CN107051433A - The preparation method of zinc oxide supported palladium/platinum catalyst and the application in CO catalysis oxidations - Google Patents
The preparation method of zinc oxide supported palladium/platinum catalyst and the application in CO catalysis oxidations Download PDFInfo
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- CN107051433A CN107051433A CN201710134761.XA CN201710134761A CN107051433A CN 107051433 A CN107051433 A CN 107051433A CN 201710134761 A CN201710134761 A CN 201710134761A CN 107051433 A CN107051433 A CN 107051433A
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01D53/86—Catalytic processes
- B01D53/864—Removing carbon monoxide or hydrocarbons
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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
- B01J23/54—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
- B01J23/58—Platinum group metals with alkali- or alkaline earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/22—Carbon dioxide
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The preparation method of zinc oxide supported palladium/platinum catalyst of the present invention：(1) prepare zinc salt metal salt solution (2) and prepare oxalate solution；(3) metal salt solution is added dropwise in oxalate solution；(4) mixed solution is cooled down, suction filtration, separation, cleaning, obtain zinc oxalate solid；(5) calcining obtains zinc oxide carrier at a certain temperature after drying；(6) zinc oxide carrier is mixed with palladium/platinum salting liquid, hydrazine hydrate reduction, obtains zinc oxide supported palladium/platinum solid mixed solution；(7) mixed solution is cooled down, suction filtration, separation, cleaning, obtain catalyst solid；(8) it is dried to obtain zinc oxide supported palladium/platinum catalyst.The preparation method of the present invention is simple and easy to control, and building-up process is time-consuming few, workable；Zinc oxide supported palladium/platinum catalyst of preparation has less amount of palladium/platinum, a higher ratio surface, and shows good catalysis CO oxidation activities and stability at room temperature, with more preferable actual application value.
Description
Technical field
The present invention relates to catalyst preparation technical field, and in particular to zinc oxalate synthesizing zinc oxide simultaneously passes through in-situ reducing
Method supported palladium and platinum synthesizing zinc oxide supported palladium/platinum catalyst and zinc oxide supported palladium/platinum catalyst are aoxidized in normal temperature one
Carbon（CO）Application in oxidation.
Background technology
Due to importance of the catalyzing carbon monoxide in practical application and academic research, so Oxidation of Carbon Monoxide is catalyzed
Always one very important research topic.Oxidation of Carbon Monoxide catalysis technique is to have been used for indoor air cleaning in recent years
Change, breathing mask, CO gas sensors, reducing discharge of waste gases, CO2Laser, Hydrogen Proton exchange film fuel battery（PEMFC）And automobile
The fields such as exhaust gas cleaner.
Even to this day, most of research work for Oxidation of Carbon Monoxide is carried out under dry environment.However,
Steam is unavoidable in actual applications, is especially played at low ambient temperatures for the catalyst steam of carried noble metal
Entirely different effect.In identical catalyzing carbon monoxide type, for transition-metal catalyst, it is probably destructive
Intoxicating agent, and for noble metal catalyst, it is probably the accelerator of catalysis oxidation.So for containing catalyst under the conditions of steam
The research of catalytic reaction be vital.
1987, Haruta et al. prepared nanogold particle on metal oxide carrier using coprecipitation method, obtains
Material show good catalysis CO oxidation susceptibilities when less than 0 DEG C, and then propose：Interaction pair between gold and carrier
Catalytic activity has important influence.Although Au catalyst system shows good catalytic activity at low temperature, by
The large-scale application of the antigravity system is hindered in its rarity and high consuming
Due to the multivalent state of transition metal, it plays the role of brilliance in the storage and release of oxygen, and this is also influence low temperature
The key factor of catalyzing carbon monoxide oxidation.And relative to the catalyst of gold-supported, the catalyst of supported palladium or platinum has more
Good stability, while also play obvious facilitation to catalyzing carbon monoxide oxidation, especially when its noble-metal-supported in
On when.And discounting for the size or form of noble metal nano particles, the synergy between noble metal and carrier is to low
Warm CO oxidation catalysis plays vital effect.In recent years, zinc oxide is being eliminated as carrier-supported precious metal catalysis material
Cause concern extensively in car tail hydrocarbon in gas, CO and other pernicious gases.Wherein, zinc oxide supported palladium/platinum is urged
Agent shows higher catalytic activity, CO can be oxidized into CO at room temperature2, and shown within the scope of wider temperature
Good stability.
But, the catalyst that most of noble metals are combined with metal oxide is larger to the amount demand of noble metal, prepares work
Skill is more complicated, and further raising is still needed to low-temperature catalyzed CO oxidation activities.Accordingly, it would be desirable to a kind of easily operated, cheap side
Method is to prepare the low-temperature catalyzed CO oxidation catalysts of high catalytic performance.
The content of the invention
It is an object of the invention to solve the above problems there is provided a kind of preparation method of zinc oxide supported palladium/platinum catalyst,
It is using zinc salt as zinc source, using palladium salt as palladium source, and chloroplatinic acid or other platinum salts are platinum source, by calcining zinc oxalate synthesizing zinc oxide,
And using method supported palladium/platinum of in-situ reducing, so that synthesizing zinc oxide supported palladium/platinum mesoporous material, the zinc oxide of preparation is born
Carry the characteristics of palladium/platinum catalyst has high-specific surface area, be uniformly dispersed compared to other Zinc oxide catalytics；The second of the present invention
Purpose is to provide the zinc oxide supported palladium/application of the platinum catalyst in normal temperature Oxidation of Carbon Monoxide.
To achieve the above object, this invention takes following technical scheme.
A kind of preparation method of zinc oxide supported palladium/platinum catalyst, it is characterized in that, comprise the steps of：
（1）Zinc salt is added in deionized water and is stirred, the mol ratio of Xin Yan ︰ deionized waters is 0.004：1, after dissolving
Obtain metal salt solution；
（2）Oxalates is dissolved in deionized water solution is made, oxalates:The mol ratio of deionized water is 0.005:1,80 DEG C
Stirred at ambient temperature at least 5min, obtains oxalate solution；
（3）In the state of being stirred continuously, by step（1）Obtained metal salt solution is added to step（2）Obtained oxalates
Continue to stir at least 120min in solution, at a temperature of 80 DEG C, obtain mixed solution；
（4）By step（3）Suction filtration after resulting mixed solution cooling；Separated；To the sediment deionization after separation
Water and ethanol are cleaned, and obtain zinc oxalate solid；
（5）By step（4）Processing is dried in obtained zinc oxalate solid：The zinc oxalate solid is placed in 60 DEG C of environment temperatures
Lower drying at least 3 hours, obtains zinc oxalate solid.By obtained zinc oxalate solid respectively in 300 DEG C, 350 DEG C, 400 DEG C, 450
Calcined under DEG C temperature conditionss in Muffle furnace, so as to obtain the different destination carrier of calcining heat --- zinc oxide carrier；
（6）Zinc oxide solid is added with palladium salt/chloroplatinic acid and is stirred in deionized water, 0.5g zinc oxide is gone added to 25ml
In ionized water, and a certain amount of palladium salt/chloroplatinic acid is added, stir at least 120min, obtain mixed solution.Stir after 120min,
0.1mol/L hydrazine hydrates are slowly added dropwise into above-mentioned mixed solution, 12h is stirred, zinc oxide supported palladium/platinum solid mixing is obtained
Liquid.
（7）Will（6）Mixed liquor suction filtration separation after load, and obtained solid is carried out clearly with deionized water and ethanol
Wash, obtain zinc oxide supported palladium/platinum solid.
（8）By step（7）Processing is dried in obtained zinc oxide supported palladium/platinum solid：By the zinc oxide supported palladium/
Platinum solid is placed under 60 DEG C of environment temperatures and dried at least 3 hours, obtains target product --- zinc oxide supported palladium/platinum catalyst.
（2-1）Further, step（1）Described zinc salt be zinc nitrate and its hydrate, zinc chloride and its hydrate or
Other soluble zinc salts.
（3-1）Further, step（2）Described oxalates be sodium oxalate and its hydrate, potassium oxalate and its hydrate or
Other Soluble oxalate salt of person.
（4-1）Further, step（6）Described palladium salt is the sour sodium of chlorine palladium, potassium chloropalladate or ammonium chloropalladate.
（5-1）Further, step（6）Described chloroplatinic acid can be replaced platinic sodium chloride, potassium chloroplatinate or ammonium chloroplatinate.
To realize above-mentioned second purpose, this invention takes following technical scheme.
Using the zinc oxide supported palladium of the preparation method preparation of zinc oxide supported palladium/platinum catalyst, platinum catalyst in normal temperature
Application in Oxidation of Carbon Monoxide.
The positive effect of the present invention is：
（1）The present invention is used as carrier using transition metal, it is to avoid using the high cost required for noble metal catalyst, makes production
Process cost is relatively low, it is easy to industrialized production, with preferable application prospect.
（2）Preparation method is simple directly easy to control, and building-up process is time-consuming few, and not high to equipment requirement, reaction condition is not severe
Carve, it is workable.
（3）Zinc oxide supported palladium/the platinum catalyst prepared using the preparation method of the present invention has less amount of palladium/platinum,
Of a relatively high ratio surface, and show good catalysis CO oxidation activities and stability at room temperature, similar is urged than existing
Agent is more cheap, with more preferable actual application value.
Brief description of the drawings
The X of the zinc oxide loaded palladium catalyst obtained under the conditions of the different calcining heats that Fig. 1 is prepared for the embodiment of the present invention 1
X ray diffraction（XRD）Collection of illustrative plates.
The X of the zinc oxide load platinum catalyst obtained under the conditions of the different calcining heats that Fig. 2 is prepared for the embodiment of the present invention 1
X ray diffraction（XRD）Collection of illustrative plates.
Fig. 3 be embodiment 1 prepare different calcining heats under the conditions of zinc oxide loaded palladium catalyst under the conditions of containing steam
To the catalytic performance test result of CO oxidation reactions.
Fig. 4 be embodiment 1 prepare different calcining heats under the conditions of zinc oxide load platinum catalyst under the conditions of containing steam
To the catalytic performance test result of CO oxidation reactions.
Embodiment
The embodiment of the preparation method of zinc oxide supported palladium/platinum catalyst of the present invention is introduced below in conjunction with accompanying drawing,
5 embodiments are provided；1 Application Example.It should be noted that the implementation of the present invention is not limited to following embodiment.
Embodiment 1
A kind of preparation method of zinc oxide supported palladium/platinum catalyst, is comprised the steps of：
（1）50ml deionized waters are taken, 14.87g zinc nitrate solids are then added into ionized water（The production point of traditional Chinese medicines reagent Co., Ltd
Analyse pure, quality purity >=99%）, metal salt solution is obtained after stirring 10min, dissolving under normal temperature.
（2）200ml deionized waters are taken, 5.7g sodium oxalates are then added into ionized water（The production point of traditional Chinese medicines reagent Co., Ltd
Analyse pure, quality purity >=99%）, 10min is stirred at 80 DEG C, obtains sodium oxalate solution.
（3）By step（1）Obtained metal salt solution is added to step（2）In obtained sodium oxalate solution, 80 DEG C of temperature
It is lower to continue to stir at least 120min, obtain mixed solution.
（4）By step（3）Suction filtration after resulting mixed solution cooling；Separated；Sediment after separation is spent
Ionized water and ethanol are cleaned, and obtain zinc oxalate solid.
（5）By step（4）Processing is dried in obtained zinc oxalate solid：The zinc oxalate solid is placed in 60 DEG C of environment
At a temperature of dry 12 hours, obtain zinc oxalate solid.By obtained zinc oxalate solid respectively in 300 DEG C, 350 DEG C, 400 DEG C, 450
Calcined under DEG C temperature conditionss in Muffle furnace, so as to obtain the different destination carrier of calcining heat --- zinc oxide carrier；
（6）Take 0.5g zinc oxide solid and 0.017g chlorine palladium acid sodium/0.03g chloroplatinic acid to add in 25ml deionized waters to carry out
Stirring, stirs at least 120min, obtains mixed solution.Stir after 120min, 0.1mol/L hydrazine hydrates are slowly added dropwise to above-mentioned
In mixed solution, 12h is stirred, zinc oxide supported palladium/platinum solid mixed liquor is obtained.
（7）Will（6）Mixed liquor suction filtration separation after load, and obtained solid is carried out clearly with deionized water and ethanol
Wash, obtain zinc oxide supported palladium/platinum solid.
（8）By step（7）Processing is dried in obtained zinc oxide supported palladium/platinum solid：By the zinc oxide supported palladium/
Platinum solid is placed under 60 DEG C of environment temperatures and dried 12 hours, obtains target product --- zinc oxide supported palladium/platinum catalyst.
Zinc oxide supported palladium/the platinum catalyst prepared to embodiment 1 carries out analysis detection using x-ray powder diffraction instrument：
X-ray diffraction（XRD）The result of collection of illustrative plates shows（Referring to Fig. 1, Fig. 2）, embodiment 1 prepare zinc oxide supported palladium/platinum urge
Agent has good crystallinity.
Embodiment 2
A kind of preparation method of zinc oxide supported palladium/platinum catalyst, basic step be the same as Example 1.
Embodiment 2 and embodiment 1 except that：
Step（1）The zinc salt used is zinc chloride.
Step（2）The oxalates used is potassium oxalate
Step（6）The palladium salt used is potassium chloroplatinate for potassium chloropalladate/platinum salt.
Embodiment 3
A kind of preparation method of zinc oxide supported palladium/platinum catalyst, basic step be the same as Example 1.
Embodiment 3 and embodiment 1 except that：
Step（1）The cerium salt used is zinc acetate.
Step（2）The oxalates used is sodium oxalate.
Step（6）The palladium salt used is potassium chloroplatinate for ammonium chloropalladate/platinum salt.
Embodiment 4
A kind of preparation method of zinc oxide supported palladium/platinum catalyst, basic step be the same as Example 1.
Embodiment 4 and embodiment 1 except that：
Step（1）The zinc salt used is zinc chloride.
Step（2）Oxalates is used for potassium oxalate.
Step（6）The palladium salt used is ammonium chloroplatinate for ammonium chloropalladate/platinum salt.
Embodiment 5
A kind of preparation method of zinc oxide supported palladium/platinum catalyst, basic step be the same as Example 1.
Embodiment 5 and embodiment 1 except that：
Step（1）The zinc salt used is zinc nitrate.
Step（2）The oxalates used is sodium oxalate.
Step（6）The palladium salt used is platinic sodium chloride for potassium chloropalladate/platinum salt.
Application Example 1（Low temperature carbon monoxide oxidation catalytic activity）
The evaluation of the catalytic activity of the zinc oxide supported palladium/platinum catalyst prepared to embodiment 1：
Catalytic evaluation experiment is carried out in U-shaped quartz reactor：200mg catalyst is added in U-shaped quartz reactor, using journey
Sequence temperature elevation system, 150 DEG C are risen to 10 DEG C/min by room temperature；With 1%vol CO, 20%vol O2, 79%vol N2It is used as unstripped gas；
Used during wet environment and gas is taken out of a certain amount of steam by bubbler, total gas flow rate is 50ml/min；Air speed is
15000ml h-1g-1；Using the gas-chromatography equipped with methane reborner（GC）, use hydrogen flame ionization detector（FID）To reaction
Front and rear gas componant is detected.
Zinc oxide supported palladium/platinum catalyst catalytic result prepared by embodiment 1 is as shown in Figure 2,3.The CO oxidation catalysis
As a result show：Zinc oxide supported palladium/platinum catalyst prepared by the embodiment of the present invention 1 shows good normal temperature at ambient conditions
Catalytic CO oxidation susceptibility, with the catalytic activity being remarkably reinforced.Zinc oxide supported palladium/platinum catalysis under the conditions of water flowing vapour
Agent has good catalytic activity, and this is due to that hydroxyl occurs in zinc oxide supported palladium/platinum catalyst surface under the conditions of water flowing vapour, so as to promote
CO oxidation reaction is entered.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, on the premise of the inventive method is not departed from, can also make some improvements and modifications, these improvements and modifications also should be regarded as
Protection scope of the present invention.
Claims (10)
1. a kind of preparation method of zinc oxide supported palladium/platinum catalyst, it is characterised in that comprise the steps of：
（1）Zinc salt is added in deionized water and is stirred, the mol ratio of Xin Yan ︰ deionized waters is 0.004：1, after dissolving
To metal salt solution；
（2）Oxalates is dissolved in deionized water solution is made, oxalates:The mol ratio of deionized water is 0.005:1,80 DEG C of temperature
The lower stirring at least 5min of degree, obtains oxalate solution；
（3）In the state of being stirred continuously, by step（1）Obtained metal salt solution is added to step（2）Obtained oxalates
Continue to stir at least 120min in solution, under 80 DEG C of environment temperatures, obtain mixed solution；
（4）By step（3）Suction filtration after resulting mixed solution cooling；Separated；To the sediment deionization after separation
Water and ethanol are cleaned, and obtain zinc oxalate solid；
（5）By step（4）Processing is dried in obtained zinc oxalate solid：The zinc oxalate solid is placed in 60 DEG C of environment temperatures
Lower drying at least 3 hours, obtains zinc oxalate solid.
2. obtained zinc oxalate solid is carried out under 300 DEG C, 350 DEG C, 400 DEG C, 450 DEG C of temperature conditionss in Muffle furnace respectively
Calcining, so as to obtain the different destination carrier of calcining heat --- zinc oxide carrier；
（6）Zinc oxide solid is added with palladium salt/chloroplatinic acid and is stirred in deionized water, 0.5g zinc oxide is gone added to 25ml
In ionized water, and a certain amount of palladium salt/chloroplatinic acid is added, stir at least 120min, obtain mixed solution.
3. stirring after 120min, 0.1mol/L hydrazine hydrates are slowly added dropwise into above-mentioned mixed solution, 12h is stirred, is aoxidized
Zinc supported palladium/platinum solid mixed liquor.
4.（7）Will（6）Mixed liquor suction filtration separation after load, and obtained solid is cleaned with deionized water and ethanol,
Obtain zinc oxide supported palladium/platinum solid.
5.（8）By step（7）Processing is dried in obtained zinc oxide supported palladium/platinum solid：By the zinc oxide supported palladium/platinum
Solid is placed under 60 DEG C of environment temperatures and dried at least 3 hours, obtains target product --- zinc oxide supported palladium/platinum catalyst.
6. the preparation method of zinc oxide supported palladium/platinum catalyst according to claim 1, it is characterised in that step（1）Institute
The zinc salt stated is zinc nitrate and its hydrate, zinc chloride and its hydrate or other soluble zinc salts.
7. the preparation method of zinc oxide supported palladium/platinum catalyst according to claim 1, it is characterised in that step（2）Institute
Oxalates is stated for sodium oxalate and its hydrate, potassium oxalate and its hydrate or other Soluble oxalate salt.
8. the preparation method of zinc oxide supported palladium/platinum catalyst according to claim 1, it is characterised in that step（6）Institute
The palladium salt stated is the sour sodium of chlorine palladium, potassium chloropalladate or ammonium chloropalladate.
9. the preparation method of zinc oxide supported palladium/platinum catalyst according to claim 1, it is characterised in that step（6）Institute
The chloroplatinic acid stated can be replaced platinic sodium chloride, potassium chloroplatinate or ammonium chloroplatinate.
10. the zinc oxide supported palladium/platinum catalyst prepared using the preparation method described in claim 1 is in normal temperature carbon monoxide oxygen
Application in change.
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| CN111790378A (en) * | 2020-07-13 | 2020-10-20 | 苏州大学 | Manganese dioxide loaded PtPd bimetallic nanosphere and preparation method and application thereof |
| CN113546620A (en) * | 2021-07-22 | 2021-10-26 | 山西大学 | Palladium oxide supported zinc-based catalyst and preparation method and application thereof |
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| CN115414931A (en) * | 2022-08-31 | 2022-12-02 | 北京工业大学 | Preparation method of Pd/ZnO catalyst for hydrogen production by methanol steam reforming |
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Application publication date: 20170818 |