CN103657650A - Preparation method for Cu-rich magnesium copper metal composite oxide with magnesium oxide as raw material - Google Patents
Preparation method for Cu-rich magnesium copper metal composite oxide with magnesium oxide as raw material Download PDFInfo
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- CN103657650A CN103657650A CN201310660440.5A CN201310660440A CN103657650A CN 103657650 A CN103657650 A CN 103657650A CN 201310660440 A CN201310660440 A CN 201310660440A CN 103657650 A CN103657650 A CN 103657650A
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Abstract
The invention provides a preparation method for Cu-rich magnesium copper metal composite oxide with magnesium oxide as a raw material, which relates to a preparation method for Cu-rich magnesium copper metal composite oxide. The preparation method comprises the following steps: step 1, with active magnesium oxide and copper chloride as raw materials, preparing copper-rich magnesium copper metal oxide; step 2, dissolving active magnesium oxide in water so as to form a hydrated magnesium oxide complex; step 3, preparing an aqueous solution with certain concentration from copper chloride and adding the aqueous solution into an aqueous solution of the hydrated magnesium oxide complex drop by drop; and step 4, subjecting an obtained emulsion to filtration, washing and drying and then carrying out calcining so as to obtain the CuO-Cu4MgO5 magnesium copper composite metal oxide. According to the invention, active magnesium oxide and copper chloride are used as the raw materials to prepare the copper-rich magnesium copper composite oxide, a copolymer of metal ion water and a hydroxyl group is formed by using the phenomenon of copolymerization of metal ion complexes in an aqueous solution, no additive is added, and the method is simple; the prepared CuO-Cu4MgO5 magnesium copper composite metal oxide has duplex metal centers and can be used as a catalyst or carrier for a plurality of organic reactions.
Description
Technical field
The present invention relates to a kind of method of preparing rich copper type magnesium copper composite oxide of metal, particularly relate to and a kind ofly take magnesia and prepare the method for rich copper type magnesium copper composite oxide of metal as raw material.
Background technology
China is magnesium resource big country, and magnesite gross reserves is 3,100,000,000 tons, accounts for the more than 1/4th of world's gross reserves, and high value added utilization magnesite becomes the emphasis of research.
Because cupric oxide and magnesia can be used as catalyst in a lot of reactions, and composite metal oxide has the many character that is better than single metal oxide, take MgO and CuCl2 obtains presoma magnesium copper composite metal hydroxide as raw material reaction, the CuO-Cu4MgO5 catalyst that to obtain through XRD analysis molecular formula after calcining be Cu4MgO5, the magnesium copper composite metal oxide of preparation is the composite oxides with bimetallic center, the catalyst or the carrier that can be used as some organic reflection, wherein Mg can suppress the carrying out of side reaction in chemical reaction as alkali center.Cu in Cu4MgO5 catalyst and the Cu in Supported CuO, as acid centre, can obtain because it has not shared electron the carrying out that organic electronics promotes organic reaction.
According to the polymerism of bimetallic ion in the aqueous solution, form spatial network shape metal hydroxy polymer.The method is simple to operate, compares with additive method, has retained original natural structure; Not high to equipment, specification requirement; Do not introduce other auxiliary agents, product purity is high; Cost is low; Because the OH – in solution discharges gradually, so the pattern of products therefrom is controlled.
Summary of the invention
The object of the present invention is to provide and a kind ofly take magnesia and prepare the method for rich copper type magnesium copper composite oxide of metal as raw material, the method is utilized metal ion match copolymerization phenomenon in the aqueous solution, prepare rich copper type magnesium copper composite oxide of metal, the CuO-Cu4MgO5 magnesium copper composite metal oxide preparing has bimetallic center, can be used as catalyst or the carrier of some organic reaction.
The object of the invention is to be achieved through the following technical solutions:
The magnesia of take is prepared the method for rich copper type magnesium copper composite oxide of metal as raw material, and described method comprises the first step, take activated magnesia and copper chloride as raw material, prepares rich copper type magnesium copper composite oxide of metal; Second step, is dissolved in the water activated magnesia, forms aqua oxidation magnesium complex; The 3rd step, is made into the aqueous solution by copper chloride, is added drop-wise in hydrated magnesium complex solution, and the 4th step, obtains CuO-Cu4MgO5 magnesium copper composite metal oxide by emulsion suction filtration, washing, dry rear calcining.
Described take magnesia and prepare the method for rich copper type magnesium copper composite oxide of metal as raw material, described in the CuO-Cu4MgO5 magnesium copper composite metal oxide that obtains there is bimetallic center, as catalyst or the carrier of organic reaction.
Advantage of the present invention and effect are:
1. the present invention proposes that a kind of to take activated magnesia and copper chloride be raw material, utilizes the polymerism of metal ion in the aqueous solution to prepare rich copper type magnesium copper composite oxide of metal, and without any additive, method is simple, and cost is low.
2. prepare CuO-Cu4MgO5 magnesium copper composite metal oxide.
3. the CuO-Cu4MgO5 magnesium copper composite metal oxide preparing has bimetallic center, can be used as catalyst or the carrier of some organic reaction.。
Accompanying drawing explanation
Fig. 1 is the technology of the present invention route schematic diagram;
Fig. 2 is product SEM figure of the present invention;
Fig. 3 is product XRD figure of the present invention;
Fig. 4 is the peak area figure of the magnesium copper composite metal oxide CO absorption 2 that makes of differential responses thing proportioning of the present invention;
Fig. 5 is the peak area figure of the magnesium copper composite metal oxide absorption NH3 that makes of differential responses thing proportioning of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing illustrated embodiment, the invention will be further described.
It is raw material that activated magnesia and copper chloride are take in the present invention, prepares rich copper type magnesium copper 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 to CuO-Cu4MgO5 magnesium copper composite metal oxide.The CuO-Cu4MgO5 magnesium copper composite metal oxide preparing has bimetallic center, can be used as catalyst or the carrier of some organic reaction.
Basic principle of the present invention: the water-soluble generation hydrated magnesium of magnesia, then generate hydroxyl magnesium ion, the aobvious alkalescence of solution, under polyhydroxyl ion existence condition more, forms hydroxyl Hydrated Magnesium Ion 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 copper chloride solution, along with copper chloride concentration increases, solution acidic increases, reach under certain pH value condition, form hydroxyl hydration copper ion complex,
Cu2++ 4H2O→[Cu(H2O)4]2+ ⑦
Cu2++ 4OH–→[Cu(OH)4]2- ⑧
Utilize both Acidity of Aikalinitys different, under certain proportion condition, when solution pH value is certain, form magnesium copper water and the hydroxyl polymeric body of spacial framework.
Basic scheme of the present invention: the first step, activated magnesia is dissolved in the water, form aqua oxidation magnesium complex; With second step, copper chloride is made into the certain density aqueous solution, be added drop-wise in hydrated magnesium complex solution.The 3rd step, obtains CuO-Cu4MgO5 magnesium copper composite metal oxide by emulsion suction filtration, washing, dry rear calcining.
Technical method of the present invention: it is raw material that this project be take activated magnesia and copper chloride, utilize the polymerism of metal ion in the aqueous solution, prepare the emulsion of magnesium copper combined polymerization, after filtration washing is dry, calcining obtains CuO-Cu4MgO5 magnesium copper composite metal oxide.
Embodiment 1:
(1) activated magnesia pretreatment is put into Muffle furnace and is calcined 2h at 600 ℃.After each activity recovery, can use 4 days, after 4 days, re-use need be first with above-mentioned steps activity recovery again.
(2) the activated magnesia 4g taking after calcining adds in 250ml there-necked flask, in there-necked flask, adds 100ml distilled water, 50 ℃ of ultrasonic reaction 1h.
(3) measure 1mol/L copper chloride solution, dropwise add in magnesium oxide solution, drip and finish its pH value of rear survey, after pH value stabilization (about 1.5h), stop experiment.
(4) suction filtration, dry, under 800 ℃ of conditions, calcine, 2h, obtains product.
Claims (2)
1. the magnesia of take is prepared the method for rich copper type magnesium copper composite oxide of metal as raw material, it is characterized in that, described method comprises the first step, take activated magnesia and copper chloride as raw material, prepares rich copper type magnesium copper composite oxide of metal; Second step, is dissolved in the water activated magnesia, forms aqua oxidation magnesium complex; The 3rd step, is made into the aqueous solution by copper chloride, is added drop-wise in hydrated magnesium complex solution, and the 4th step, obtains CuO-Cu4MgO5 magnesium copper composite metal oxide by emulsion suction filtration, washing, dry rear calcining.
2. according to claim 1ly take magnesia and prepare the method for rich copper type magnesium copper composite oxide of metal as raw material, it is characterized in that, the described CuO-Cu4MgO5 magnesium copper composite metal oxide obtaining has bimetallic center, as catalyst or the carrier of organic reaction.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105413671A (en) * | 2015-11-11 | 2016-03-23 | 沈阳化工大学 | Method for preparing magnesium zinc metal composite oxide with active magnesium oxide as raw material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441381A (en) * | 2011-10-28 | 2012-05-09 | 昆山德泰新材料科技有限公司 | Catalyst produced by using copper oxide powder and production method thereof |
| 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 |
| CN103623822A (en) * | 2013-12-04 | 2014-03-12 | 沈阳化工大学 | Method for preparing copper-rich type metal compound oxide by using magnesium oxide as raw material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441381A (en) * | 2011-10-28 | 2012-05-09 | 昆山德泰新材料科技有限公司 | Catalyst produced by using copper oxide powder and production method thereof |
| 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 |
| CN103623822A (en) * | 2013-12-04 | 2014-03-12 | 沈阳化工大学 | Method for preparing copper-rich type metal compound oxide by using magnesium oxide as raw material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105413671A (en) * | 2015-11-11 | 2016-03-23 | 沈阳化工大学 | Method for preparing magnesium zinc metal composite oxide with active magnesium oxide as raw material |
| 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 |
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Application publication date: 20140326 |