CN109513464A - A kind of rare earth oxide carries platinum hydrophobic catalyst and its preparation method and application - Google Patents
A kind of rare earth oxide carries platinum hydrophobic catalyst and its preparation method and application Download PDFInfo
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- CN109513464A CN109513464A CN201811508396.5A CN201811508396A CN109513464A CN 109513464 A CN109513464 A CN 109513464A CN 201811508396 A CN201811508396 A CN 201811508396A CN 109513464 A CN109513464 A CN 109513464A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- B01J23/63—Platinum group metals with rare earths or actinides
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/024—Multiple impregnation or coating
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The invention discloses a kind of rare earth oxides to carry platinum hydrophobic catalyst and its preparation method and application, and catalytic performance is low in the prior art for solution, and regeneration frequency is high, the bad problem of stability.A kind of rare earth oxide of the present invention carries platinum hydrophobic catalyst, is support carrier with metal fiber felt using polytetrafluoroethylene (PTFE) as bonding agent and main hydrophobic medium to carry platinum rare earth oxide as active component；The load capacity for carrying platinum in platinum rare earth oxide is 0.1wt%~10wt%, and the platinum rare earth oxide and the weight ratio of polytetrafluoroethylene (PTFE) of carrying is 1:1~4, and for the quality of the catalyst based on 100%, the content of the metal fiber felt is 30wt%~70wt%.Design science of the present invention, method is simple, and catalyst of the invention has excellent catalytic properties, and regeneration frequency is low, and stability is good.
Description
Technical field
The invention belongs to HYDROGEN-WATER ISOTOPE EXCHANGE catalyst technical fields, and in particular to a kind of rare earth oxide load platinum is thin
Water catalyst and its preparation method and application.
Background technique
Currently, can be used for water to remove tritiated technological approaches mainly including hydrogen-water isotope liquid-phase catalysis exchange (Liquid
Phase Catalytic Exchange, is abbreviated as LPCE), vapor phase catalysis exchange (VaporPhase Catalytic
Exchange is abbreviated as VPCE) and combination electrolysis/catalysis exchange (Combined Electrolysis Catalytic
Exchange is abbreviated as CECE) etc..Wherein, LPCE refers to that hydrogen isotope gas and liquid water occur together under the action of catalyst
The plain exchange reaction in position；VPCE refers to that isotope occurs under the action of catalyst for hydrogen isotope gas and vapor (~200 DEG C)
Exchange reaction；And CECE be substantially LPCE process is combined together with water electrolysis process, to realize higher detritiation because
Son (note: this is because the electrolytic process of water is with isotope effect, it can be achieved that the concentration of tritium).In summary, hydrogen isotope gas
Hydrogen isotopic exchange occurs between body and water (liquid or gaseous state) to react to be core reaction mistake that above-mentioned three kinds of water goes tritiated technology
Journey.In these three technological approaches, the operating condition of LPCE is most mild, energy consumption is minimum, equipment requirement is also most simple, therefore by
Universal attention.
Due to hereinafter, water exists in liquid form, hindering hydrogen to reach to prevent water to be covered on active metal surface at 100 DEG C
To active site (causing catalyst poisoning), needed in LPCE technique using hydrophobic catalyst.Currently, in countries in the world
LPCE device in be widely used that with the hydrophobic catalyst of platinum active metal, there are mainly three types of type: the first kind is direct
Platinum is supported on hydrophobic medium, such as Pt/SDBC (Styrene Divinylbenzene Copolymer, i.e. polyethylene-two
Vinyl benzene polymer)；Second class is that first platinum is supported on the carrier with high-specific surface area (mainly including Carbon Materials, oxygen
Change aluminium, silica), silicic acid anhydride is then carried out using PTFE (Polytetrafluoroethene, i.e. polytetrafluoroethylene (PTFE))
Hydrophobic catalyst is made；Third class is that first platinum is supported on the carrier with high-specific surface area, is then coated together with PTFE
Hydrophobic catalyst is made on to stainless steel fibre felt.Noble metal platinum is that HYDROGEN-WATER ISOTOPE EXCHANGE is urged with hydrophobic due to expensive
The prime cost constituent element of agent.In above-mentioned three classes hydrophobic catalyst, the noble metal platinum of third class hydrophobic catalyst is utilized
Efficiency is relatively higher.But there is also following both sides problems for the type hydrophobic catalyst: one, currently used carrier is to hydrogen-
Water isotope exchange reaction be it is inert, main function is the dispersion degree for improving noble metal platinum, is helped substantial
Catalytic action, therefore it is limited to the promotion effect of hydrophobic catalyst catalytic performance；Two, most common metallic carrier material
Material --- Carbon Materials are easy to adsorb vapor, and the type hydrophobic catalyst is caused just to need to carry out regeneration treatment at regular intervals,
And then reduce the operational efficiency that water removes tritiated device.
Therefore it provides a kind of hydrophobic catalyst for HYDROGEN-WATER ISOTOPE EXCHANGE, has excellent catalytic properties, regeneration
Frequency is low, and stability is good, becomes those skilled in the art's urgent problem to be solved.
Summary of the invention
Technical problem solved by the present invention is providing a kind of rare earth oxide load platinum hydrophobic catalyst, the prior art is solved
Middle catalytic performance is low, and regeneration frequency is high, the bad problem of stability.
The present invention also provides the preparation methods that the rare earth oxide carries platinum hydrophobic catalyst.
Invention further provides the applications that the rare earth oxide carries platinum hydrophobic catalyst.
The technical solution adopted by the invention is as follows:
A kind of rare earth oxide of the present invention carries platinum hydrophobic catalyst, to carry platinum rare earth oxide as active component,
It is support carrier with metal fiber felt using polytetrafluoroethylene (PTFE) as bonding agent and main hydrophobic medium；The load platinum rare earth oxide
The load capacity of middle platinum is 0.1wt%~10wt%, and the platinum rare earth oxide and the weight ratio of polytetrafluoroethylene (PTFE) of carrying is 1:1~4,
For the quality of the catalyst based on 100%, the content of the metal fiber felt is 30wt%~70wt%.
Further, the load capacity for carrying platinum in platinum rare earth oxide is 2wt%；Or/and the load platinum rare-earth oxidation
The weight ratio of object and polytetrafluoroethylene (PTFE) is 1:2；Or/and the content of the metal fiber felt is 50wt%.Of the present invention one
Kind rare earth oxide carries the preparation method of platinum hydrophobic catalyst, comprising the following steps:
Step 1. preparation carries platinum rare earth oxide: platinum is loaded on rare earth oxide carrier；
Step 2. prepares suspension: load platinum rare earth oxide made from step 1 is mixed by a certain percentage with polytetrafluoroethylene (PTFE)
It closes, is configured to suspension；
Step 3. coating: suspension made from step 2 is coated on metal fiber felt, is then dried, obtains coating
Sample；
Step 4. heat treatment: the coated sample is placed in atmosphere heat treatment furnace, be passed through after vacuumizing hydrogen with it is lazy
Property gas gaseous mixture, with the heating of certain heating rate, constant temperature certain time then cools to room temperature with the furnace.
Further, the metal fiber felt is stainless steel fibre felt, and aperture is 20 mesh.
Further, in the step 1, platinum is loaded to by rare-earth oxidation using the technique of " dipping+calcining+gas reduction "
On object carrier.
Further, the specific operation process of the step 1 are as follows:
A. it impregnates: chloroplatinic acid hydrate being dissolved into deionized water and is made into platinum acid chloride solution, weighs ceria, then
It is required that chloroplatinic acid aqueous solution is added into ceria according to load capacity, is sufficiently stirred, it is dry；
B. it calcines: the sample after step A is dry being put into tube furnace and is calcined, in the zero level that flow is 300ml/min
Be heated to 400 DEG C, constant temperature 2h under air atmosphere with 10K/min, after cool to room temperature with the furnace；
C. it restores: will be through the calcined sample reduction treatment of step B, it is 300ml/min's that treatment conditions, which are in flow,
10%H2Be heated to 400 DEG C, constant temperature 2h under/Ar gaseous mixture atmosphere with 5K/min, after cool to room temperature with the furnace.
Further, it in the step 2, carries platinum rare earth oxide and is mixed with polytetrafluoroethylene (PTFE) 1:2 in mass ratio, addition is gone
Ionized water forms mixture aqueous solution, then surfactant is added into mixture aqueous solution, forms suspension.
Further, in the step 2, resistivity >=15M Ω of the deionized water, additive amount is to carry platinum rare earth oxygen
10~20 times of compound quality；The surfactant is triton X-100, and additive amount is carry platinum rare-earth oxidation amount of substance 5
~10 times.
Further, in the step 3, using multiple coating processes, suspension made from step 2 is coated to metal fibre
After tieing up on felt, heated baking water removal, after preliminarily dried, coating, heated baking again, until reaching required load capacity, institute
The temperature for stating baking is 110-130 DEG C.
Further, in the step 4, the volume content of hydrogen is 1~10% in the gaseous mixture of hydrogen and inert gas,
The flow of gaseous mixture is 100~500ml/min；Heating rate is 1~10 DEG C/min, is heated to 350-380 DEG C.
A kind of rare earth oxide of the present invention carries application of the platinum hydrophobic catalyst in HYDROGEN-WATER ISOTOPE EXCHANGE.
Compared with prior art, the invention has the following advantages:
(1) design science of the present invention, method is simple, and catalyst of the invention has excellent catalytic properties, regeneration frequency
Low, stability is good.
(2) present invention to be to carry platinum rare earth oxide as active component, and polytetrafluoroethylene (PTFE) is bonding agent and main hydrophobic medium,
Metal fiber felt is support carrier, and the hydrophobic catalyst being prepared is excellent to the catalytic efficiency of HYDROGEN-WATER ISOTOPE EXCHANGE reaction
In same type using Pt/C as the hydrophobic catalyst of active component.For example, under the test condition that temperature is 80 DEG C, gas liquid ratio is 1,
Pt/C hydrophobic catalyst has been better than to the catalysis reaction column efficiency that HYDROGEN-WATER ISOTOPE EXCHANGE is reacted in Pt/CeO2 hydrophobic catalyst
When, the half of the dosage of noble metal platinum is still insufficient the latter, economy is more preferable.
(3) present invention can since rare earth oxide surface has Lacking oxygen abundant as carrier using rare earth oxide
Play the role of activated water molecule, and then promotes the isotope exchange reaction between hydrogen and water；On the other hand, due to rare-earth oxidation
Object has good intrinsic hydrophobicity, is not easy to cause catalyst inactivation because of water vapor adsorption, to help to maintain hydrophobic catalyst
Long-time stability under LPCE work condition environment.The present invention with intrinsic hydrophobic rare earth oxide as active metal to carry
Body, the hydrophobic catalyst being prepared are weaker than using Carbon Materials as hydrophobic catalyst made from carrier the adsorption capacity of vapor,
The problem of can effectivelying prevent hydrophobic catalyst that vapor poisoning occurs in high humidity environment, helps to reduce catalyst regeneration frequency
Rate, and then promote the operational efficiency that water removes tritiated device.
(4) cost performance of the present invention is high, stable in catalytic performance is good, can remove tritiated, heavy water detritiation and again in tritium-containing liquid waste
Commercial applications are realized in the fields such as aquatic production, therefore the present invention has very high practical value and promotional value.
Detailed description of the invention
Fig. 1 is the Contact-angle measurement result that the ceria that the present invention is prepared carries platinum hydrophobic catalyst.
Fig. 2 is the Pt/CeO that the present invention is prepared2Hydrophobic catalyst and tradition Pt/C hydrophobic catalyst are same to hydrogen-water
The catalysis reaction column efficiency of the plain exchange reaction in position compares.
Fig. 3 is the Pt/CeO that the present invention is prepared2Hydrophobic catalyst and tradition Pt/C hydrophobic catalyst inhale vapor
The comparison of desorption performance.
Specific embodiment
The invention will be further described with embodiment for explanation with reference to the accompanying drawing, and mode of the invention includes but not only limits
In following embodiment.
Embodiment 1
Present embodiment discloses rare earth oxide of the invention carry platinum hydrophobic catalyst preparation method, specifically:
Step 1. preparation carries platinum rare earth oxide: chloroplatinic acid hydrate being dissolved into deionized water and is made into aqueous solution, is claimed
A certain amount of ceria is taken, is then required that a certain amount of chloroplatinic acid aqueous solution is added thereto according to load capacity, is sufficiently stirred.
After sample preliminarily dried, it is put into vacuum oven and 12h is further dried at 110 DEG C.Then, the sample after drying is put into
It is calcined in tube furnace, is heated to 400 DEG C, constant temperature 2h in the case where flow is the zero level air atmosphere of 300ml/min with 10K/min, after
Cool to room temperature with the furnace.Calcined sample then carries out reduction treatment, and treatment conditions are in 10% that flow is 300ml/min
H2Be heated to 400 DEG C, constant temperature 2h under/Ar gaseous mixture atmosphere with 5K/min, after cool to room temperature with the furnace, be made carry platinum rare-earth oxidation
Object.
Step 2. prepares suspension: being made after carrying platinum rare earth oxide, will carry platinum rare earth oxide and press with polytetrafluoroethylene (PTFE)
Mass ratio 1:2 mixing is added deionized water and forms mixture aqueous solution, then surfactant song is added into mixture aqueous solution
Logical X100 is drawn, suspension is formed.Wherein, the resistivity of deionized water >=15M Ω, additive amount are to carry platinum rare-earth oxidation amount of substance
10~20 times；The additive amount of triton X-100 is 5~10 times for carrying platinum rare-earth oxidation amount of substance.
Step 3. is supported using multiple coating processes on stainless steel fibre felt, and suspension made from step 2 is applied
After being layed on metal fiber felt, heated baking water removal, after preliminarily dried, coating, heated baking again, until reaching required
Load capacity, the temperature of the baking are 110-130 DEG C.
The coated sample is placed in atmosphere heat treatment furnace by step 4., is passed through after vacuumizing after vacuumizing and is passed through hydrogen
It is the 10%H of 200ml/min in flow with the gaseous mixture of inert gas2365 are heated to under/Ar gaseous mixture atmosphere with 2K/min
DEG C, constant temperature 15min, after cool to room temperature with the furnace.
Embodiment 2
Present embodiment discloses the performances that rare earth oxide made from embodiment 1 carries platinum hydrophobic catalyst.
Rare earth oxide made from embodiment 1 is carried into platinum hydrophobic catalyst and carries out Contact-angle measurement, the results show that itself and water
Contact angle be greater than 130 °, as shown in Fig. 1, show it with good hydrophobicity.
We are cut, after moulding, contrast test present invention under conditions of 80 DEG C, hydrogen and aqueous vapor liquor ratio are 1
The catalytic performance that prepared hydrophobic catalyst reacts HYDROGEN-WATER ISOTOPE EXCHANGE with traditional Pt/C hydrophobic catalyst.As a result
It shows, 2wt%Pt/CeO prepared by the present invention2The catalytic performance of hydrophobic catalyst is better than 10wt%Pt/C hydrophobic catalyst,
As shown in Fig. 2.From noble metal platinum with taking temperature, the dosage of the former platinum still not as good as the half of the latter, shows prepared by the present invention
Hydrophobic catalyst catalytic efficiency it is higher, corresponding economy is also more preferable.
In addition, the Pt/CeO that we are also prepared in 60 DEG C of contrast tests present invention2Hydrophobic catalyst and tradition Pt/
C hydrophobic catalyst is to vapor adsorption desorption performance.Test result is shown, compared with traditional Pt/C hydrophobic catalyst, Pt/CeO2It dredges
The water vapor adsorption capacity of water catalyst activity substance is less, and the vapor adsorbed is easier to be desorbed, as shown in Fig. 3.
Therefore, the hydrophobic catalyst prepared by the present invention, which has, goes the potentiality being on active service for a long time in tritiated device in LPCE water.
In the present invention, use CeO 2 supporting chloroplatinic acid hydrate for the prior art.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit protection model of the invention
It encloses, as long as that in body design thought of the invention and mentally makes has no the change of essential meaning or polishing, is solved
The technical issues of it is still consistent with the present invention, should all be included within protection scope of the present invention.
Claims (10)
1. a kind of rare earth oxide carries platinum hydrophobic catalyst, which is characterized in that carry platinum rare earth oxide as active component, with poly-
Tetrafluoroethene is bonding agent and main hydrophobic medium, is support carrier with metal fiber felt；Platinum in the load platinum rare earth oxide
Load capacity be 0.1wt%~10wt%, the weight ratio for carrying platinum rare earth oxide and polytetrafluoroethylene (PTFE) is 1:1~4, described
For the quality of catalyst based on 100%, the content of the metal fiber felt is 30wt%~70wt%.
2. a kind of rare earth oxide according to claim 1 carries platinum hydrophobic catalyst, which is characterized in that the load platinum rare earth
The load capacity of platinum is 2wt% in oxide；Or/and the platinum rare earth oxide and the weight ratio of polytetrafluoroethylene (PTFE) of carrying is 1:2；
Or/and the content of the metal fiber felt is 50wt%.
3. a kind of rare earth oxide according to claim 1 or 2 carries the preparation method of platinum hydrophobic catalyst, feature exists
In, comprising the following steps:
Step 1. preparation carries platinum rare earth oxide: platinum is loaded on rare earth oxide carrier；
Step 2. prepares suspension: load platinum rare earth oxide made from step 1 being mixed in a certain ratio with polytetrafluoroethylene (PTFE), is matched
Suspension is made；
Step 3. coating: suspension made from step 2 is coated on metal fiber felt, is then dried, coated sample is obtained
Product；
Step 4. heat treatment: the coated sample is placed in atmosphere heat treatment furnace, is passed through hydrogen and indifferent gas after vacuumizing
The gaseous mixture of body, with the heating of certain heating rate, constant temperature certain time then cools to room temperature with the furnace.
4. the preparation method that a kind of rare earth oxide according to claim 3 carries platinum hydrophobic catalyst, which is characterized in that institute
It states in step 1, is loaded to platinum on rare earth oxide carrier using the technique of " dipping+calcining+gas reduction ".
5. the preparation method that a kind of rare earth oxide according to claim 4 carries platinum hydrophobic catalyst, which is characterized in that institute
State the specific operation process of step 1 are as follows:
A. it impregnates: chloroplatinic acid hydrate being dissolved into deionized water and is made into platinum acid chloride solution, weighs ceria, then basis
Load capacity requires that chloroplatinic acid aqueous solution is added into ceria, is sufficiently stirred, dry；
B. it calcines: the sample after step A is dry being put into tube furnace and is calcined, in the zero level air that flow is 300ml/min
Be heated to 400 DEG C, constant temperature 2h under atmosphere with 10K/min, after cool to room temperature with the furnace；
C. it restores: will be the 10%H for being 300ml/min in flow through the calcined sample reduction treatment of step B, treatment conditions2/
Be heated to 400 DEG C, constant temperature 2h under Ar gaseous mixture atmosphere with 5K/min, after cool to room temperature with the furnace.
6. the preparation method that a kind of rare earth oxide according to claim 3 carries platinum hydrophobic catalyst, which is characterized in that institute
It states in step 2, carries platinum rare earth oxide and mixed with polytetrafluoroethylene (PTFE) 1:2 in mass ratio, deionized water is added and forms mixture water
Solution, then surfactant is added into mixture aqueous solution, form suspension.
7. the preparation method that a kind of rare earth oxide according to claim 6 carries platinum hydrophobic catalyst, which is characterized in that institute
It states in step 2, resistivity >=15M Ω of the deionized water, additive amount is 10~20 times for carrying platinum rare-earth oxidation amount of substance；
The surfactant is triton X-100, and additive amount is 5~10 times for carrying platinum rare-earth oxidation amount of substance.
8. the preparation method that a kind of rare earth oxide according to claim 3 carries platinum hydrophobic catalyst, which is characterized in that institute
It states in step 3, using multiple coating processes, after suspension made from step 2 is coated on metal fiber felt, heated baking is removed
Water, after preliminarily dried, coating, heated baking again, until reaching required load capacity, the temperature of the baking is 110-
130℃。
9. the preparation method that a kind of rare earth oxide according to claim 3 carries platinum hydrophobic catalyst, which is characterized in that institute
It states in step 4, the volume content of hydrogen is 1~10% in the gaseous mixture of hydrogen and inert gas, the flow of gaseous mixture is 100~
500ml/min；Heating rate is 1~10 DEG C/min, is heated to 350-380 DEG C.
10. a kind of rare earth oxide described in -9 any one carries platinum hydrophobic catalyst in hydrogen-water isotope according to claim 1
Application in exchange.
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Cited By (2)
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| CN111359605A (en) * | 2020-02-28 | 2020-07-03 | 中国工程物理研究院材料研究所 | Preparation method and application of novel bifunctional catalyst filler |
| CN113522358A (en) * | 2021-07-19 | 2021-10-22 | 河北工业大学 | Steam poisoning resistant catalyst applied to removal of volatile organic pollutants in coal-fired flue gas and preparation method and application thereof |
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| CN111359605A (en) * | 2020-02-28 | 2020-07-03 | 中国工程物理研究院材料研究所 | Preparation method and application of novel bifunctional catalyst filler |
| CN111359605B (en) * | 2020-02-28 | 2022-11-25 | 中国工程物理研究院材料研究所 | Preparation method and application of novel bifunctional catalyst filler |
| CN113522358A (en) * | 2021-07-19 | 2021-10-22 | 河北工业大学 | Steam poisoning resistant catalyst applied to removal of volatile organic pollutants in coal-fired flue gas and preparation method and application thereof |
| CN113522358B (en) * | 2021-07-19 | 2022-05-17 | 河北工业大学 | Steam poisoning resistant catalyst applied to removal of volatile organic pollutants in coal-fired flue gas and preparation method and application thereof |
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Application publication date: 20190326 |