CN102500386A - Preparation method for cerium nickel composite oxide catalytic material - Google Patents
Preparation method for cerium nickel composite oxide catalytic material Download PDFInfo
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- CN102500386A CN102500386A CN2011103474951A CN201110347495A CN102500386A CN 102500386 A CN102500386 A CN 102500386A CN 2011103474951 A CN2011103474951 A CN 2011103474951A CN 201110347495 A CN201110347495 A CN 201110347495A CN 102500386 A CN102500386 A CN 102500386A
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Abstract
The invention relates to a simple, convenient and quick preparation method for a cerium nickel composite oxide catalyst. The preparation method comprises the following steps of: placing a certain amount of cerous nitrate and nickel nitrate into a mortar; grinding for certain time; roasting under air atmosphere at the temperature of 550 DEG C for 5 hours; and naturally cooling to obtain the cerium nickel composite oxide catalyst. The preparation method has the advantages that: solvents are not involved in the preparation process, so loss of active species and pollution to the water environment can be effectively avoided; and the nickel species can be dispersed on cerium dioxide well. More importantly, the solvents do not exist, so gas released when metal salt is roasted can effectively serve as a pore-forming agent, and the cerium nickel catalyst with a large specific surface area and high activity can be obtained. The whole equipment has the characteristics of low energy consumption, simplicity and the like.
Description
Technical field
The present invention relates to a kind of cerium ni compound oxide catalysis material and preparation method thereof.
Background technology
China has abundant rare earth resources, and the rare earth reserves account for nearly 60% of world's gross reserves.Rare earth element makes rare earth oxide show good character at aspects such as light, electricity, magnetic and catalysis owing to have unique 4f orbital electron.Wherein, ceria is owing to have Ce
3+And Ce
4+Redox cycle takes place in two kinds of oxidation state easily.Under oxygen deprivation or reducing condition, surface portion Ce
4+Be reduced into trivalent, produce the oxygen room, form a series of uncertain CeO with oxygen defect structure
2-xUnder oxygen enrichment or oxidizing condition, Ce
3+Be prone to be oxidized to tetravalence again, make CeO
2-xBe converted into CeO
2Thereby CeO
2Show stronger storage oxygen oxygen release ability.When forming a large amount of oxygen defects, CeO
2-xStill can keep the crystal structure of fluorite type, good chemical stability is arranged.
In recent years, there is report research to point out that NiO loads to CeO
2On, the interaction owing between two kinds of metal oxides has taken into account CeO
2Good storage oxygen oxygen release ability and the good redox property of NiO have good catalytic effect.It is as catalyst, but the reaction of catalysis number of different types, like partial oxidation (POM), water-gas shift (WGS) and the hydrogenation of olefins dechlorination (HDC) etc. of methane.Recently, there are some researches show NiO-CeO
2Catalyst purifies in the reaction (NO+CO) at little molecular contaminants has good activity and selectivity, and this provides a feasible approach for efficient, the cheap non-precious metal catalyst of seeking low-temperature catalyzed elimination vehicle exhaust.
As everyone knows, the performance of catalyst receives the influence of its preparation method consumingly.At present, the cerium ni compound oxide Preparation of catalysts method of common report has: infusion process, coprecipitation, sol-gal process and firing method etc.A common trait of above method is to prepare all in solution, to carry out.Because the formulations prepared from solutions process can relate to steps such as washing, filtration, may bring active specy to run off, cause water environment pollution simultaneously.But, what deserves to be mentioned is that as a kind of method of newly reporting in the last few years, firing method can effectively utilize a large amount of gases that discharge in the roasting process, thereby makes catalyst produce fluffy structure, helps obtaining of bigger serface.In the present invention, we have reported a kind of method of solid phase preparation cerium ni compound oxide catalysis material, and wherein the nickel species can be dispersed on the ceria well, and the gas that the slaine decomposition produces in the preparation process can effectively utilize.Through comparing, find that the catalyst that method for preparing solid phase obtains has bigger specific area and pore passage structure, and the interaction between nickel and the cerium can be strengthened with other common methods.Because this method prepares raw material and is easy to get, and is simple and efficient to handle, additional low in the pollution of the environment, make it good prospects for application arranged at catalytic field.
Summary of the invention
The purpose of this invention is to provide a kind of new method for preparing cerium ni compound oxide catalysis material.The preparation process does not relate to the aqueous solution, and method is simple and efficient, and can mass preparation.The catalyst that obtains has bigger specific area and certain pore passage structure.
Principle of the present invention is following: utilize cerous nitrate and nickel nitrate the characteristics of molten condition when being heated, can occur, place mortar to grind two kinds of metallic precursor, mix back intensification roasting.After reaching fusing point, slaine can be converted into the fused salt with certain flowability, and this can make the nickel species be dispersed on the cerium well.Through the higher temperature roasting, can obtain cerium ni compound oxide catalysis material.
Technical scheme of the present invention is following:
A kind of preparation method of cerium ni compound oxide catalysis material; It is that nickel nitrate and cerous nitrate are mixed; Nickel nitrate with the ratio of the amount of substance of cerous nitrate is: 1:99-1:4; Grind evenly, in air atmosphere behind 550 ℃ of roasting 5 h, obtain ceria can keep cube fluorite structure, nickel oxide is dispersed in the cerium ni compound oxide catalysis material on the ceria well.
Through comparing with pure ceria cell parameter, find that variation has taken place the cell parameter of cerium ni compound oxide, this is because Ni
2+Got into CeO
2Lattice replaces portion C e
4+Due to.In addition, transmission electron microscope and N
2The adsorption desorption result shows that there is the double-hole structure in the cerium ni compound oxide of preparation.Compare with the prepared by other catalyst, the cerium Raney nickel of solid phase method preparation has bigger specific area and reactivity.
The preparation method's that the present invention adopted advantage:
1. preparation process does not relate to solvent, can avoid the loss of species effectively;
2. method is simple and efficient, but mass preparation;
3. energy consumption is low, pollutes few;
4. specific area is big.
Description of drawings
Fig. 1 is the XRD result of the cerium ni compound oxide catalyst of different nickel cerium ratios.It is 0,1%, 5%, 10%, 20% sample that a, b, c, d, e represent the nickel molar content respectively.By figure can, solid phase method can realize well that NiO is at CeO
2On dispersion.
Fig. 2 is (A) N of the cerium ni compound oxide catalyst of different nickel cerium ratios
2Adsorption desorption thermoisopleth and (B) graph of pore diameter distribution.It is 0,1%, 5%, 10%, 20% sample that a, b, c, d, e represent the nickel molar content respectively.Can know that by figure all samples all has meso-hole structure.
Fig. 3 is the TEM results of representative cerium ni compound oxide catalyst (nickel molar content 20%).Can know that by figure except having the meso-hole structure of accumulation, the nickel cerium catalyst also has very little interior living hole.
Fig. 4 prepares the NO+CO reaction result of cerium ni compound oxide catalyst for distinct methods, and wherein A is the NO conversion ratio, and B is N
2Selectivity.A, b, c represent the cerium ni compound oxide catalyst of the 10%Ni molar content of solid phase method, coprecipitation and immersion process for preparing respectively.
The practical implementation method
Accurately take by weighing the cerous nitrate of 5 part of 4.34 gram and accurately take by weighing 0,0.029,0.153,0.323 and 0.727 gram nickel nitrate respectively; Every part of cerous nitrate is placed mortar with every part of nickel nitrate respectively; Be transferred in the crucible after grinding 10 min, under the air atmosphere in 550
oCooling naturally can obtain cerium ni compound oxide catalysis material behind C roasting 5 h.
The XRD of sample is characterized on Philips X ' the pert X-ray diffractometer and carries out, and its result sees Fig. 1.TEM characterize be with sample dispersion in ethanol, sonicated a period of time is placed on the copper mesh observes, used instrument is JEM-2100.N
2Adsorption desorption is characterized on Micromeritics ASAP-2020 type specific surface and the pore size determination appearance and carries out, and the result sees table 1.
The NO+CO reactivity evaluation of the cerium Raney nickel that distinct methods obtains is carried out on anti-in that fixed bed is little.Quartzy microreactor, catalyst amount 50 mg, the volume of reaction gas is formed: CO 5%, NO 2.5 %, He 92.5 %, overall flow rate are 10 mL/min, corresponding air speed is 9000 mLg
-1H
-1Product (separates NO, N through 13X with the 5A molecular sieve
2With CO) and Paropak Q (separate N
2O and CO
2) separate and then detect with thermal conductivity detector (TCD).The NO conversion ratio and the N of catalyst
2Selectivity is calculated by following formula:
Table 1 distinct methods prepares the specific area of cerium ni compound oxide catalyst
| ? | Specific area (m 2 g -1) |
| 10NiO-CeO 2(solid phase method) | 107.3 |
| 10NiO-CeO 2(coprecipitation) | 71.8 |
| 10NiO-CeO 2(infusion process) | 44.8 |
Claims (1)
1. the preparation method of a cerium ni compound oxide catalysis material; It is that nickel nitrate and cerous nitrate are mixed; Nickel nitrate with the ratio of the amount of substance of cerous nitrate is: 1:99-1:4 grinds evenly; In air atmosphere behind 550 ℃ of roasting 5 h, obtain ceria can keep cube fluorite structure, nickel oxide is dispersed in the cerium ni compound oxide catalysis material on the ceria well.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007979A (en) * | 2012-12-14 | 2013-04-03 | 南京大学 | Supported copper-cerium catalyst for selective oxidation of CO and preparation method of supported copper-cerium catalyst |
| CN105080537A (en) * | 2015-07-21 | 2015-11-25 | 中国科学院福建物质结构研究所 | Non-precious metal catalyst for CO oxidative dehydrogenation and preparation method for non-precious metal catalyst |
| CN113617380A (en) * | 2021-08-17 | 2021-11-09 | 安徽工业大学 | Preparation method of HZSM-5 molecular sieve modified high-performance cerium-based denitration catalyst |
| CN114522691A (en) * | 2022-02-21 | 2022-05-24 | 福州大学 | Preparation method of composite metal oxide for organic sulfur catalytic hydrolysis |
| CN115445627A (en) * | 2022-09-29 | 2022-12-09 | 武汉工程大学 | Cerium-nickel-copper composite oxide denitration catalyst and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791568A (en) * | 2010-03-18 | 2010-08-04 | 南京大学 | Preparation method of thermostable load-type nanometer metal catalyst |
-
2011
- 2011-11-07 CN CN2011103474951A patent/CN102500386A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791568A (en) * | 2010-03-18 | 2010-08-04 | 南京大学 | Preparation method of thermostable load-type nanometer metal catalyst |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007979A (en) * | 2012-12-14 | 2013-04-03 | 南京大学 | Supported copper-cerium catalyst for selective oxidation of CO and preparation method of supported copper-cerium catalyst |
| CN105080537A (en) * | 2015-07-21 | 2015-11-25 | 中国科学院福建物质结构研究所 | Non-precious metal catalyst for CO oxidative dehydrogenation and preparation method for non-precious metal catalyst |
| CN113617380A (en) * | 2021-08-17 | 2021-11-09 | 安徽工业大学 | Preparation method of HZSM-5 molecular sieve modified high-performance cerium-based denitration catalyst |
| CN114522691A (en) * | 2022-02-21 | 2022-05-24 | 福州大学 | Preparation method of composite metal oxide for organic sulfur catalytic hydrolysis |
| CN115445627A (en) * | 2022-09-29 | 2022-12-09 | 武汉工程大学 | Cerium-nickel-copper composite oxide denitration catalyst and preparation method and application thereof |
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Application publication date: 20120620 |