CN103623831A - Copper oxide-cerium oxide compound and preparation method thereof as well as application of compound in catalytic field - Google Patents
Copper oxide-cerium oxide compound and preparation method thereof as well as application of compound in catalytic field Download PDFInfo
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Abstract
The invention relates to a copper oxide-cerium oxide compound and a preparation method thereof as well as an application of the compound in the catalytic field. The chemical formula of the copper oxide-cerium oxide compound is xCuO-(1-x)-CeO2(x=0.1-0.9), wherein the size distribution of CuO is 20-50nm and the size distribution of CeO2 is 5-10nm. The copper oxide-cerium oxide compound is structurally characterized in that part of CeO2 nanoparticles are interspersed on CuO particles in a cluster manner. The synthetic method of the copper oxide-cerium oxide compound is a two-step coprecipitation method. The copper oxide-cerium oxide compound is applied as a catalytic material and is particularly suitable for selective catalytic oxidation of CO in a hydrogen-enriching environment. The material is low in preparation cost and easy to synthesize in a large scale. The copper oxide-cerium oxide compound has a wide application prospect in a hydrogen preparation system in a water gas conversion process and a hydrogen supply system of proton-exchange membrane fuel cells.
Description
Technical field
The present invention relates to cupric oxide-cerium oxide compound and preparation method thereof and application in catalytic field.
Background technology
Proton Exchange Membrane Fuel Cells is a kind of fuel cell that produces electric power and heating power with hydrogen-containing fuel and air effect, take noble metal as electrode, solid macromolecule PEM be dielectric, without any chemical liquid, 80 ℃～100 ℃ temperature ranges operate under normal pressure, produce pure water and heat after generating.
Hydrogen is a kind of desirable Proton Exchange Membrane Fuel Cells fuel, has operating temperature low, and energy density is high, and the feature that toggle speed is fast has broad prospect of application in transportation power type, type field and the unit field such as portable.Hydrogen is generally prepared through reforming reaction, water gas shift reaction by hydrocarbon (as methyl alcohol, natural gas, oil) at present, approximately 200 ℃ of gained mixture temperatures.In this technique gained hydrogen-rich gas, still contain 0.5%～1% CO residual, fuel cell is had to strong toxic action, reduce battery power output and operating efficiency.Therefore CO concentration in hydrogen-rich gas must be reduced to below 50ppm.
Selective catalytic oxidation CO is the method for CO in the rich hydrogen environment of simple and economically viable reduction.About the catalyst of selective oxidation CO under rich hydrogen environment, mainly take the methods such as the noble metals such as different carriers load Au, Pt, Pd, Rh and Ru and hydro-thermal and prepare cupric oxide-cerium oxide, compound such as oxidation copper-zine oxide etc. as main.But these catalyst exist cost high, the problem such as completely conversion temperature window is narrow, is difficult to meet growing industrial requirement, and it is still extremely urgent that therefore preparation is applicable to the rich hydrogen environmental selection of 80 ℃～180 ℃ wide windows carbon monoxide oxidation materials.The present invention reports a kind of cupric oxide-cerium oxide compound and preparation method thereof, this compound has excellent selective catalytic oxidation CO performance under rich hydrogen environment, is specially adapted to the hydrogen-feeding system of Water gas shift/WGS technique hydrogen manufacturing system and Proton Exchange Membrane Fuel Cells.
Summary of the invention
The object of the invention is to provide a kind of cupric oxide-cerium oxide compound catalyze material and preparation method thereof.
Cupric oxide-cerium oxide compound catalyze material chemical composition provided by the invention is xCuO-(1-x) CeO
2(x=0.1～0.9);
Cupric oxide-cerium oxide compound provided by the invention, CuO particle diameter is distributed as 20～50nm, CeO
2particle diameter is distributed as 5～10nm;
Cupric oxide-cerium oxide compound provided by the invention, CeO
2nano particle cluster is partly interspersed on CuO particle;
The preparation method of cupric oxide-cerium oxide compound provided by the invention, adopting water-soluble mantoquita and water-soluble cerium salt is raw material, adopts two step coprecipitations synthetic;
Described water-soluble mantoquita is selected from one or more in copper nitrate, copper acetate, copper chloride, copper sulphate; Described water-soluble cerium salt is selected from one or more in cerous nitrate, cerous acetate, cerium chloride, ammonium ceric nitrate, cerous sulfate.
The preparation method of described cupric oxide-cerium oxide compound, wherein said two step coprecipitations, first step reaction is used weak base as coprecipitator.
The preparation method of described cupric oxide-cerium oxide compound, wherein said two step coprecipitations, second step reaction is used highly basic as coprecipitator.
Cupric oxide-cerium oxide compound provided by the invention, in air, roasting coprecipitate obtains;
Cupric oxide-cerium oxide compound provided by the invention is applied as catalysis material;
Described cupric oxide-cerium oxide compound is specially adapted to selective catalytic oxidation carbon monoxide under rich hydrogen environment;
The application of described cupric oxide-cerium oxide compound, the catalytic reaction row atmosphere heat treatment of advancing;
Accompanying drawing explanation
Fig. 1 is cupric oxide-cerium oxide compound 0.3CuO-0.7CeO in embodiment
2powder x-ray diffraction collection of illustrative plates.
Fig. 2 is cupric oxide-cerium oxide compound 0.3CuO-0.7CeO in embodiment
2powder transmission electron microscope photo, and energy dispersion X-ray spectrum.
Fig. 3 is cupric oxide-cerium oxide compound 0.3CuO-0.7CeO in embodiment
2powder, selective catalytic oxidation CO performance under rich hydrogen environment has provided catalytic oxidation performance curve that hydro-thermal method prepares cupric oxide-cerium oxide compound as a comparison case simultaneously.
Fig. 4 is cupric oxide-cerium oxide compound 0.1CuO-0.9CeO in embodiment
2powder, selective catalytic oxidation CO performance under rich hydrogen environment has provided catalytic oxidation performance curve that hydro-thermal method prepares cupric oxide-cerium oxide compound as a comparison case simultaneously.
Fig. 5 is cupric oxide-cerium oxide compound 0.7CuO-0.3CeO in embodiment
2powder, selective catalytic oxidation CO performance under rich hydrogen environment has provided catalytic oxidation performance curve that hydro-thermal method prepares cupric oxide-cerium oxide compound as a comparison case simultaneously.
The specific embodiment
Tester and condition
X-ray powder diffraction instrument (XRD model Rigaku MiniFlex II), test specification: 20～80 °.
Transmission electron microscope (model of TEM: JEM-2010), accelerating potential 200KV.
Gas chromatograph (gas chromatograph model: Shimadzu GC-2014).
Catalytic performance test condition
Selective catalytic oxidation CO under rich hydrogen environment: take 0.1g cupric oxide-cerium oxide compound powder body material and insert in fixed bed reactors, first carry out atmosphere heat treatment, pass into subsequently gaseous mixture, its component is H
250%, CO1%, O
21%, all the other are He.Mixed gas flow is 40mL/min, pressure 0.3Mpa, 60 ℃～180 ℃ of probe temperatures, the conversion ratio of CO and CO
2selectively by chromatogram GC-2014, analyzed.Hydro-thermal method is prepared cupric oxide-cerium oxide compound catalysis material and under similarity condition, is tested as a comparison case.
Further set forth by the following examples feature of the present invention, but be not limited to embodiment.
Embodiment 1:0.3CuO-0.7CeO
2compound
Take 3mmol copper acetate, 7mmol cerous nitrate is dissolved in appropriate amount of deionized water altogether; Get 30mmol ammoniacal liquor; Copper acetate and cerous nitrate mixed solution liquid are added in ammonia spirit, stir 4h it is fully reacted; Dripping 0.5M NaOH solution to pH value is 6～9, continues to stir 2h; Then sediment will be obtained after reacted product separation; The sediment obtaining is fully washed with deionization, and 80 ℃ dry; After finally calcining 4h in air again, obtain cupric oxide-cerium oxide compound.
Fig. 1 0.3CuO-0.7CeO that for this reason prepared by embodiment
2the X-ray diffracting spectrum of composite materials, the spectrogram of powder can the cerium oxide of index fluorite structure and the cupric oxide of monoclinic phase structure, and therefore, synthetic product is cupric oxide-cerium oxide compound.Fig. 2 and Fig. 3 be transmission electron microscope photo and the energy dispersion X-ray spectrum of sample for this reason, can find out the about 6nm of crystallite dimension of cerium oxide, and the crystallite dimension of cupric oxide is 40nm, and partial oxidation cerium nano particle cluster is interspersed on copper oxide particle.
This cupric oxide-cerium oxide compound can be used as catalyst, selective catalytic oxidation CO under rich hydrogen environment.According to above-mentioned catalytic performance test condition, the catalytic performance curve obtaining as shown in Figure 3, and is prepared cupric oxide-cerium oxide compound catalysis material with hydro-thermal method and is contrasted.Cupric oxide-cerium oxide compound catalysis material provided by the invention under rich hydrogen environment 60 ℃ time the conversion ratio of CO arrive 75%, be selectively 90%; At 90 ℃ of conversion ratios, arriving 100%, is selectively 96%, at 180 ℃ of conversion ratios, is 100%, and conversion ratio is 88%.Therefore, 0.3CuO-0.7CeO provided by the invention
2composite materials has excellent selective catalysis performance within the scope of 80 ℃～180 ℃.
Embodiment 2:0.1CuO-0.9CeO
2compound
Take 1mmol copper nitrate, 9mmol cerium chloride is dissolved in appropriate amount of deionized water altogether; Get 10mmol urea and be dissolved in appropriate amount of deionized water; Copper nitrate and cerium chloride cerium mixed solution liquid are added in aqueous solution of urea, stir 4h it is fully reacted; Dripping 0.5M NaOH solution to pH value is 6～9, continues to stir 2h; Then sediment will be obtained after reacted product separation; The sediment obtaining is fully washed with deionization, and 80 ℃ dry; After finally calcining 4h in air again, obtain cupric oxide-cerium oxide compound.
0.1CuO-0.9CeO prepared by this embodiment
2the spectrogram of the X-ray diffraction of composite materials can the cerium oxide of index fluorite structure and the cupric oxide of monoclinic phase structure, shows that synthetic product is cupric oxide-cerium oxide compound.According to X-ray diffracting spectrum, calculate and show, the average grain size of cerium oxide is about 8nm.
This cupric oxide-cerium oxide compound is as catalyst, selective catalytic oxidation CO under rich hydrogen environment.According to above-mentioned catalytic performance test condition, the catalytic performance curve obtaining as shown in Figure 4, and is prepared cupric oxide-cerium oxide compound catalysis material with hydro-thermal method and is contrasted.Cupric oxide-cerium oxide compound catalysis material provided by the invention under rich hydrogen environment 90 ℃ time CO conversion ratio arrive 90%, be selectively 100%; In the time of 120 ℃, conversion ratio arrives 100%, is selectively 96%; At 180 ℃ of conversion ratios, be 100%, conversion ratio is 90%.Therefore, 0.1CuO-0.9CeO provided by the invention
2composite materials has excellent selective catalysis performance within the scope of 90 ℃～180 ℃.
Embodiment 3:0.7CuO-0.3CeO
2compound
Take 7mmol copper acetate, 3mmol cerium chloride is dissolved in appropriate amount of deionized water altogether, (A liquid); Get 10mmol urea and be dissolved in appropriate amount of deionized water (B liquid); Copper nitrate and cerium chloride cerium mixed solution liquid are added in aqueous solution of urea, stir 4h it is fully reacted; Dripping 0.5M NaOH solution to pH value is 6～9, continues to stir 2h; Then sediment will be obtained after reacted product separation; The sediment obtaining is fully washed with deionization, and 80 ℃ dry; After finally calcining 4h in air again, obtain cupric oxide-cerium oxide compound.
0.7CuO-0.3CeO prepared by this embodiment
2the X-ray diffracting spectrum of composite materials, the spectrogram of powder can the cerium oxide of index fluorite structure and the cupric oxide of monoclinic phase structure, shows that synthetic product is cupric oxide-cerium oxide compound.According to X-ray diffracting spectrum, calculate and show, the average grain size of cerium oxide is about 18nm, and cupric oxide average grain size is 25nm.
This cupric oxide-cerium oxide compound is as catalyst, selective catalytic oxidation CO under rich hydrogen environment.According to above-mentioned catalytic performance test condition, the catalytic performance curve obtaining as shown in Figure 5, and is prepared cupric oxide-cerium oxide compound catalysis material with hydro-thermal method and is contrasted.Cupric oxide-cerium oxide compound catalysis material provided by the invention has excellent selective catalysis performance within the scope of 150 ℃～180 ℃.Under rich hydrogen environment, the conversion ratio of CO arrives 97% 150 ℃ time, is selectively 100%; At 180 ℃ of conversion ratios, arriving 100%, is still selectively 100%.
Claims (10)
1. cupric oxide-cerium oxide compound, is characterized in that: its chemical molecular formula is xCuO-(1-x) CeO
2(x=0.1～0.9).
2. compound according to claim 1, is characterized in that: CuO particle diameter is distributed as 20～50nm, CeO
2particle diameter is distributed as 5～10nm.
3. the preparation method of compound described in claim 1, adopting water-soluble mantoquita and water-soluble cerium salt is raw material, it is characterized in that: adopt two step coprecipitations synthetic.
4. method claimed in claim 3, is characterized in that: described water-soluble mantoquita is selected from one or more in copper nitrate, copper acetate, copper chloride, copper sulphate; Described water-soluble cerium salt is selected from one or more in cerous nitrate, cerous acetate, cerium chloride, ammonium ceric nitrate, cerous sulfate.
5. method according to claim 3, is characterized in that: the first step reaction in two described step coprecipitations is used weak caustic solution as coprecipitator, and second step reaction is used strong base solution as coprecipitator.
6. method according to claim 5, is characterized in that: described weak caustic solution is selected from one or more in ammoniacal liquor, urea, sodium acid carbonate, dibastic sodium phosphate; Described strong base solution is selected from one or both in NaOH, potassium hydroxide.
7. method according to claim 3, is characterized in that: roasting coprecipitate in air, sintering temperature is 300 ℃～500 ℃.
8. compound claimed in claim 1 is applicable to selective catalytic oxidation carbon monoxide under rich hydrogen environment.
9. according to the application of compound described in right 8, it is characterized in that: the row atmosphere heat treatment of advancing of described material catalytic reaction.
10. according to the application of compound described in right 8, it is characterized in that: the temperature of affiliated catalytic reaction is 80 ℃～180 ℃.
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Cited By (10)
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|---|---|---|---|---|
| CN104014345A (en) * | 2014-06-25 | 2014-09-03 | 福州大学 | CuO-CeO2 catalyst for water gas conversion reaction and preparation method thereof |
| CN106732654A (en) * | 2017-01-13 | 2017-05-31 | 昆明理工大学 | A kind of preparation method of the oxidation carbon/carbon-copper composite material of loading nano silvery |
| CN106732625A (en) * | 2016-12-09 | 2017-05-31 | 中南大学 | A kind of Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure and its preparation and application |
| CN106935872A (en) * | 2017-03-07 | 2017-07-07 | 福州大学 | A kind of preparation method of the modified fuel battery anode catalyst of precipitating reagent |
| CN107445194A (en) * | 2017-09-11 | 2017-12-08 | 吉林大学 | The preparation method of cerium dopping copper sulfide CdS quantum dots |
| CN107473260A (en) * | 2017-09-11 | 2017-12-15 | 吉林大学 | Twin cupric oxide mixes the preparation method of europium room temperature ferromagnetic semiconductor material |
| CN107597130A (en) * | 2017-09-29 | 2018-01-19 | 济南大学 | Different scale high-specific surface area cerium oxide cupric oxide composite mesopore ball and preparation method |
| CN111871418A (en) * | 2020-06-29 | 2020-11-03 | 润泰化学（泰兴）有限公司 | Coated nano catalyst for one-step synthesis of isobutyraldehyde from methanol and ethanol and preparation method thereof |
| CN111905735A (en) * | 2020-08-24 | 2020-11-10 | 清华大学深圳国际研究生院 | Preparation method and application of waxberry-shaped catalytic material |
| CN112844394A (en) * | 2019-11-27 | 2021-05-28 | 中国科学院大连化学物理研究所 | CuO-CeO2Preparation method of supported catalyst and application of supported catalyst in tail gas NOxAnd application in anaerobic elimination of CO |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104014345A (en) * | 2014-06-25 | 2014-09-03 | 福州大学 | CuO-CeO2 catalyst for water gas conversion reaction and preparation method thereof |
| CN104014345B (en) * | 2014-06-25 | 2016-05-04 | 福州大学 | For the CuO-CeO of water gas shift reaction2Catalysts and its preparation method |
| CN106732625A (en) * | 2016-12-09 | 2017-05-31 | 中南大学 | A kind of Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure and its preparation and application |
| CN106732654A (en) * | 2017-01-13 | 2017-05-31 | 昆明理工大学 | A kind of preparation method of the oxidation carbon/carbon-copper composite material of loading nano silvery |
| CN106935872A (en) * | 2017-03-07 | 2017-07-07 | 福州大学 | A kind of preparation method of the modified fuel battery anode catalyst of precipitating reagent |
| CN106935872B (en) * | 2017-03-07 | 2019-12-17 | 福州大学 | Preparation method of precipitator modified fuel cell anode catalyst |
| CN107473260A (en) * | 2017-09-11 | 2017-12-15 | 吉林大学 | Twin cupric oxide mixes the preparation method of europium room temperature ferromagnetic semiconductor material |
| CN107473260B (en) * | 2017-09-11 | 2019-03-19 | 吉林大学 | Twin copper oxide mixes the preparation method of europium room temperature ferromagnetic semiconductor material |
| CN107445194B (en) * | 2017-09-11 | 2019-04-09 | 吉林大学 | The preparation method of cerium dopping copper sulfide CdS quantum dots |
| CN107445194A (en) * | 2017-09-11 | 2017-12-08 | 吉林大学 | The preparation method of cerium dopping copper sulfide CdS quantum dots |
| CN107597130A (en) * | 2017-09-29 | 2018-01-19 | 济南大学 | Different scale high-specific surface area cerium oxide cupric oxide composite mesopore ball and preparation method |
| CN112844394A (en) * | 2019-11-27 | 2021-05-28 | 中国科学院大连化学物理研究所 | CuO-CeO2Preparation method of supported catalyst and application of supported catalyst in tail gas NOxAnd application in anaerobic elimination of CO |
| CN111871418A (en) * | 2020-06-29 | 2020-11-03 | 润泰化学（泰兴）有限公司 | Coated nano catalyst for one-step synthesis of isobutyraldehyde from methanol and ethanol and preparation method thereof |
| CN111905735A (en) * | 2020-08-24 | 2020-11-10 | 清华大学深圳国际研究生院 | Preparation method and application of waxberry-shaped catalytic material |
| CN111905735B (en) * | 2020-08-24 | 2023-02-24 | 清华大学深圳国际研究生院 | Preparation method and application of waxberry-shaped catalytic material |
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