CN105413692A - Method for preparing magnesium cobalt metal compound oxide with active magnesium oxide as raw material - Google Patents

Method for preparing magnesium cobalt metal compound oxide with active magnesium oxide as raw material Download PDF

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Publication number
CN105413692A
CN105413692A CN201510763917.1A CN201510763917A CN105413692A CN 105413692 A CN105413692 A CN 105413692A CN 201510763917 A CN201510763917 A CN 201510763917A CN 105413692 A CN105413692 A CN 105413692A
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China
Prior art keywords
magnesium
oxide
cobalt
metal compound
raw material
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CN201510763917.1A
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Inventor
王国胜
王迪
房安娜
杨鹤南
郎嘉朋
宁志高
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Shenyang University of Chemical Technology
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Shenyang University of Chemical Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/75—Cobalt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Catalysts (AREA)

Abstract

The invention provides a method for preparing a magnesium cobalt metal compound oxide with active magnesium oxide as the raw material and relates to a method for preparing metal compound oxides. The method includes the steps that 1, the active magnesium oxide and cobalt chloride serve as raw materials, and magnesium cobalt metal compound oxide is obtained; 2, the active magnesium oxide is dissolved in water, and a hydrated magnesium oxide complex is obtained; 3, the cobalt chloride is blended into an aqueous solution of certain concentration and dropwise added to a hydrated magnesium oxide complex solution; 4, emulsion is subjected to suction filtration, washing and drying and then calcined, and the Mg<2>CoO<4> and MgCo<2>O<4> magnesium cobalt metal compound oxide is obtained. According to the method, the active magnesium oxide and the cobalt chloride serve as the raw materials to prepare the magnesium cobalt metal compound oxide, the metal ion complex copolymerization phenomenon in the aqueous solution is utilized, metal ionized hydrated hydroxyl copolymer is formed, no additive exists, and the method is simple. The obtained Mg<2>CoO<4> and MgCo<2>O<4> magnesium cobalt metal compound oxide has double metal centers and can serve as a catalyst or a carrier of certain organic reactions.

Description

A kind of take activated magnesia as the method that magnesium cobalt composite oxide of metal prepared by raw material
Technical field
The present invention relates to a kind of method preparing composite oxide of metal, particularly relating to a kind of take activated magnesia as the method that magnesium cobalt composite oxide of metal prepared by raw material.
Background technology
The composite metal oxide that magnesium is relevant with transition metal all has good application background at catalytic field, as Al-Mg composite metal oxide, magnesium manganese composite metal oxide, magnesium iron composite metal oxide, copper cobalt composite metal oxide, copper-chromic composite metal oxide, copper iron composite metal oxide etc.Wherein most composite metal oxide has good application in solid propellant.As magnesium iron composite metal oxide, copper cobalt composite metal oxide, copper-chromic composite metal oxide, copper iron composite metal oxide to be used in solid propellant as burningrate catalyst time, obviously can reduce the pyrolysis temperature of AP, improve boron powder once with second-time burning efficiency, after carrying out further modification, coated process to catalyst, catalytic performance is got back and is further improved, and have also been obtained solution with the compatibility of end hydroxy butadiene in system.Composite metal oxide has stable crystal structure, good optics, electricity, magnetic performance, is important laser material, pyroelectricity material, piezoelectric and strong magnetic material etc., applies very extensive.For the aspect such as hydrocarbon reforming reaction of the burningrate catalyst of solid propellant, photocatalytic hydrogen production by water decomposition and petroleum chemical industry.Its distortion of lattice of adulterating mutually and causing, cause existing in the crystal grain of composite oxides more defects, activated centre showed increased, its combination property is often better than single oxide.Composite metal oxide also has very high oxidation-reduction quality, hydrogenolysis, isomerization, electro-catalysis isoreactivity, as a kind of new function material with characteristics such as air-sensitive, giant magnetoresistance, electrical conductances, have broad application prospects in information, the energy, electronics, metallurgy, chemical industry, biology and medicine and other fields.
Be the polynary complex oxide be composited by magnesium and one or more transition metal oxides containing magnesium compound transition metal oxide, it has better character than unit oxide in electricity, light, magnetic etc.Also there is good stability, corrosion-resistant, high temperature resistant, the character features such as high rigidity.In cobalt-based compound oxide, about the report of the bimetal composite oxide magnesium cobalt composite oxide of magnesia and cobalt oxide is little.Cobalt base oxide can be used for synthesis gas artificial oil or as auxiliary agent for the synthesis of low-carbon alcohols etc., what have real industrial application value prospect is the mixture that Co based compound or Co and other metal oxide are formed.The nanocatalyst of cobalt/cobalt oxide has good catalysis efficiency to N2O=N2+O2 decomposition reaction.The research of recent years finds: be cobalt oxide, cobalt hydroxide can significantly improve the performance of battery: the high-output power and the specific capacity that strengthen battery, increase the life-span during charge/discharge cycles of battery, reduce automatic discharging phenomenon and improve the additives for battery that overcharging resisting power etc. is excellent performance.It is also the research potential that tool is very large in the field such as magnetic material and electrode material in addition.。
In magnesium cobalt composite metal oxide, the interaction of Co and Mg is conducive to the activation of active sites, thus can improve the reaction condition such as catalytic performance, reduction reaction temperature.Cobalt oxide is a kind of common catalyst or catalyst carrier, in a lot of reaction, all demonstrate good catalytic performance.MgO activity position can suppress the carrying out of side reaction in reaction in the reaction.
China is magnesium resource big country, and magnesite gross reserves is 3,100,000,000 tons, accounts for more than 1/4th of world's gross reserves, and high value added utilization magnesite becomes the emphasis of research.
Because cobalt oxide and magnesia can be used as catalyst in a lot of reaction, and composite metal oxide has the many character being better than single metal oxide, with MgO and CoCl2 for raw material reaction obtains presoma magnesium cobalt complex metal hydroxide, obtain after calcining through XRD analysis molecular formula be Mg2CoO4 and MgCo2O4 catalyst, the magnesium cobalt composite metal oxide of preparation is the composite oxides with bimetallic center, can be used as catalyst or the carrier of some organic reflection, wherein Mg can suppress the carrying out of side reaction in chemical reaction as alkali center.Co in Mg2CoO4 and MgCo2O4 catalyst and the Co in load C oO, as acid centre, can obtain because it has non-shared electron the carrying out that organic electronics promotes organic reaction.
Spatial network shape metal hydroxy polymer is formed according to the polymerism of bimetallic ion in the aqueous solution.The method is simple to operate, compared with additive method, remains initial native structure; Not high to equipment, technical requirement; 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 cobalt composite oxide of metal prepared by raw material, and the method utilizes metal ion match copolymerization phenomenon in the aqueous solution, prepares magnesium cobalt composite oxide of metal.Mg2CoO4 and the MgCo2O4 magnesium cobalt composite metal oxide prepared 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:
Take activated magnesia as the method that magnesium cobalt composite oxide of metal prepared by raw material, described method comprises following process: the first step, with activated magnesia and cobalt chloride for raw material, prepares magnesium cobalt composite oxide of metal; Second step, is dissolved in the water activated magnesia, forms aqua oxidation magnesium complex; 3rd step, is made into the certain density aqueous solution by cobalt chloride, is added drop-wise in hydrated magnesium complex solution; 4th step, obtains Mg2CoO4 and MgCo2O4 magnesium cobalt composite metal oxide by emulsion suction filtration, washing, dry rear calcining;
Concrete preparation process is:
(1) activated magnesia pretreatment, puts into Muffle 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) taking the activated magnesia 4g after calcining adds in 250ml there-necked flask, adds 100ml distilled water in there-necked flask, 50 DEG C of ultrasonic reaction 1h;
(3) measure 1mol/L cobalt chloride solution, dropwise add in magnesium oxide solution, drip and terminate its pH value of rear survey, after pH value is stable (about 1.5h), stop experiment;
(4) add 100mL distilled water, with Persian funnel, emulsion is filtered, then use absolute ethyl alcohol cyclic washing 2-3 time of about 100mL;
(5) filter cake is put into vacuum drying chamber 80 DEG C (absolute ethyl alcohol boiling point 78.3 DEG C) dry 2-3h, obtain magnesium ni compound oxide presoma;
(6) by the material after grinding, 750 DEG C of calcining 2h, obtain pressed powder.
Advantage of the present invention and effect are:
1. the present invention propose a kind of with activated magnesia and cobalt chloride for raw material, utilize the polymerism of metal ion in the aqueous solution to prepare magnesium cobalt composite oxide of metal, without any additive, method is simple, and cost is low.
2. prepare Mg2CoO4 and MgCo2O4 magnesium cobalt composite metal oxide.
3. Mg2CoO4 and the MgCo2O4 magnesium cobalt composite metal oxide prepared has bimetallic center, can be used as catalyst or the carrier of some organic reaction.
Accompanying drawing explanation
Fig. 1 is present invention process flow chart;
Fig. 2 is that product SEM of the present invention schemes;
Fig. 3 is that product XRD of the present invention schemes.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.
1. general principle of the present invention
The water-soluble generation hydrated magnesium of magnesia, generates hydroxyl magnesium ion then, the aobvious alkalescence of solution, under more polyhydroxyl ion existence condition, forms hydroxyl Hydrated Magnesium Ion complex.
MgO+H 2O→[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 nickel chloride solution, along with nickel chloride concentration increases, solution acidic increases, under reaching certain pH value condition, form hydroxyl hydration nickel ion complex,
Co2+＋H2O→[Co(OH)]+＋H+………………⑦
[Co(OH)]+＋H2O→[Co(OH)2]（aq）＋H+………………⑧
[Co(OH)2]（aq）＋H2O→[Co(OH)3]-＋H+………………⑨
[Co (OH) 3]-+H2O → [Co (OH) 4] 2-+H+ ... 10. the Acidity of Aikalinity both utilizing is different, under certain proportion condition, when solution pH value is certain, form magnesium cobalt water and the hydroxyl polymeric body of spacial framework.
2. basic scheme of the present invention
The first step, is dissolved in the water activated magnesia, forms aqua oxidation magnesium complex; With second step, cobalt chloride is made into the certain density aqueous solution, is added drop-wise in hydrated magnesium complex solution.3rd step, obtains Mg2CoO4 and MgCo2O4 magnesium cobalt composite metal oxide by emulsion suction filtration, washing, dry rear calcining.
3. technical method of the present invention
This project for raw material with activated magnesia and cobalt chloride, utilizes the polymerism of metal ion in the aqueous solution, prepares the emulsion of magnesium cobalt combined polymerization, and after filtration washing drying, calcining obtains Mg2CoO4 and MgCo2O4 magnesium cobalt composite metal oxide.
4. specific embodiment of the present invention
(1) activated magnesia pretreatment, puts into Muffle 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) taking the activated magnesia 4g after calcining adds in 250ml there-necked flask, adds 100ml distilled water in there-necked flask, 50 DEG C of ultrasonic reaction 1h.
(3) measure 1mol/L cobalt chloride solution, dropwise add in magnesium oxide solution, drip and terminate its pH value of rear survey, after pH value is stable (about 1.5h), stop experiment.
(7) add 100mL distilled water, with Persian funnel, emulsion is filtered, then use absolute ethyl alcohol cyclic washing 2-3 time of about 100mL.
Filter cake is put into vacuum drying chamber 80 DEG C (absolute ethyl alcohol boiling point 78.3 DEG C) dry 2-3h, obtain magnesium ni compound oxide presoma.

Claims (1)

1. be the method that magnesium cobalt composite oxide of metal prepared by raw material with activated magnesia, it is characterized in that, described method comprises following process: the first step, with activated magnesia and cobalt chloride for raw material, prepares magnesium cobalt composite oxide of metal; Second step, is dissolved in the water activated magnesia, forms aqua oxidation magnesium complex; 3rd step, is made into the certain density aqueous solution by cobalt chloride, is added drop-wise in hydrated magnesium complex solution; 4th step, obtains Mg2CoO4 and MgCo2O4 magnesium cobalt composite metal oxide by emulsion suction filtration, washing, dry rear calcining;
Concrete preparation process is:
(1) activated magnesia pretreatment, puts into Muffle 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) taking the activated magnesia 4g after calcining adds in 250ml there-necked flask, adds 100ml distilled water in there-necked flask, 50 DEG C of ultrasonic reaction 1h;
(3) measure 1mol/L cobalt chloride solution, dropwise add in magnesium oxide solution, drip and terminate its pH value of rear survey, after pH value is stable (about 1.5h), stop experiment;
Add 100mL distilled water, with Persian funnel, emulsion is filtered, then use absolute ethyl alcohol cyclic washing 2-3 time of about 100mL;
Filter cake is put into vacuum drying chamber 80 DEG C (absolute ethyl alcohol boiling point 78.3 DEG C) dry 2-3h, obtain magnesium ni compound oxide presoma;
By the material after grinding, 750 DEG C of calcining 2h, obtain pressed powder.
CN201510763917.1A 2016-01-08 2016-01-08 Method for preparing magnesium cobalt metal compound oxide with active magnesium oxide as raw material Pending CN105413692A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103626234A (en) * 2013-12-11 2014-03-12 沈阳化工大学 Method for preparing magnesium manganese metal composite oxide by taking 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
CN103657650A (en) * 2013-12-10 2014-03-26 沈阳化工大学 Preparation method for Cu-rich magnesium copper metal composite oxide with magnesium oxide as raw material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN103657650A (en) * 2013-12-10 2014-03-26 沈阳化工大学 Preparation method for Cu-rich magnesium copper metal composite oxide with magnesium oxide as raw material
CN103626234A (en) * 2013-12-11 2014-03-12 沈阳化工大学 Method for preparing magnesium manganese metal composite oxide by taking active magnesium oxide as raw material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
C.A. QUERINI 等: "Catalytic combustion of diesel soot particles. Activity and characterization of Co/MgO and Co,K/MgO catalysts", 《APPLIED CATALYSIS B: ENVIRONMENTAL》 *
TAKESHI FURUSAWA 等: "Comparison of Co/MgO and Ni/MgO catalysts for the steam reforming of naphthalene as a model compound of tar derived from biomass gasification", 《APPLIED CATALYSIS A》 *

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Application publication date: 20160323