CN103626234B - Method for preparing magnesium manganese metal composite oxide by taking active magnesium oxide as raw material - Google Patents
Method for preparing magnesium manganese metal composite oxide by taking active magnesium oxide as raw material Download PDFInfo
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- CN103626234B CN103626234B CN201310665830.1A CN201310665830A CN103626234B CN 103626234 B CN103626234 B CN 103626234B CN 201310665830 A CN201310665830 A CN 201310665830A CN 103626234 B CN103626234 B CN 103626234B
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Abstract
The invention discloses a method for preparing magnesium manganese metal composite oxide by taking active magnesium oxide as a raw material, and relates to a method for preparing magnesium manganese metal composite oxide. The method comprises the following steps: firstly, preparing magnesium manganese metal composite oxide by taking active magnesium oxide and manganese chloride as raw materials; secondly, dissolving the active magnesium oxide in water, so as to form aquated magnesium oxide complex; thirdly, preparing the manganese chloride into aqueous solution with certain concentration, and dropwise adding the aqueous solution into aquated magnesium oxide complex solution; fourthly, performing suction filtration, cleaning, drying and calcining to emulsion, so as to obtain the magnesium manganese metal composite oxide. The method adopts the active magnesium oxide and manganese chloride as raw materials to prepare magnesium manganese metal composite oxide, adopts the copolymerization phenomenon of metal ion complex in aqueous solution to form metal ion aquated hydroxyl copolymer, has no additive, and is simple. The prepared magnesium manganese metal composite oxide not only has double metal centers served as catalyst or carrier for certain organic reaction, but also has paramagnetism.
Description
Technical field
The present invention relates to a kind of method preparing magnesium manganese composite oxide of metal, particularly relating to a kind of take activated magnesia as the method that magnesium manganese composite oxide of metal prepared by raw material.
Background technology
China is magnesium resource big country, and magnesite total reserves is 3,100,000,000 tons, accounts for more than 1/4th of world's total reserves, and high value added utilization magnesite becomes the emphasis of research.
Because manganese oxide and magnesium oxide can be used as catalyzer in a lot of reaction, and complex metal oxides has the many character being better than single metal oxide compound, obtain presoma magnesium manganese complex metal hydroxide with activated magnesia and Manganous chloride tetrahydrate for raw material reaction, after calcining, obtain magnesium manganese complex metal oxides.The magnesium manganese complex metal oxides obtained has bimetallic center, can be used as catalyzer or the carrier of some organic reflection, and wherein Mg can suppress the carrying out of side reaction in chemical reaction as alkali center.Cu in Cu and Supported CuO, as acid sites, can obtain because it has non-shared electron the carrying out that organic electronics promotes organic reaction.
Research finds, mangaic acid magnesium can be applied as sorbent material, and zinc manganate can as catalyst application.Other functional performances of exploitation mangaic acid magnesium, have development prospect undoubtedly.
Form spatial network shape metal hydroxy polymkeric substance according to the copolymerization phenomenon of bimetal ionic complex in the aqueous solution, it can be used as precursor power manganese magnesium complex metal oxides.The method is simple to operate, compared with additive method, remains initial native structure; Not high to equipment, technical requirements; Do not introduce other auxiliary agents, product purity is high; Cost is low; Because the OH – in solution discharges gradually, the therefore morphology controllable of products therefrom.
Summary of the invention
The object of the present invention is to provide a kind of take activated magnesia as the method that magnesium manganese composite oxide of metal prepared by raw material, the method utilizes metal ion match copolymerization phenomenon in the aqueous solution, prepare magnesium manganese composite oxide of metal, the magnesium manganese complex metal oxides prepared has bimetallic center, can be used as catalyzer or the carrier of some organic reaction, there is paramagnetism simultaneously.
The object of the invention is to be achieved through the following technical solutions:
Take activated magnesia as the method that magnesium manganese composite oxide of metal prepared by raw material, described method comprises the first step, is dissolved in the water by activated magnesia, forms aqua oxidation magnesium complex; Second step, is made into the aqueous solution by Manganous chloride tetrahydrate, is added drop-wise in hydrated magnesium complex solution; 3rd step, obtains magnesium manganese complex metal oxides by emulsion suction filtration, washing, dry rear calcining.
Described a kind of take activated magnesia as the method that magnesium manganese composite oxide of metal prepared by raw material, described magnesium manganese complex metal oxides has bimetallic center, as catalyzer or the carrier of organic reaction.
Described a kind of take activated magnesia as the method that magnesium manganese composite oxide of metal prepared by raw material, described magnesium manganese complex metal oxides has paramagnetism.
Advantage of the present invention and effect are:
1. the present invention propose a kind of with activated magnesia and Manganous chloride tetrahydrate for raw material, utilize the copolymerization phenomenon of metal ion match in the aqueous solution to prepare magnesium manganese composite oxide of metal, without any additive, method is simple, and cost is low.
2. prepare magnesium manganese complex metal oxides and have Mg2MnO4 and MgMn2O4.
3. the magnesium manganese complex metal oxides prepared has bimetallic center, can be used as catalyzer or the carrier of some organic reaction.
4. the magnesium manganese complex metal oxides prepared has paramagnetism.
Accompanying drawing explanation
Fig. 1 is the technology of the present invention route schematic diagram;
Fig. 2 is the SEM figure of molar product of the present invention than 1.3;
Fig. 3 is the SEM figure of molar product of the present invention than 1.7;
Fig. 4 is mol ratio of the present invention is the XRD figure that 1.3:1 reacts 3h product;
Fig. 5 is mol ratio of the present invention is the XRD figure that 1.7:1 reacts 3h product;
Fig. 6 is unit mass susceptibility χ
σwith foreign field Η Changing Pattern figure;
Fig. 7 is absorption of sample CO2 desorption curve figure;
Fig. 8 is sample adsorption NH3 desorption curve figure.
Embodiment
Below in conjunction with accompanying drawing illustrated embodiment, the invention will be further described.
The present invention for raw material with activated magnesia and Manganous chloride tetrahydrate, prepares magnesium manganese composite oxide of metal, utilizes the copolymerization phenomenon of metal ion match in the aqueous solution, without any additive.Emulsion suction filtration, washing, dry rear calcining are obtained magnesium manganese complex metal oxides.The magnesium manganese complex metal oxides prepared has bimetallic center, can be used as catalyzer or the carrier of some organic reaction.The magnesium manganese complex metal oxides prepared has paramagnetism.
Ultimate principle of the present invention: the water-soluble generation hydrated magnesium of magnesium oxide, generates hydroxyl magnesium ion then, the aobvious alkalescence of solution, under more polyhydroxyl ion existence condition, forms hydroxyl Hydrated Magnesium Ion title complex.
MgO+H2O→[Mg(OH)] ①
[Mg(OH)]+ + OH–→[Mg(OH)2]（aq） ②
[Mg(OH)2]（aq）+OH–→[Mg(OH)3]– ③
[Mg(OH)3]–+OH–→[Mg(OH)4]2– ④
[Mg(OH)4]2–+OH–→[Mg(OH)5]3– ⑤
[Mg(OH)5]3–+OH–→[Mg(OH)6]4– ⑥
And in manganese chloride solution, along with Manganous chloride tetrahydrate concentration increases, solution acidic increases, under reaching certain pH value condition, form hydroxyl hydration mn ion title complex or mangaic acid root MnO4-ion,
2Mn2+＋3OH–→Mn2(OH)3 + ⑦
Mn2+＋OH–→Mn(OH)+ ⑧
The acid-basicity of both utilizations is different, under certain proportion condition, when solution pH value is certain, forms magnesium manganese water and the hydroxyl polymeric body of spacial framework.
Technological method of the present invention: this project for raw material with activated magnesia and Manganous chloride tetrahydrate, utilizes the copolymerization phenomenon of metal ion match in the aqueous solution, prepares the emulsion of magnesium manganese copolymerization, after filtration washing drying, calcining obtains magnesium manganese complex metal oxides.
As seen from the figure, sample is magnesium manganese complex metal oxides, obtains obtaining mangaic acid magnesium MgMn2O4 when mixture M g2MnO4 and MgMn2O4, Mn/Mg mol ratio are 1.7:1 when Mn/Mg mol ratio is 1.3:1.
As seen from the figure, sample has paramagnetism, and when Mn/Mg mol ratio is 1:4, magnetic is the strongest.
As seen from the figure, the magnesium manganese complex metal oxides prepared has bimetallic center.
Embodiment 1:
(1) activated magnesia pre-treatment, puts into retort furnace and calcines 2h at 600 DEG C.After each activity recovery, can use 4 days, re-using after 4 days need first with above-mentioned steps activity recovery again.
(2) electronic scales takes magnesium oxide (MgO) 4g, pours into and is equipped with in the 250ml there-necked flask of 100ml water, stir under ultrasonic frequency 30HZ condition, temperature of reaction 50 DEG C, 60 minutes reaction times.
(3) electronic scales takes Manganous chloride tetrahydrate (MnCl2), is mixed with the manganese chloride solution of 1mol/L.The manganese chloride solution of 1mol/L is loaded in dropping funnel, dripping (reaction times mean value) speed with 3-4s/ drops in milk of magnesia, after dropwising, continues to stir, remain temperature of reaction 50 DEG C, measure the pH value of emulsion in whole process with PHS-3C acidometer.
(4) stop stirring, add 1000ml distilled water, emulsion is filtered, then use dehydrated alcohol repetitive scrubbing 2-3 time of about 100ml.Filter cake is put into vacuum drying oven 80 DEG C of dry 2-3h, obtain mangaic acid magnesium presoma.
(5) load in porcelain crucible by after the grinding of mangaic acid magnesium presoma, 700 DEG C of calcining 2h, obtain pressed powder.
Claims (1)
1. be the method that magnesium manganese composite oxide of metal prepared by raw material with activated magnesia, it is characterized in that, described method comprises the first step, is dissolved in the water by activated magnesia, forms aqua oxidation magnesium complex; Second step, is made into the aqueous solution by Manganous chloride tetrahydrate, is added drop-wise in hydrated magnesium complex solution; 3rd step, obtains magnesium manganese complex metal oxides by emulsion suction filtration, washing, dry rear calcining;
Described magnesium manganese complex metal oxides has bimetallic center, as catalyzer or the carrier of organic reaction;
Described magnesium manganese complex metal oxides has paramagnetism.
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| CN103626234B true CN103626234B (en) | 2015-05-27 |
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| CN105413692A (en) * | 2016-01-08 | 2016-03-23 | 沈阳化工大学 | Method for preparing magnesium cobalt metal compound oxide with active magnesium oxide as raw material |
| CN106540534A (en) * | 2016-12-08 | 2017-03-29 | 盐城工学院 | A kind of magnesium manganese composite oxide sulfur transfer additive and preparation method thereof |
| CN111573738A (en) * | 2020-05-25 | 2020-08-25 | 山东大学 | Pure cubic phase Mg2MnO4Spinel material and preparation method and application thereof |
| CN113753957B (en) * | 2021-10-13 | 2022-08-16 | 吉林大学 | MgMn 3 (OH) 6 Cl 2 Nano material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0623556A1 (en) * | 1993-04-02 | 1994-11-09 | Texaco Development Corporation | Hydrothermal synthesis of octahedral molecular sieve |
| CN103073063A (en) * | 2012-12-17 | 2013-05-01 | 沈阳化工大学 | Method for preparing nanometer magnesium ferrite through utilizing active magnesium oxide as raw material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0623556A1 (en) * | 1993-04-02 | 1994-11-09 | Texaco Development Corporation | Hydrothermal synthesis of octahedral molecular sieve |
| CN103073063A (en) * | 2012-12-17 | 2013-05-01 | 沈阳化工大学 | Method for preparing nanometer magnesium ferrite through utilizing active magnesium oxide as raw material |
Non-Patent Citations (1)
| Title |
|---|
| Synthesis of Binary Magnesium–Transition Metal Oxides via Inverse Coprecipitation;Shunsuke Yagi et al.;《Japanese Journal of Applied Physics》;20130117;第52卷;025501-1-6 * |
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