile exhaust treatment accessories. The traditional platinum oxide is one of the main materials of the catalyst, and because the particles are large, the distribution specific surface area of the equivalent platinum oxide in the catalyst is smaller, the contact area with gas is relatively small, and the phenomenon of waste exists. The nano platinum oxide has larger specific surface area energy and higher catalytic activity because the size is in the nano level, so that the preparation of the nano platinum oxide can better reduce the catalyst cost and save more precious metal resources for the country.
Platinum oxide particles prepared by the traditional method are formed at high temperature in the sintering process, atoms among different platinum particles are easy to diffuse, so platinum oxide in a catalyst carrier coating prepared by the method has larger particle diameter due to mutual bonding, which is about hundreds of nanometers to tens of micrometers, and can be sintered with other noble metal elements (such as rhodium) to form a larger alloy body, so that the formed noble metal alloy has relatively weaker catalytic activity, and meanwhile, the alloy and the noble metal oxide have relatively smaller specific surface area due to larger particles, so that noble metal at the core part of the particles cannot be in direct contact with tail gas components, the effective and full utilization of the noble metal is reduced, and the waste of the noble metal in use is caused.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a nano platinum oxide catalyst, which solves the problem of large particle size distribution in the existing platinum oxide process, can form nano platinum oxide by utilizing the dispersibility and the coating property of high-substituted hydroxypropyl cellulose, and has strong particle size controllability.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of a nano platinum oxide catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding chloroplatinic acid into an alkali solution, filtering, washing and drying to obtain a white platinum hydroxide precipitate;
step 2, adding the white platinum hydroxide precipitate into distilled water, stirring, adding the high-substituted hydroxypropyl cellulose, and uniformly stirring at a low temperature to obtain a suspension;
step 3, putting the suspension into a reaction kettle, slowly heating, stirring and reacting for 2-5 hours, standing for 1-2 hours at constant temperature, and filtering to obtain gel;
step 4, putting the gel into reduced pressure distilled water for reduced pressure distillation reaction for 1-3h to obtain mixed dry glue;
and 5, putting the dry glue into absolute ethyl alcohol, ultrasonically washing for 20-40min, filtering, and drying to obtain the nano platinum oxide catalyst.
Washing in the step 1 by using absolute ethyl alcohol, drying at 40-60 ℃, wherein the alkali liquor is potassium hydroxide or sodium hydroxide, and the concentration of the alkali liquor is 0.3-0.7 mol/L; step 1, adding chloroplatinic acid into an alkali solution, and reacting with chloroplatinic acid by using hydroxide radical of alkali to obtain platinum hydroxide precipitate; because the platinum hydroxide is insoluble in water, precipitate is formed and filtered to obtain white precipitate, and the white precipitate is dried at low temperature to form platinum hydroxide precipitate and ensure that the platinum hydroxide is not decomposed.
The adding amount of the high-substituted hydroxypropyl cellulose in the step 2 is 40-70% of the mass of the platinum hydroxide, the concentration of the platinum hydroxide in distilled water is 20-50g/L, and the low-temperature stirring temperature is 20-30 ℃; adding the white platinum hydroxide precipitate into distilled water, uniformly stirring, adding the high-substituted hydroxypropyl cellulose, and uniformly stirring to form a dispersion system to obtain a suspension; the high-substituted hydroxypropyl cellulose has good dispersibility, and can directly act on the surface of the platinum hydroxide to form a good suspension dispersion system; the low-temperature stirring mode can ensure that the high-substituted hydroxypropyl cellulose does not form solidification.
The maximum temperature of the slow heating and stirring in the step 3 is 80-90 ℃, the heating speed is 2-3 ℃/min, and the temperature of constant-temperature standing is 90-95 ℃; the method comprises the steps of heating and stirring turbid liquid in a slow heating mode, gradually forming gel by highly-substituted hydroxypropyl cellulose in the stirring process, directly coating platinum hydroxide by the gel to form a wrapping structure, continuously and uniformly dispersing the gel in the stirring process, continuously accumulating the gel along with the rise of the temperature, continuously improving the gel immobilization phenomenon, standing at a constant temperature to obtain solidified gel, and uniformly dispersing platinum hydroxide particles in the gel.
The pressure of the reduced pressure distillation in the step 4 is 50-60% of the atmospheric pressure, and the temperature is 100-120 ℃; and (3) putting the gel into a reduced pressure distillation kettle, removing water molecules in the gel in a reduced pressure distillation reaction mode to form dry gel, and shrinking the gel to form a porous structure.
The concentration of the dry glue in the absolute ethyl alcohol in the step 5 is 100-150g/L, the temperature of ultrasonic washing is 30-60 ℃, the frequency is 40-60kHz, and the drying temperature is 70-90 ℃; adding the dry glue into absolute ethyl alcohol, and gradually dissolving the high-substituted hydroxypropyl cellulose in the absolute ethyl alcohol by adopting an ultrasonic washing mode to form a dispersion system to act on the surface of the platinum hydroxide; the clutch energy of ultrasonic washing can play a large amount of heat to convert the platinum hydroxide into platinum oxide, and a good dispersion suspension effect is formed under the dispersion action, and the nano platinum oxide forms ultrasonic passivation in the ultrasonic washing process, so that the problem of agglomeration of nano materials is solved.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of larger particle size distribution of the existing platinum oxide process, can form nano platinum oxide by utilizing the dispersibility and the coating property of the high-substituted hydroxypropyl cellulose, and has strong particle size controllability.
2. The invention fully utilizes the coating property of the high-substituted hydroxypropyl cellulose to disperse the platinum hydroxide in a solid state, and utilizes the characteristics of solubility and thermal gelation property of the high-substituted hydroxypropyl cellulose to form physical conversion reaction, thereby reducing the reaction and the pollution of the whole system, and simultaneously the high-substituted hydroxypropyl cellulose does not react and can be completely recycled.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
A preparation method of a nano platinum oxide catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding chloroplatinic acid into an alkali solution, filtering, washing and drying to obtain a white platinum hydroxide precipitate, wherein the washing in the step 1 adopts absolute ethyl alcohol for washing, the drying adopts drying at 40 ℃, the alkali solution adopts potassium hydroxide, and the concentration of the alkali solution is 0.3 mol/L;
step 2, adding the white platinum hydroxide precipitate into distilled water, stirring, adding the high-substituted hydroxypropyl cellulose, and uniformly stirring at a low temperature to obtain a suspension, wherein the addition amount of the high-substituted hydroxypropyl cellulose is 40% of the mass of the platinum hydroxide, the concentration of the platinum hydroxide in the distilled water is 20g/L, and the low-temperature stirring temperature is 20 ℃;
step 3, placing the suspension into a reaction kettle, slowly heating, stirring and reacting for 2 hours, standing at constant temperature for 1 hour, and filtering to obtain gel, wherein the highest temperature of the slow heating and stirring is 80 ℃, the heating speed is 2 ℃/min, and the temperature of the constant-temperature standing is 90 ℃;
step 4, putting the gel into reduced pressure distilled water for reduced pressure distillation reaction for 1 hour to obtain mixed dry glue, wherein the pressure of the reduced pressure distillation is 50% of the atmospheric pressure, and the temperature is 100 ℃;
and 5, putting the dry adhesive into absolute ethyl alcohol, ultrasonically washing for 20min, filtering, and drying to obtain the nano platinum oxide catalyst, wherein the concentration of the dry adhesive in the absolute ethyl alcohol is 100g/L, the ultrasonic washing temperature is 30 ℃, the frequency is 40kHz, and the drying temperature is 70 ℃.
Example 2
A preparation method of a nano platinum oxide catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding chloroplatinic acid into an alkali solution, filtering, washing and drying to obtain a white platinum hydroxide precipitate, wherein the washing in the step 1 adopts absolute ethyl alcohol for washing, the drying adopts drying at 60 ℃, the alkali solution adopts sodium hydroxide, and the concentration of the alkali solution is 0.7 mol/L;
step 2, adding the white platinum hydroxide precipitate into distilled water, stirring, adding high-substituted hydroxypropyl cellulose, and uniformly stirring at a low temperature to obtain a suspension, wherein the addition amount of the high-substituted hydroxypropyl cellulose is 70% of the mass of the platinum hydroxide, the concentration of the platinum hydroxide in the distilled water is 50g/L, and the low-temperature stirring temperature is 30 ℃;
step 3, placing the suspension into a reaction kettle, slowly heating, stirring and reacting for 5 hours, standing at a constant temperature for 2 hours, and filtering to obtain gel, wherein the highest temperature of the slow heating and stirring is 90 ℃, the heating speed is 3 ℃/min, and the temperature of the constant-temperature standing is 95 ℃;
step 4, putting the gel into reduced pressure distilled water for reduced pressure distillation reaction for 3 hours to obtain mixed dry glue, wherein the pressure of the reduced pressure distillation is 50-60% of the atmospheric pressure, and the temperature is 120 ℃;
and 5, putting the dry adhesive into absolute ethyl alcohol, ultrasonically washing for 40min, filtering, and drying to obtain the nano platinum oxide catalyst, wherein the concentration of the dry adhesive in the absolute ethyl alcohol is 150g/L, the ultrasonic washing temperature is 60 ℃, the frequency is 60kHz, and the drying temperature is 90 ℃.
Example 3
A preparation method of a nano platinum oxide catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding chloroplatinic acid into an alkali solution, filtering, washing and drying to obtain a white platinum hydroxide precipitate, wherein the washing in the step 1 adopts absolute ethyl alcohol for washing, the drying adopts drying at 50 ℃, the alkali solution adopts potassium hydroxide, and the concentration of the alkali solution is 0.5 mol/L;
step 2, adding the white platinum hydroxide precipitate into distilled water, stirring, adding the high-substituted hydroxypropyl cellulose, and uniformly stirring at a low temperature to obtain a suspension, wherein the addition amount of the high-substituted hydroxypropyl cellulose is 60% of the mass of the platinum hydroxide, the concentration of the platinum hydroxide in the distilled water is 40g/L, and the low-temperature stirring temperature is 25 ℃;
step 3, placing the suspension into a reaction kettle, slowly heating and stirring for reaction for 4 hours, standing at a constant temperature for 2 hours, and filtering to obtain gel, wherein the highest temperature of the slow heating and stirring is 85 ℃, the heating speed is 3 ℃/min, and the temperature of the constant-temperature standing is 93 ℃;
step 4, putting the gel into reduced pressure distilled water for reduced pressure distillation reaction for 2 hours to obtain mixed dry glue, wherein the pressure of the reduced pressure distillation is 55% of the atmospheric pressure, and the temperature is 110 ℃;
and 5, putting the dry adhesive into absolute ethyl alcohol, ultrasonically washing for 30min, filtering, and drying to obtain the nano platinum oxide catalyst, wherein the concentration of the dry adhesive in the absolute ethyl alcohol is 130g/L, the ultrasonic washing temperature is 50 ℃, the frequency is 50kHz, and the drying temperature is 80 ℃.
Performance detection
| Example 1 | Example 2 | Example 3 | Comparative example | |
| Yield of | 98.92％ | 99.11％ | 95.29％ | 95.32％ |
| Particle size | 80-90nm | 75-85nm | 45-50nm | 200-400nm |
| Catalytic performance | 84.3％ | 84.9％ | 86.1％ | 65.9％ |
The comparative example used commercially available nano platinum oxide.
Catalytic performance testing the acetylene catalytic hydrogenation reaction according to routine experiments.
In summary, the invention has the following advantages:
1. the invention solves the problem of larger particle size distribution of the existing platinum oxide process, can form nano platinum oxide by utilizing the dispersibility and the coating property of the high-substituted hydroxypropyl cellulose, and has strong particle size controllability.
2. The invention fully utilizes the coating property of the high-substituted hydroxypropyl cellulose to disperse the platinum hydroxide in a solid state, and utilizes the characteristics of solubility and thermal gelation property of the high-substituted hydroxypropyl cellulose to form physical conversion reaction, thereby reducing the reaction and the pollution of the whole system, and simultaneously the high-substituted hydroxypropyl cellulose does not react and can be completely recycled.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (6)
1. A preparation method of a nano platinum oxide catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding chloroplatinic acid into an alkali solution, filtering, washing and drying to obtain a white platinum hydroxide precipitate;
step 2, adding the white platinum hydroxide precipitate into distilled water, stirring, adding the high-substituted hydroxypropyl cellulose, and uniformly stirring at a low temperature to obtain a suspension; the concentration of the platinum hydroxide in the distilled water is 20-50g/L, and the low-temperature stirring temperature is 20-30 ℃;
step 3, putting the suspension into a reaction kettle, slowly heating, stirring and reacting for 2-5 hours, standing for 1-2 hours at constant temperature, and filtering to obtain gel; the highest temperature of the slow heating and stirring is 80-90 ℃, and the heating speed is 2-3 ℃/min; standing at constant temperature of 90-95 deg.C;
step 4, putting the gel into reduced pressure distilled water for reduced pressure distillation reaction for 1-3h to obtain mixed dry glue;
and 5, putting the dry glue into absolute ethyl alcohol, ultrasonically washing for 20-40min, filtering, and drying to obtain the nano platinum oxide catalyst.
2. The method for preparing a nano platinum oxide catalyst according to claim 1, wherein: washing in the step 1 is carried out by adopting absolute ethyl alcohol, and drying is carried out at 40-60 ℃.
3. The method for preparing a nano platinum oxide catalyst according to claim 1, wherein: the alkali liquor in the step 1 is potassium hydroxide or sodium hydroxide, and the concentration of the alkali liquor is 0.3-0.7 mol/L.
4. The method for preparing a nano platinum oxide catalyst according to claim 1, wherein: the adding amount of the high-substituted hydroxypropyl cellulose in the step 2 is 40-70% of the mass of the platinum hydroxide.
5. The method for preparing a nano platinum oxide catalyst according to claim 1, wherein: the pressure of the reduced pressure distillation in the step 4 is 50-60% of the atmospheric pressure, and the temperature is 100-120 ℃.
6. The method for preparing a nano platinum oxide catalyst according to claim 1, wherein: the concentration of the dry glue in the absolute ethyl alcohol in the step 5 is 100-150g/L, the temperature of ultrasonic washing is 30-60 ℃, the frequency is 40-60kHz, and the drying temperature is 70-90 ℃.
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| CN112871156B (en) * | 2021-01-20 | 2023-03-24 | 陕西瑞科新材料股份有限公司 | Preparation method of platinum oxide catalyst based on porous zirconia |
| CN114163835B (en) * | 2021-12-16 | 2024-01-26 | 江苏盛吉化工有限公司 | Preparation method of acid black 172 dye |
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|---|---|---|---|---|
| CN103623874A (en) * | 2012-08-27 | 2014-03-12 | 中国石油化工股份有限公司 | Preparation method of C2 selective hydrogenation catalyst |
| CN106669662A (en) * | 2017-01-21 | 2017-05-17 | 杨林 | Preparation method of platinum nano catalyst |
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