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CN1626437A - Method for preparing series of solid solution of metal oxide through carbamide combustion method - Google Patents

Method for preparing series of solid solution of metal oxide through carbamide combustion method Download PDF

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CN1626437A
CN1626437A CN 200310117394 CN200310117394A CN1626437A CN 1626437 A CN1626437 A CN 1626437A CN 200310117394 CN200310117394 CN 200310117394 CN 200310117394 A CN200310117394 A CN 200310117394A CN 1626437 A CN1626437 A CN 1626437A
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mole number
urea
nitrate
combustion
solid solution
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CN1247449C (en
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季生福
李成岳
雷志刚
陈标华
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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Abstract

本发明用尿素燃烧法制备系列金属氧化物固溶体的方法，该方法是用尿素燃烧法将硝酸盐与尿素按一定摩尔数的质量充分混合均匀后燃烧制成氧化物固溶体固体粉末。采用Ce与La、Ce与Zr、Ce与Ni、La与Al和Fe、La与Fe和Mg或Zn与Co的硝酸盐，得到Ce1－xLaxO2－x/2(0.1≤X≤0.9)、Ce1－xZrxO2(0.1≤X≤0.9)、Ce1－xNixO2(0.1≤X≤0.5)、LaAl1－xFexO3 (0.1≤X≤0.9)、LaFe1－xMgxO3 (0.1≤X≤0.5)、ZnxCo1－xCo2O4 (0.1≤X≤0.9)等一系列的金属氧化物固溶体，可以用于催化剂或催化剂载体。The invention uses a urea combustion method to prepare a series of metal oxide solid solutions. The method uses the urea combustion method to fully mix nitrate and urea according to a certain molar mass, and then combusts to form oxide solid solution solid powder. Using nitrates of Ce and La, Ce and Zr, Ce and Ni, La and Al and Fe, La and Fe and Mg or Zn and Co, Ce 1－x La x O 2－x/2 (0.1≤X≤ 0.9), Ce 1－x Zr x O 2 (0.1≤X≤0.9), Ce 1－x Ni x O 2 (0.1≤X≤0.5), LaAl 1－x Fe x O 3 (0.1≤X≤0.9) , LaFe 1－x Mg x O 3 (0.1≤X≤0.5), Zn x Co 1－x Co 2 O 4 (0.1≤X≤0.9) and a series of metal oxide solid solutions, which can be used as catalysts or catalyst supports .

Description

The method that is equipped with the series metal oxide solid solution with the burning urea legal system
Technical field
The present invention relates to a kind of method for preparing metal oxide solid solution, particularly prepare the method for highly purified series metal oxide solid solution with the burning urea method.This type of metal oxide solid solution can be used for catalyzer or support of the catalyst.
Background technology
Metal oxide solid solution has been widely used in catalyzer or support of the catalyst at catalytic field.Pickling process, coprecipitation method or sol-gel method are adopted in the preparation of traditional metal oxide solid solution mostly.For example: M.F.Wilkes etc. are at " Catalytic studies on ceria lanthana solidsolutions I.Oxidation of methane " (Journal of Catalysis, 2003, Vol.219 pp.286-294) has reported with coprecipitation method and has prepared Ce 1-xLa xO 2-x/2(X=0.1-0.9) sosoloid, this sosoloid have good methyl hydride catalyzed oxidation susceptibility and CO catalytic oxidation performance; A.Solinas etc. are at " Preparation, characterization and activity of CeO 2-ZrO 2Catalysts foralcohol dehydration " (Journal of Molecular Catalysis A, 2003, Vol.204-205 pp.629-635) has reported with sol-gel method and has prepared CeO 2-ZrO 2(CeO 2Content from 25 to 75%) sosoloid, this sosoloid have good primary isoamyl alcohol catalysis dehydrogenation performance; W.Shan etc. are at " Reduction property and catalytic activity of Ce 1-xNi xO 2Mixedoxide catalysts for CH 4Oxidation " (Applied Catalysis A, 2003, Vol.246 PP.1-9) has reported respectively and has prepared Ce with pickling process, coprecipitation method, sol-gel method 1-xNi xO 2(X=0.05-0.5) sosoloid, and compared the methyl hydride catalyzed oxidation susceptibility of the sosoloid of different methods preparation, find Ce 0.7Ni 0.3O 2Has good catalytic performance; P.Ciambelli etc. are at " CO oxidationand methane combustion on LaAl 1-xFe xO 3Perovskite solid solutions " (AppliedCatalysis B, 2002, Vol.37 is pp.231-241) with " AFeO 3(A=La, Nd, Sm) andLaFe 1-xMg xO 3Perovskite as methane combustion and CO oxidationcatalysts:structural, redox and catalytic properties " (Applied Catalysis B; 2001, Vol.29 pp.239-250) have reported with sol-gel method and have prepared LaAl 1-xFe xO 3(0≤X≤1) sosoloid and LaFe 1-xMg xO 3(X=0.1-0.5) sosoloid, and these sosoloid have good methane and CO catalytic combustion properties; L.Yan etc. are at " Excellent catalyticperformance of Zn xCo 1-xCo 2O 4Spinel catalysts for the decompositon ofnitrous oxide " (Catalysis Communications, 2003, Vol.4 pp.505-509) has reported with coprecipitation method and has prepared Zn xCo 1-xCo 2O 4(X=0-0.98) sosoloid, this sosoloid has good N 2O catalytic decomposition performance etc.
Yet among the preparation method of these metal oxide solid solutions, during immersion process for preparing, impregnated component concentration is lower because impregnated component concentration height what generate is mixed oxide compound, can not get pure sosoloid.When coprecipitation method and sol-gel method prepare, need precipitation or gelling, processes such as washing, multiple times of filtration repeatedly, concerning scale operation, have shortcomings such as operating procedure complexity, the production cycle is long, energy consumption is big.
Inventor Ji Shengfu etc. are at " Catalytic combustion of methane overcobalt-magnesium oxide solid solution catalysts " (Catalysis Letters, 2001Vol.75, pp.65-71) reported with the burning urea legal system and be equipped with the lower Co of Co content xMg 1-xO (X=0.05-0.20) sosoloid, find that this sosoloid has good methane catalytic combustion performance, the method of CoMgO catalyzer with the sosoloid preparation disclosed in this paper, with Xiao Suangu, magnesium nitrate preparation, urea is added in by a certain percentage the cobalt and the salt of magnesium, in 650～850 ℃ of burnings preparation in 10～30 minutes, still unexposed detailed preparation method.Recently, G.Avgouropoulos etc. is at " Selective CO oxidation over CuO-CeO 2Catalysts prepared via theurea-nitrate combustion method " (Applied Catalysis A, 2003, Vol.244 PP.155-167) has prepared CuO-CeO with the burning urea method 2(Cu/ (Cu+Ce)=0.1-0.2) sosoloid finds that this sosoloid has good CO selective oxidation catalytic performance.In addition, prepare other metal oxide solid solution, do not appear in the newspapers as yet with the burning urea method.
From existing research as can be seen, the burning urea legal system is equipped with oxide solid solution and prepares oxide solid solution with traditional pickling process, coprecipitation method or sol-gel method and compare, and biggest advantage is that simple, the required preparation time of operating procedure is short, energy consumption is low.Moment produces a large amount of N during simultaneously, owing to burning urea 2And CO 2Gas make that the sosoloid specific surface area and the pore volume that generate are bigger, thereby catalytic performance is better.
Summary of the invention
The object of the present invention is to provide a kind of urea of using cheapness as incendiary material, prepare the method for a series of multiple metal oxide solid solution simply, easily and quickly.This method is particularly suitable for large-scale industrialization production.
The present invention is equipped with the method for series metal oxide solid solution with the burning urea legal system, be with the even afterfire of quality thorough mixing of nitrate and urea with the burning urea method by certain mole number, and cooling naturally behind the maintenance certain hour, promptly can be made into the oxide solid solution pressed powder.Technology of the present invention is characterized in that: use two or three nitrate, that is: the nitrate of Ce and La, Ce and Zr, Ce and Ni, La and Al and Fe, La and Fe and Mg or Zn and Co, the mole number of incendiary material urea is 3～5 times of mole number sum of used nitrate, and temperature of combustion is 650～900 ℃; Hold-time obtains a series of metal oxide solid solution at 10～60min.
Nitrate of the present invention Ce (NO 3) 36H 2O and La (NO 3) 35H 2O; The mol ratio of Ce/ (Ce+La) is 1～9; The mole number of urea is Ce and La mole number sum 3～5 times; Temperature of combustion is 800～900 ℃; Hold-time is at 20～50 (min); Obtain solid-solution powder Ce 1-xLa xO 2-x/2(0.1≤X≤0.9).
Nitrate of the present invention Ce (NO 3) 36H 2O and Zr (NO 3) 45H 2O; The mol ratio of Ce/ (Ce+Zr) is 1～9; The mole number of urea is Ce and Zr mole number sum 3～5 times; Temperature of combustion is 650～800 ℃; Hold-time is at 10～60 (min); Obtain solid-solution powder Ce 1-xZr xO 2(0.1≤X≤0.9).
Nitrate of the present invention Ce (NO 3) 36H 2O and Ni (NO 3) 26H 2O; The mol ratio of Ce/ (Ce+Ni) is 1～5; The mole number of urea is Ce and Ni mole number sum 3～5 times; Temperature of combustion is 650～750 ℃; Hold-time is at 20～55 (min); Obtain solid-solution powder Ce 1-xNi xO 2(0.1≤X≤0.5).
Nitrate of the present invention La (NO 3) 35H 2O, Al (NO 3) 39H 2O and Fe (NO 3) 39H 2O; The mole number of La is the mole number sum of Al and Fe; The mol ratio of Al/ (Al+Fe) is 1～9; The mole number of urea is La, Al and Fe mole number sum 3～5 times; Temperature of combustion is 800～900 ℃; Hold-time is at 10～35 (min); Obtain solid-solution powder LaAl 1-xFe xO 3(0.1≤X≤0.9)
Nitrate of the present invention La (NO 3) 35H 2O, Fe (NO 3) 39H 2O and Mg (NO 3) 26H 2O; The mole number of La is the mole number sum of Fe and Mg; The mol ratio of Fe/ (Fe+Mg) is 1～5; The mole number of urea is La, Fe and Mg mole number sum 3～5 times; Temperature of combustion is 800～900 ℃; Hold-time is at 20～45 (min); Obtain solid-solution powder LaFe 1-xMg xO 3(0.1≤X≤0.5).
Nitrate of the present invention Zn (NO 3) 26H 2O and Co (NO 3) 26H 2O; The mol ratio of Zn/ (Zn+Co) is 1～9; The mole number of urea is Zn and Co mole number sum 3～5 times; Temperature of combustion is 650～750 ℃; Hold-time is at 10～30 (min); Obtain solid-solution powder Zn xCo 1-xCo 2O 4(0.1≤X≤0.9).
Operation steps of the present invention is as follows: when the burning urea legal system is equipped with oxide solid solution, by stoichiometric ratio take by weighing a certain amount of, contain crystal water, analytically pure metal nitrate and analytically pure urea, after at room temperature abundant ground and mixed is even, transfer in crucible or the quartz boat, directly put into the constant temperature High Temperature Furnaces Heating Apparatus that preestablishes temperature of combustion and carry out combustion reactions, and keep the predefined hold-time, naturally cooling promptly obtains corresponding metal oxide sosoloid pressed powder then.
Be equipped with in the oxide solid solution in the burning urea legal system, the metal content of some oxide solid solution can not be too high, as Ce 1-xNi xO 2Sosoloid, if the content of Ni is greater than 50 (mol) %, that obtain will be Ce 1-xNi xO 2The mixture of sosoloid and NiO is not pure Ce 1-xNi xO 2Sosoloid.The amount of incendiary material urea can not be very little, otherwise, generation be mixture, be not pure sosoloid; And the amount of incendiary material urea is too much, though what generate is pure sosoloid, and sosoloid structural the same substantially, this is a kind of waste to incendiary material urea.Therefore, the amount of incendiary material urea is doubly more suitable with the 3-5 of the mole number of used metal nitrate.For temperature of combustion, different oxide solid solutions has own suitable temperature range, and temperature of combustion is low excessively, and what obtain will be sosoloid and single metal hopcalite, not be pure sosoloid; The too high structure properties to metal oxide solid solution of temperature of combustion does not have big variation.
Coprecipitation method prepares Ce 1-xZr xO 2During sosoloid, the cerous nitrate and the zirconium nitrate aqueous solution that at first with concentration are 0.2M are even, then under agitation to the certain density ammoniacal liquor of mixed solution and dripping up to precipitation fully (the pH value is about 10), filter, the filter cake deionized water wash refilters, washs to neutral (repeating approximately to operate 5 times), through about 15 hours of 100 ℃ of dryings, at last, 650 ℃ of roastings 4 hours, can obtain Ce 1-xZr xO 2Sosoloid.
Description of drawings
Fig. 1～Fig. 6 is respectively the X-ray powder diffraction pattern (XRD) of 18 oxide solid solutions of 6 series preparing of the present invention.
Fig. 1 is the X-ray powder diffraction pattern (XRD) of the oxide solid solution of embodiment 1～3.(a) and (b) among the figure, (c) are respectively the XRD spectra of embodiment 1,2,3.
Fig. 2 is the X-ray powder diffraction pattern (XRD) of the oxide solid solution of embodiment 4～6.(a) and (b) among the figure, (c) are respectively the XRD spectra of embodiment 4,5,6.
Fig. 3 is the X-ray powder diffraction pattern (XRD) of the oxide solid solution of embodiment 7～9.(a) and (b) among the figure, (c) are respectively the XRD spectra of embodiment 7,8,9.
Fig. 4 is the X-ray powder diffraction pattern (XRD) of the oxide solid solution of embodiment 10～12.(a) and (b) among the figure, (c) are respectively the XRD spectra of embodiment 10,11,12.
Fig. 5 is the X-ray powder diffraction pattern (XRD) of the oxide solid solution of embodiment 13～15.(a) and (b) among the figure, (c) are respectively the XRD spectra of embodiment 13,14,15.
Fig. 6 is the X-ray powder diffraction pattern (XRD) of the oxide solid solution of embodiment 16～18.(a) and (b) among the figure, (c) are respectively the XRD spectra of embodiment 16,17,18.
The crystal phase structure of the oxide solid solution of the present invention's preparation is recorded by Rigaku D/MAX 2500VB2+/PC type X-ray powder diffraction instrument.By the X-ray powder diffraction pattern of the oxide solid solution of Fig. 1～Fig. 6 as can be known the oxide solid solution of the present invention's preparation be purified pressed powder.
As known from Table 2, experiment has prepared Ce with coprecipitation method as a comparison 1-xZr xO 2(0.1≤X≤0.9) sosoloid, and with the Ce of burning urea method preparation 1-xZr xO 2(0.1≤X≤0.9) sosoloid has carried out the mensuration in specific surface, pore volume, aperture (by Micrometrics ASAP 2010 type specific surface determinator N 2Absorption method records).By contrast as can be seen, the sosoloid of burning urea method preparation has bigger specific surface area and pore volume than the sosoloid of coprecipitation method preparation.
The metal oxide solid solution of 6 kinds of series of the present invention's preparation is the metal oxide solid solution of not open at present report with the preparation of burning urea method, compares with existing traditional pickling process, coprecipitation method or sol-gel method, and following advantage is arranged:
1. it is simple to be equipped with the operating procedure of oxide solid solution with this legal system, and preparation cost is low, can be mass-produced.
2. because the multiple metal oxide solid solution among the present invention is the nitrate of respective metal and the uniform mixture of the urea thorough mixing formation that at high temperature deflagrates, therefore, the specific surface area and the pore volume of its oxide solid solution are bigger.
3. be equipped with oxide solid solution with this legal system and be difficult for introducing other material, therefore, the purity of metal oxide solid solution is very high.
Embodiment
The processing condition of the embodiment of 18 oxide solid solutions of 6 series of the present invention (embodiment 1～embodiment 18) are listed in the table 1.
Embodiment 1～embodiment 3 is preparation Ce 1-xLa xO 2-x/2The example of (0.1≤X≤0.9) sosoloid.
Embodiment 4～embodiment 6 is preparation Ce 1-xZr xO 2The example of (0.1≤X≤0.9) sosoloid.
Embodiment 7～embodiment 9 is preparation Ce 1-xNi xO 2The example of (0.1≤X≤0.5) sosoloid.
Embodiment 10～embodiment 12 is preparation LaAl 1-xFe xO 3The example of (0.1≤X≤0.9) sosoloid.
Embodiment 13～embodiment 15 is preparation LaFe 1-xMg xO 3The example of (0.1≤X≤0.5) sosoloid.
Embodiment 16～embodiment 18 is preparation Zn xCo 1-xCo 2O 4The example of (0.1≤X≤0.9) sosoloid.
Comparative Examples 1 is the Ce with the coprecipitation method preparation 0.9Zr 0.1O 2Specific surface area, pore volume, mean pore size.
Comparative Examples 2 is the Ce with the coprecipitation method preparation 0.5Zr 0.5O 2Specific surface area, pore volume, mean pore size.
Comparative Examples 3 is the Ce with the coprecipitation method preparation 0.1Zr 0.9O 2Specific surface area, pore volume, mean pore size.
The Ce for preparing respectively by embodiment 4,5,6 1-xZr xO 2Specific surface area, pore volume and mean pore size (N that sosoloid is measured 2Determination of adsorption method) result with list in the table 2.Comparative Examples 1～3rd is with the Ce of coprecipitation method preparation 1-xZr xO 2Specific surface area, pore volume, the mean pore size of (0.1≤X≤0.9) sosoloid are also listed in the table 2.The sosoloid of burning urea method preparation has bigger specific surface area and pore volume than the sosoloid of coprecipitation method preparation as can be seen from Table 2.
Table 1
The urea urea of real metal nitrate nitric acid nitrate urea and burning keep sosoloid
Execute salt the nitrate temperature-time that rubs of molar mass
Molecular formula
The mole (min) of your number of example total mass number (g)
(℃)
(g) (Mol) (Mol) compares
1 Ce(NO 3) 3
7.82 0.018
6H 2O
4.80 0.08 4 900 20 Ce 0.9La 0.1O 1.95
La(NO 3) 3
0.83 0.002
5H 2O
2 Ce(NO 3) 3
4.34 0.010
6H 2O
6.01 0.10 5 850 35 Ce 0.5La 0.5O 1.75
La(NO 3) 3
4.15 0.010
5H 2O
3 Ce(NO 3) 3
0.87 0.002
6H 2O
3.60 0.06 3 800 50 Ce 0.1La 0.9O 1.55
La(NO 3) 3
7.47 0.018
5H 2O
4 Ce(NO 3) 3
7.82 0.018
6H 2O
6.01 0.10 5 800 10 Ce 0.9Zr 0.1O 2
Zr(NO 3) 4
0.86 0.002
5H 2O
5 Ce(NO 3) 3
4.34 0.010
6H 2O
3.60 0.06 3 700 30 Ce 0.5Zr 0.5O 2
Zr(NO 3) 4
4.29 0.010
5H 2O
6 Ce(NO 3) 3
0.87 0.002
6H 2O
4.80 0.08 4 650 60 Ce 0.1Zr 0.9O 2
Zr(NO 3) 4
7.73 0.018
5H 2O
7 Ce(NO 3) 3
7.82 0.018
6H 2O
3.60 0.06 3 750 20 Ce 0.9Ni 0.1O 2
Ni(NO 3) 2
0.58 0.002
6H 2O
8 Ce(NO 3) 3
6.08 0.014
6H 2O
4.80 0.08 4 700 35 Ce 0.7Ni 0.3O 2
Ni(NO 3) 2
1.74 0.006
6H 2O
9 Ce(NO 3) 3
4.34 0.010
6H 2O
6.01 0.10 5 650 55 Ce 0.5Ni 0.5O 2
Ni(NO 3) 2
2.91 0.010
6H 2O
10 La(NO 3) 3
8.30 0.02 9.61 0.16 4 900 10 LaAl 0.9Fe 0.1O 3
5H 2O
Al(NO 3) 3
6.75 0.018
9H 2O
Fe(NO 3) 3
0.81 0.002
9H 2O
11 La(NO 3) 3
8.30 0.020
5H 2O
Al(NO 3) 3
3.75 0.010 12.01 0.20 5 850 25 LaAl 0.5Fe 0.5O 3
9H 2O
Fe(NO 3) 3
4.04 0.010
9H 2O
12 La(NO 3) 3
8.30 0.02
5H 2O
Al(NO 3) 3
0.75 0.002 7.21 0.12 3 800 35 LaAl 0.1Fe 0.9O 3
9H 2O
Fe(NO 3) 3
7.27 0.018
9H 2O
13 La(NO 3) 3
8.30 0.02
5H 2O
Fe(NO 3) 3
7.27 0.018 12.01 0.20 5 850 30 LaFe 0.9Mg 0.1O 3
9H 2O
Mg(NO 3) 2
0.51 0.002
6H 2O
14 La(NO 3) 3
8.30 0.020
5H 2O
Fe(NO 3) 3
5.66 0.014 9.61 0.16 4 800 45 LaFe 0.7Mg 0.3O 3
9H 2O
Mg(NO 3) 2
1.54 0.006
6H 2O
15 La(NO 3) 3
8.30 0.02
5H 2O
Fe(NO 3) 3
4.04 0.010 7.21 0.12 3 900 20 LaFe 0.5Mg 0.5O 3
9H 2O
Mg(NO 3) 2
2.56 0.010
6H 2O
16 Zn(NO 3) 2
0.59 0.002
6H 2O
7.21 0.12 3 750 10 Zn 0.1Co 0.9Co 2O 4
Co(NO 3) 2
11.06 0.038
6H 2O
17 Zn(NO 3) 2
2.97 0.010
6H 2O
9.61 0.16 4 700 25 Zn 0.5Co 0.5Co 2O 4
Co(NO 3) 2
8.73 0.030
6H 2O
18 Zn(NO 3) 2
5.35 0.018
6H 2O
12.01 0.20 5 650 30 Zn 0.9Co 0.1Co 2O 4
Co(NO 3) 2
6.40 0.022
6H 2O
Table 2
The molecular formula specific surface area pore volume mean pore size of preparation method's sosoloid
(m 2g -1) (cm 3g -1) (nm)
Embodiment 4 Ce 0.9Zr 0.1O 225.3 0.0554 8.75
Embodiment 5 Ce 0.5Zr 0.5O 237.2 0.0610 6.57
Embodiment 6 Ce 0.1Zr 0.9O 214.0 0.0194 5.54
Comparative Examples 1 Ce 0.9Zr 0.1O 211.8 0.0315 9.21
Comparative Examples 2 Ce 0.5Zr 0.5O 222.9 0.0493 7.82
Comparative Examples 3 Ce 0.1Zr 0.9O 26.5 0.0102 6.19

Claims (7)

1, a kind of method that is equipped with the series metal oxide solid solution with the burning urea legal system, with the even afterfire of quality thorough mixing of nitrate and urea by certain mole number, and cooling naturally after certain hold-time, promptly can be made into the oxide solid solution pressed powder, it is characterized in that: use two or three nitrate, that is: the nitrate of Ce and La, Ce and Zr, Ce and Ni, La and Al and Fe, La and Fe and Mg or Zn and Co, the mole number of incendiary material urea is 3～5 times of mole number sum of used nitrate, and temperature of combustion is 650～900 ℃; Hold-time obtains a series of metal oxide solid solution at 10～60min.
2, method according to claim 1 is characterized in that: nitrate Ce (NO 3) 36H 2O and La (NO 3) 35H 2O; The mol ratio of Ce/ (Ce+La) is 1～9; The mole number of urea is Ce and La mole number sum 3～5 times; Temperature of combustion is 800～900 ℃; Hold-time is at 20～50 (min); Obtain solid-solution powder Ce 1-xLa xO 2-x/2(0.1≤X≤0.9).
3, method according to claim 1 is characterized in that: nitrate Ce (NO 3) 36H 2O and Zr (NO 3) 45H 2O; The mol ratio of Ce/ (Ce+Zr) is 1～9; The mole number of urea is Ce and Zr mole number sum 3～5 times; Temperature of combustion is 650～800 ℃; Hold-time is at 10～60 (min); Obtain solid-solution powder Ce 1-xZr xO 2(0.1≤X≤0.9).
4, method according to claim 1 is characterized in that: nitrate Ce (NO 3) 36H 2O and Ni (NO 3) 26H 2O; The mol ratio of Ce/ (Ce+Ni) is 1～5; The mole number of urea is Ce and Ni mole number sum 3～5 times; Temperature of combustion is 650～750 ℃; Hold-time is at 20～55 (min); Obtain solid-solution powder Ce 1-xNi xO 2(0.1≤X≤0.5).
5, method according to claim 1 is characterized in that: nitrate La (NO 3) 35H 2O, Al (NO 3) 39H 2O and Fe (NO 3) 39H 2O; The mole number of La is the mole number sum of Al and Fe; The mol ratio of Al/ (Al+Fe) is 1～9; The mole number of urea is La, Al and Fe mole number sum 3～5 times; Temperature of combustion is 800～900 ℃; Hold-time is at 10～35 (min); Obtain solid-solution powder LaAl 1-xFe xO 3(0.1≤X≤0.9).
6, method according to claim 1 is characterized in that: nitrate La (NO 3) 35H 2O, Fe (NO 3) 39H 2O and Mg (NO 3) 26H 2O; The mole number of La is the mole number sum of Fe and Mg; The mol ratio of Fe/ (Fe+Mg) is 1～5; The mole number of urea is La, Fe and Mg mole number sum 3～5 times; Temperature of combustion is 800～900 ℃; Hold-time is at 20～45 (min); Obtain solid-solution powder LaFe 1-xMg xO 3(0.1≤X≤0.5).
7, method according to claim 1 is characterized in that: nitrate Zn (NO 3) 26H 2O and Co (NO 3) 26H 2O; The mol ratio of Zn/ (Zn+Co) is 1～9; The mole number of urea is Zn and Co mole number sum 3～5 times; Temperature of combustion is 650～750 ℃; Hold-time is at 10～30 (min); Obtain solid-solution powder Zn xCo 1-xCo 2O 4(0.1≤X≤0.9).
CN 200310117394 2003-12-12 2003-12-12 Method for preparing series of solid solution of metal oxide through carbamide combustion method Expired - Fee Related CN1247449C (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101199932B (en) * 2006-12-13 2010-12-22 中国石油化工股份有限公司 Iron-based catalyst for ft synthesis and preparation thereof
CN103537288A (en) * 2013-10-25 2014-01-29 中国华能集团清洁能源技术研究院有限公司 Method for preparing methanation catalyst by adopting urea combustion method
CN103816890A (en) * 2014-02-24 2014-05-28 陕西师范大学 A kind of preparation method for CO Oxidation ethylbenzene dehydrogenation catalyst
CN104607173A (en) * 2015-01-19 2015-05-13 广西大学 Oxygen storage material and preparation method thereof
CN106582261A (en) * 2015-10-14 2017-04-26 中国石油化工股份有限公司 Deodorant for treatment of coking sewage pool stink, preparation method and application thereof
WO2019185608A1 (en) 2018-03-28 2019-10-03 Covestro Deutschland Ag Heterogeneous catalysts for the synthesis of carbamates

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101199932B (en) * 2006-12-13 2010-12-22 中国石油化工股份有限公司 Iron-based catalyst for ft synthesis and preparation thereof
CN103537288A (en) * 2013-10-25 2014-01-29 中国华能集团清洁能源技术研究院有限公司 Method for preparing methanation catalyst by adopting urea combustion method
CN103816890A (en) * 2014-02-24 2014-05-28 陕西师范大学 A kind of preparation method for CO Oxidation ethylbenzene dehydrogenation catalyst
CN103816890B (en) * 2014-02-24 2015-10-28 陕西师范大学 A kind of for CO 2the preparation method of oxidation catalyst for phenylethylene dehydrogenation
CN104607173A (en) * 2015-01-19 2015-05-13 广西大学 Oxygen storage material and preparation method thereof
CN106582261A (en) * 2015-10-14 2017-04-26 中国石油化工股份有限公司 Deodorant for treatment of coking sewage pool stink, preparation method and application thereof
WO2019185608A1 (en) 2018-03-28 2019-10-03 Covestro Deutschland Ag Heterogeneous catalysts for the synthesis of carbamates
US11406964B2 (en) 2018-03-28 2022-08-09 Covestro Intellectual Property Gmbh & Co. Kg Heterogeneous catalysts for the synthesis of carbamates

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