CN109201047A - Prepare the method that the micro-nano array of titanium oxide supports monatomic platinum catalyst - Google Patents
Prepare the method that the micro-nano array of titanium oxide supports monatomic platinum catalyst Download PDFInfo
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- CN109201047A CN109201047A CN201811093639.3A CN201811093639A CN109201047A CN 109201047 A CN109201047 A CN 109201047A CN 201811093639 A CN201811093639 A CN 201811093639A CN 109201047 A CN109201047 A CN 109201047A
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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
Abstract
The invention discloses the methods for preparing the micro-nano array of titanium oxide and supporting monatomic platinum catalyst, and feature includes the following steps: step 1: hydrothermal growth of the rutile TiOx nano array in ceramic honey comb substrate；Step 2: the ceramic honey comb that nano-array integrates impregnates in platinum activity presoma；Step 3: excess solution excludes；Step 4: microwave radiation heating, drying；Step 5: high-temperature calcination.The present invention, can be with the monatomic platinum catalyst of large scale preparation titanium oxide micro nano structure array appendix by microwave radiation assisted infusion needle.Moreover, method of the invention is different from traditional baking oven heating to deposit the incipient wetness impregnation of monatomic platinum.By using microwave radiation heat substitution baking oven heating, can the deposition process by monatomic platinum on nano-array surface foreshorten to a few minutes.
Description
Technical field
The present invention relates to field of material technology, specifically relate to and prepare the micro-nano array of titanium oxide and support monatomic platinum catalyst
Method.
Background technique
Due to the high catalytic activity and selectivity to various important chemical reactions, loaded noble metal catalyst is wide
It is general to be used in the energy such as photocatalysis, electro-catalysis, vent gas treatment and Related Industries of Environmental Protection.In general, carried precious metal catalyst
Degree of scatter of the reactivity and noble metal of agent on carrier has direct relation.Noble metal is in the carrier with high-specific surface area
The finely divided active site quantity that can increase considerably catalysis reaction on material, to there is the entirety for increasing catalyst living
Property.Therefore, the partial size of platinum grain is extremely important to the catalytic performance of attached catalyst on carrier material.If can be by platinum
The partial size of grain is reduced to single atom, then the activity of catalyst, especially low temperature active, it will obtain tremendous increase.According to report
Road, the monatomic platinum catalyst of appendix have the advantages that it is a variety of, such as cerium oxide appendix monatomic platinum catalyst to oxidation reaction
Show the low-temperature oxidation activity and hydrothermal stability of superelevation.At the same time, since the monatomic platinum of high degree of dispersion is instead of original
Some nanometers or sub-nanometer platinum grain, the dosage and industrial production cost of catalyst entirety noble metal can be greatly lowered.
Unquestionably, carried monatomic platinum catalyst is just increasingly by the concern of industry.
The technology for manufacturing carried monatomic platinum catalyst reported at present can be diveded into following two methods:
(1) coprecipitation；(2) incipient wetness.In coprecipitation, the presoma and support oxide presoma of platinum are specifically to rub
, than mixing and being dissolved in solvent, the pH value and temperature of solvent need to be maintained at particular value for you.Monatomic platinum is aoxidized in carrier
Object surface is precipitated simultaneously with oxide carrier.But this method is only applicable to the specific load being readily synthesized at normal temperatures and pressures
Body material, and it is not suitable for the carrier material that need to be prepared under given conditions.Another method, i.e. incipient wetness, refer to use
Platinum precursor solution impregnates the catalyst carrier prepared.The volume of platinum precursor solution should be with the total pore volume of catalyst carrier
It is similar, a series of processes for breeding and drying are undergone, monatomic platinum can be dispersed on carrier material.This method is suitable for
Various metal oxide carriers.But both methods all has to pass through prolonged drying process, it is small from a few houres to tens
When differ.In addition, for those of structural complexity backing material, such as the metal oxidation in cordierite honeycomb substrate
Object nano-array, both methods all cannot be used for preparing monatomic platinum catalyst.Firstly, when being related to nano-array carrier,
It can exclude coprecipitation method.Secondly, the total pore volume for the nano-array being grown on cordierite is difficult to assess, because of cordierite
Substrate occupies most of catalyst volume and pore volume.In addition, the drying process of just wet impregnation usually need to be in 50-80 DEG C of sky
It is carried out in gas.Under these conditions, platinum precursor solution tend to towards rate of drying faster substrate duct both ends flow, it is adjoint and
Come the result is that most of platinum can be gathered in the both ends of substrate and be difficult to be formed monatomic platinum dispersion, to seriously reduce whole platinum
The catalytic activity of utilization rate and gained catalyst.
Three-dimensional metal oxide nano-array has low cost, high catalysis as a kind of new structural nanocatalyst
The features such as activity, high stability.It is reported that there are many transition metal oxide nano array successful growths in cordierite honeycomb
In substrate, and reacted for being catalyzed to be catalyzed in some column of the energy and environmental correclation.Such as the oxidation reaction, hydrocarbon of carbon monoxide
The oxidation reaction of object, hydrogenation of carbon dioxide prepare methanol and low-temp desulfurization reaction.To further increase nano-array catalyst
Low-temperature catalytic activity, the appropriate noble metal that is added will be future direction.From the point of view of current development, three-dimensional manometer array supports list
Atom platinum catalyst will become a new generation i.e. for the integral catalyzer of industrialized low cost, high activity.Rutile structure
TiOx nano array as a kind of high-specific surface area, ep-type material resistant to high temperature, it is extensive single former to can be used as preparation
The ideal carrier of sub- platinum catalyst.
Summary of the invention
The purpose of the present invention is to provide a kind of to prepare the side that the micro-nano array of titanium oxide supports monatomic platinum catalyst
Method.In order to achieve the object of the present invention, it is proposed to adopt the following technical solutions:
One aspect of the present invention is related to preparing the method that the micro-nano array of titanium oxide supports monatomic platinum catalyst, and feature includes such as
Lower step:
Step 1: hydrothermal growth of the rutile TiOx nano array in ceramic honey comb substrate；
Step 2: the ceramic honey comb that nano-array integrates impregnates in platinum activity presoma；
Step 3: excess solution excludes；
Step 4: microwave radiation heating, drying, drying time is 1 ~ 20 minute, preferably 2 ~ 10 minutes；
Step 5: high-temperature calcination.
The present invention has homogeneous heating by microwave radiation heating, drying, and speed is fast, effective suppression solution volatilization shrinkage band
The uneven situation in part come.
In a preferred embodiment of the present invention, the rutile TiOx nano array is in ceramic honey comb substrate
Hydrothermal growth include cordierite honeycomb substrate after the load of titanium peroxide crystal seed, integrally immersed titanium oxide growth solution
In, and be sealed in < high-pressure reactor of 2Mpa in carry out hydrothermal growth.
In a preferred embodiment of the present invention, the titanium oxide growth solution includes titanium oxide organic precursor,
Hydrochloric acid, organic solvent are mixed, and the organic solvent is selected from one of toluene, butanone and n-hexane or a variety of combinations.
In a preferred embodiment of the present invention, the integrated ceramic honey comb of the nano-array is in platinum activity presoma
Middle dipping includes: after the integrated ceramic honey comb of TiOx nano array is by cleaning drying, to be dipped into one after hydrothermal growth
Determine in the platinum activity precursor water solution of concentration, and solution and substrate are placed in 0.5 ~ 2 minute in ultrasonic unit and received with exclusion
Bubble in rice array.By excluding bubble, be conducive to metal salt coated in its surface.
In a preferred embodiment of the present invention, excess solution exclusion includes: by honeycomb substrates from platinum forerunner
When being taken out in body aqueous solution, redundant solution is blown out out of honeycomb substrates duct with air knife.
In a preferred embodiment of the present invention, the microwave radiation heating, drying includes: that air knife is processed
Honeycomb substrates are transferred in microwave heating box and dry.
Preferably, in the drying process, honeycomb substrates keep rotation in microwave heating box, to balance honeycomb substrates everywhere
Rate of drying.By this method, it can achieve monatomic platinum being uniformly distributed in honeycomb substrates duct, avoid platinum grain
It is gathered in duct both ends.
In a preferred embodiment of the present invention, the high-temperature calcination includes being transferred to the honeycomb substrates after drying
In high-temperature calcination stove, and it is to slowly warm up to calcination temperature.
The present invention, can be with large scale preparation titanium oxide micro nano structure array appendix by microwave radiation assisted infusion needle
Monatomic platinum catalyst.Moreover, method of the invention is different from traditional baking oven heating to deposit the first immersion of monatomic platinum
Stain.By using microwave radiation heat substitution baking oven heating, can by monatomic platinum nano-array surface deposition process shorten
To a few minutes.In addition, microwave radiation can balance the rate of drying of ceramic honey comb substrate different location, and then monatomic platinum is made to exist
Dispersion on TiOx nano array carrier is more uniform.This microwave radiation assisted infusion is applicable to some list atoms
Coating of the platinum on metal oxide nano array.
Detailed description of the invention
Fig. 1: preparation process schematic diagram；
Fig. 2: the micro-nano array of titanium oxide prepared by embodiment 1 supports the transmission microscopy photo of monatomic platinum catalyst.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below, it is described be explanation of the invention without
It is to limit, method and its relevant reagent used in the present invention can have other optional and alternative solutions, can reach phase
With technical result.
Embodiment 1
Step 1: hydrothermal growth of the rutile TiOx nano array in ceramic honey comb substrate.Cordierite honeycomb substrate is passing through
After the load of titanium peroxide crystal seed, integrally immersed in titanium oxide growth solution, and be sealed in high-pressure reactor and carry out high-temperature water
It is thermally grown.Titanium oxide growth solution is generally by titanium oxide organic precursor, hydrochloric acid, and organic solvent (toluene, butanone, n-hexane) is mixed
Conjunction is made.
Step 2: dipping of the integrated ceramic honey comb of nano-array in platinum activity presoma.After hydrothermal growth, titanium oxide
After the integrated ceramic honey comb of nano-array undergoes a series of cleaning drying, it is dipped into certain density platinum activity precursor water solution
In, and solution and substrate are placed in ultrasonic unit one minute to exclude the bubble in nano-array.Platinum precursor solution
Concentration is determined by the size of honeycomb substrates and the appendix amount of platinum.
Step 3: excess solution excludes.When honeycomb substrates are taken out from platinum precursor water solution, in honeycomb substrates duct
Tank solution can be retained, needs to be blown out redundant solution from duct with air knife.
Step 4: microwave radiation heating, drying.The processed honeycomb substrates of air knife are transferred in microwave heating box and are dried.
In the drying process, honeycomb substrates need to keep rotating in microwave heating box, to balance the rate of drying of honeycomb substrates everywhere.
By this method, it can achieve monatomic platinum being uniformly distributed in honeycomb substrates duct, platinum grain avoided to be gathered in duct
Both ends.
Step 5: high-temperature calcination.Honeycomb substrates after drying are transferred in high-temperature calcination stove, and are to slowly warm up to calcine
Temperature.This step makes the decomposition of all platinum presomas be changed into monatomic platinum to be scattered in TiOx nano array surface.
The preparation method that TiOx nano array of the invention supports monatomic platinum catalyst has following benefit:
(1) preparation time can be greatly shortened.Microwave radiation can directly heat be adsorbed in nano-array surface presoma it is molten
Liquid, accelerates the evaporation of precursor solution, to avoid the long-time being subjected in the monatomic catalyst preparation process of tradition pregnant
Educate drying course.
(2) this method can be used on complicated carrier material preparing monatomic platinum catalyst.Traditional co-deposition
Method is not suitable for molded carrier material.Another incipient wetness is because be difficult to accurately estimate the total of TiOx nano array
Pore volume is also excluded from.Therefore, it not currently exists and can be used for the method for large-scale production to prepare TiOx nano array load
The monatomic platinum catalyst carried, by improving the process for impregnating and drying, this patent the method can be used for a variety of nano-arrays
Integrated substrate.
(3) uniformity that platinum is distributed on nano-array carrier can be improved.For the honeycomb substrates that nano-array integrates, pass
The heating means of system will lead to platinum precursor solution and tend to flow to rate of drying faster substrate duct both ends.Microwave radiation auxiliary
Drying can balance the rate of drying of integral honeycomb substrate, be distributed on nano-array in substrate duct so as to improve monatomic platinum
Uniformity, avoid excessive platinum from being gathered in the formation on the nano-array at duct both ends and influencing monatomic platinum.
The above specific embodiment is only presently preferred embodiments of the present invention, is not intended to limit the invention, all in the present invention
Spirit and principle within any modification, equivalent substitution, improvement and etc. done, should be included in protection scope of the present invention it
It is interior.The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art,
Under the premise of not departing from principle of the present invention, it can also make several improvements and retouch, these improvements and modifications also should be regarded as
Protection scope of the present invention.
Claims (8)
1. preparing the method that the micro-nano array of titanium oxide supports monatomic platinum catalyst, feature includes the following steps:
Step 1: hydrothermal growth of the rutile TiOx nano array in ceramic honey comb substrate；
Step 2: the ceramic honey comb that nano-array integrates impregnates in platinum activity presoma；
Step 3: excess solution excludes；
Step 4: microwave radiation heating, drying, drying time is 1 ~ 20 minute, preferably 2 ~ 10 minutes；
Step 5: high-temperature calcination.
2. according to the method described in claim 1, hydro-thermal of the rutile TiOx nano array in ceramic honey comb substrate
Growth includes cordierite honeycomb substrate after the load of titanium peroxide crystal seed, is integrally immersed in titanium oxide growth solution, and close
It is enclosed in high-pressure reactor and carries out hydrothermal growth.
3. hydrochloric acid has according to the method described in claim 1, the titanium oxide growth solution includes titanium oxide organic precursor
Solvent is mixed, and the organic solvent is selected from one of toluene, butanone and n-hexane or a variety of combinations.
4. according to the method described in claim 1, the ceramic honey comb that the nano-array integrates impregnates in platinum activity presoma
It include: after hydrothermal growth, after the integrated ceramic honey comb of TiOx nano array is by cleaning drying, before being dipped into platinum activity
It drives in body aqueous solution, and solution and substrate is placed in ultrasonic unit 0.5 ~ 2 minute to exclude the bubble in nano-array.
5. according to the method described in claim 1, excess solution exclusion includes: by honeycomb substrates from platinum precursor water solution
When middle taking-up, redundant solution is blown out out of honeycomb substrates duct with air knife.
6. according to the method described in claim 1, the microwave radiation heating, drying includes: by the processed honeycomb substrates of air knife
It is transferred in microwave heating box and dries.
7. honeycomb substrates keep rotation in microwave heating box according to the method described in claim 6, during the drying process, with
Balance the rate of drying of honeycomb substrates everywhere.
8. according to the method described in claim 1, the high-temperature calcination includes that the honeycomb substrates after drying are transferred to high temperature to forge
It burns in furnace, and is to slowly warm up to calcination temperature.
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| CN110227486A (en) * | 2019-06-21 | 2019-09-13 | 福建龙新三维阵列科技有限公司 | Multiple active components catalyst and preparation method thereof for VOCs catalysis burning |
| CN110302803A (en) * | 2019-07-19 | 2019-10-08 | 福建龙新三维阵列科技有限公司 | Composite catalyst and preparation method thereof for VOCs catalysis burning |
| CN110479261A (en) * | 2019-09-10 | 2019-11-22 | 福建龙新三维阵列科技有限公司 | VOCs catalysis oxidation loaded catalyst and preparation method thereof |
| CN110479260A (en) * | 2019-09-10 | 2019-11-22 | 福建龙新三维阵列科技有限公司 | The preparation method of high activity noble metal carrier catalyst |
| CN112844490A (en) * | 2021-01-27 | 2021-05-28 | 福建龙新三维阵列科技有限公司 | Universal organic waste gas catalyst, preparation method and application |
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| CN110227486A (en) * | 2019-06-21 | 2019-09-13 | 福建龙新三维阵列科技有限公司 | Multiple active components catalyst and preparation method thereof for VOCs catalysis burning |
| CN110302803A (en) * | 2019-07-19 | 2019-10-08 | 福建龙新三维阵列科技有限公司 | Composite catalyst and preparation method thereof for VOCs catalysis burning |
| CN110479261A (en) * | 2019-09-10 | 2019-11-22 | 福建龙新三维阵列科技有限公司 | VOCs catalysis oxidation loaded catalyst and preparation method thereof |
| CN110479260A (en) * | 2019-09-10 | 2019-11-22 | 福建龙新三维阵列科技有限公司 | The preparation method of high activity noble metal carrier catalyst |
| CN110479261B (en) * | 2019-09-10 | 2022-07-12 | 福建龙新三维阵列科技有限公司 | VOCs catalytic oxidation supported catalyst and preparation method thereof |
| CN112844490A (en) * | 2021-01-27 | 2021-05-28 | 福建龙新三维阵列科技有限公司 | Universal organic waste gas catalyst, preparation method and application |
| CN112844490B (en) * | 2021-01-27 | 2023-06-30 | 福建龙新三维阵列科技有限公司 | Universal organic waste gas catalyst, preparation method and application |
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Application publication date: 20190115 |