CN102070197A - Preparation method of spherical manganous oxide - Google Patents
Preparation method of spherical manganous oxide Download PDFInfo
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- CN102070197A CN102070197A CN 201110027508 CN201110027508A CN102070197A CN 102070197 A CN102070197 A CN 102070197A CN 201110027508 CN201110027508 CN 201110027508 CN 201110027508 A CN201110027508 A CN 201110027508A CN 102070197 A CN102070197 A CN 102070197A
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Abstract
The invention discloses a preparation method of spherical manganous oxide. In the preparation method, precursor spherical manganous carbonate is synthesized, and then spherical manganous carbonate is calcined to synthesize spherical manganous oxide. The preparation method comprises the following specific steps: using industrial level manganese salt and an additive to prepare a solution A with deionized water; using an industrial level alkaline precipitator and a complexing agent to prepare a solution B with deionized water; pouring deionized water in a reaction container, wherein the volume of the deionized water is 1/10-2/3 of that of the container, adding the solutions A and B in the reaction container in a volume ratio of (1:1)-(1:10), and controlling the PH value to 5-12; spilling the generated precipitate in a washing and filtering device, washing the precipitate to ensure that the PH value of the washing water is 7+/-0.5, filtering, drying filter cake in an oven with the temperature of 50-200 DEG C for 2-10 hours, and sieving with a 80 meshes of screen to obtain spherical manganese carbonate powder; and placing the spherical manganese carbonate in an atmosphere furnace, and heating to 400-700 DEG C to calcine for 8-15 hours and synthesize the spherical manganous oxide. The preparation method of the invention has simple process, the industrial production is easy to achieve, and the obtained spherical manganous oxide powder is good in mobility.
Description
Technical field
The present invention relates to a kind of preparation method of spherical manganese monoxide, the particularly preparation of high-density spherical manganese monoxide, the catalyzer of main siccative, amylalcohol manufacturing, beverage auxiliary, trace element fertilizer, smelting, welding, fabric reduction printing and dyeing as raw material, coating and the varnish of producing the iron oxysome, glass-ceramic is painted and fade, grease bleaching and battery production.
Background technology
In modern industry, manganese and compound thereof are applied to the every field of national economy.Wherein Iron And Steel Industry is most important field, accounts for 90%～95% with the manganese amount, mainly as reductor and the sweetening agent in ironmaking and the steelmaking process, and is used for alloying.All the other manganese of 5%～10% are used for other industrial circles, as chemical industry, light industry, building materials industry, national defense industry, electronic industry or the like.In recent years, high and new technology projects such as high performance magnetic material, superfine powdery material, inorganic nano and functional material, high-quality artificial crystal material are made it be supported on national policy by the project that country is decided to be encourage growth.
Manganese monoxide claims manganese monoxide again, be important a kind of in the manganic compound, the catalyzer of main siccative, amylalcohol manufacturing, beverage auxiliary, trace element fertilizer, smelting, welding, fabric reduction printing and dyeing as raw material, coating and the varnish of producing the iron oxysome, glass-ceramic is painted and fade, grease bleaching and battery production etc.
Present domestic manganese already material enterprise is a lot, major part is positioned at the Guangxi that China abounds with manganese ore, substantially belong to mineral products roughing type enterprise, its product grade is not high, a lot of enterprises manganese monoxide product content is 60%～90%, is being subjected to some restrictions to the higher magneticsubstance industry of its quality requirements, ceramic industry are relative with the battery industry.Industry begins to obtain its widespread use in these industries by the quality that improves the manganese monoxide product, to fill up the demand in market at present.
With the be applied as example of manganese monoxide: along with progress of science and technology in magneticsubstance and battery material industry, soft magnetic ferrite is as a kind of important basic function material, be widely used in the electronic industries such as communication, sensing, audio and video equipment, wave filter, transformer, for vast market has been opened in the application of soft magnetic ferrite.Simultaneously, because the fast development of electronics and information industries such as communication, computer network makes the demand of high performance soft magnetic ferrite material grow with each passing day.Present most widely used soft magnetic ferrite surely belongs to the MnZn series and the Ni-Zn series row of spinel type, lower valency such as manganese monoxide or trimanganese tetroxide Mn oxide accounts for 25%～32%(mol ratio in Mn-Zn soft magnetic ferrite), the output of present China Mn-Zn soft magnetic ferrite is about 300,000 tons, and every year is with 20% speed increase.Along with the sector progressively to the development of high-end magneticsubstance the time, certainly will the manganese monoxide demand of divalent attitude be increased greatly.The magneticsubstance industry of China relies on rich in natural resources and labor force's advantage, and huge domestic and international market supports that will be arranged a stable developing period.Today, the production of magneticsubstance magnet mainly concentrated on the Asia, and Japan is based on high-grade magnet, and China is based on low and middle-grade magnets, and the expensive goods market of partitioning portion.Because China has supporting market of good complete machine and investment environment, quicken the development of the high-end magneticsubstance of China, acceleration Japan, American-European ferrimagnet production shift to China.Prediction, with the output in the whole world more than 60%, China will become magnetic material production base the biggest in the world, magnetic material selling market to the output of the ferrimagnet of China in 2010.The fast development of the sector is that condition has been created in the development in Mn-Zn soft magnetic ferrite material powder market.High-quality product be unable to do without high-quality starting material, is a good commercial opportunity as high-quality raw material supply.
Along with the develop rapidly of present secondary cell industry, being in an emergency of global rare precious metals cobalt and nickel resources, and price is constantly soaring.Sustainable development view is told us must save with generation and is done, in fact also restricting cobalt system objectively, the development of nickel based material.When other secondary cells of research, 1.5V alkali manganese chargeable battery has suitable advantage, its two big attraction: one, cost is low, alkali manganese chargeable battery and alkaline cell are close on main raw material, producing apparatus and the production environment of manufacturing processed, use substantially, its market value only is equivalent to the price of disposable high tension battery than low 2～4 one-tenth of similar rechargeable battery.Two, electric power is powerful, endurance is lasting, and the alkali manganese chargeable battery single working hour is greater than more than the Ni-based chargeable battery single working hour several times.When each precious metal price can be in any more at present, a lot of enterprises began to develop this class store battery, and 1.5V alkali manganese chargeable battery has showed its huge market potential.Manganese monoxide improves the additive of the irreversible phenomena of Manganse Dioxide in charge and discharge process and is employed as a kind of, and the research that replaces the novel alkali manganese chargeable battery of Manganse Dioxide with manganese monoxide is arranged.Also be the important raw and processed materials of some capacity batteries simultaneously.This is showing that all producing high-grade manganese monoxide certainly will bring huge economic benefit to enterprise.
Summary of the invention
The objective of the invention is to: a kind of preparation method of spherical manganese monoxide is provided, and this preparation method's technology is simple, realizes suitability for industrialized production easily, and the spherical manganese monoxide powder fluidity that obtains is good.
Technical solution of the present invention is: this preparation method is earlier synthetic precursor spheric manganese carbonate, and spheric manganese carbonate is calcined the synthesizing spherical manganese monoxide then, and concrete steps are as follows:
1. with deionized water the manganese salt and the additive of technical grade is mixed with A solution, the manganese salt concn is that 0.1M～10M, additive concentration are 0.05M～7M in the A solution;
2. with deionized water alkaline precipitating agent, the complexing agent of technical grade is made into B solution, B solution neutral and alkali precipitation agent concentration is that 0.1M～10M, complexing agent concentration are 0.05M～7M;
3. open the stirring of reaction vessel, drop into container 1/10～2/3 volumetrical deionized water as end water, Jiang Dishui is heated to 30 ℃～100 ℃, under violent stirring, A solution and B solution carry out replacement(metathesis)reaction, control pH value 5～12 in 1:1～1:10 adding reactor by volume;
4. the precipitation of reaction generation overflows to washing and filtering equipment, washing of precipitate is qualified to foreign matter content, and washing water PH filters 7 ± 0.5, filter cake dried by the fire in 50～200 ℃ baking oven 2～10 hours, and the spheric manganese carbonate powder that 80 mesh sieves get purity Wei ≧ 99% is crossed in the oven dry back;
5. spheric manganese carbonate is positioned in the atmosphere furnace, feeds 1～2m
3The nitrogen and hydrogen mixture of/h is warming up to 400～700 ℃ of calcining 8～15h, synthetic spherical manganese monoxide.
Wherein, described cobalt salt is a kind of in Manganous chloride tetrahydrate, manganous sulfate, the manganous nitrate.
Wherein, described additive is a kind of in ammonium citrate, the ammonium oxalate.
Wherein, described alkaline precipitating agent is a kind of in yellow soda ash, sodium bicarbonate, the bicarbonate of ammonia.
Wherein, described complexing agent is a kind of among ammoniacal liquor, citric acid, the EDTA.
Wherein, the nitrogen volume is 80-90% in the described nitrogen and hydrogen mixture, and hydrogen volume is 10-20%.
The present invention has the following advantages: 1, the manganese monoxide of present method preparation is that a kind of density height, crystalline structure are complete, particle shape is sphere or class spheric manganic compound, this manganic compound synthesis technique is simple, cost is low, particle diameter can be controlled, and realizes suitability for industrialized production easily; 2, the Chemical Composition of the manganese monoxide of present method preparation and the requirement that physicals all can satisfy lithium ion battery material lithium manganate Chemical Composition and physicals.
Concrete embodiment
Further specify technical solution of the present invention below in conjunction with specific embodiment, these embodiment can not be interpreted as it is restriction to technical solution.
Embodiment 1:
With deionized water Manganous chloride tetrahydrate is made into 0.1M, ammonium citrate is made into the A solution of 0.05M, with deionized water yellow soda ash is made into 0.1M, ammoniacal liquor is made into the B solution of 0.05M, open the stirring of reaction vessel, drop into container 2/3 volumetrical deionized water as end water, end water is heated to 30 ℃, A solution joins in the reaction vessel with the flow velocity of 5ml/min, B solution joins in the reaction vessel with the flow velocity of 5ml/min, the control pH value is 5, the precipitation that reaction generates overflows to washing and filtering equipment, washing of precipitate is qualified to foreign matter content, and washing water PH filters 6.5, filter cake was 50 ℃ of bakings 10 hours, the spheric manganese carbonate powder that 80 mesh sieves get purity Wei ≧ 99% is crossed in the oven dry back, and spheric manganese carbonate is positioned in the atmosphere furnace, feeds 1m
3The nitrogen and hydrogen mixture of/h, wherein nitrogen volume 80%, hydrogen volume 20% are warming up to 400 ℃ of calcining 15h, synthetic spherical manganese monoxide.
Embodiment 2:
With deionized water Manganous chloride tetrahydrate is made into 2.5M, ammonium oxalate is made into the A solution of 1.25M, with deionized water bicarbonate of ammonia is made into 2.5M, citric acid is made into the B solution of 1.25M, open the stirring of reaction vessel, drop into container 1/10 volumetrical deionized water as end water, end water is heated to 50 ℃, A solution joins in the reaction vessel with the flow velocity of 5ml/min, B solution joins in the reaction vessel with the flow velocity of 12.5ml/min, the control pH value is 7, the precipitation that reaction generates overflows to washing and filtering equipment, washing of precipitate is qualified to foreign matter content, and washing water PH filters 7, filter cake was 100 ℃ of bakings 8 hours, the spheric manganese carbonate powder that 80 mesh sieves get purity Wei ≧ 99% is crossed in the oven dry back, and spheric manganese carbonate is positioned in the atmosphere furnace, feeds 1.5m
3The nitrogen and hydrogen mixture of/h, wherein nitrogen volume 85%, hydrogen volume 15% are warming up to 500 ℃ of calcining 12h, synthetic spherical manganese monoxide.
Embodiment 3:
With deionized water manganous nitrate is made into 5M, ammonium citrate is made into the A solution of 3.5M, with deionized water sodium bicarbonate is made into 5M, ammoniacal liquor is made into the B solution of 3.5M, open the stirring of reaction vessel, drop into container 1/2 volumetrical deionized water as end water, end water is heated to 70 ℃, A solution joins in the reaction vessel with the flow velocity of 5ml/min, B solution joins in the reaction vessel with the flow velocity of 25ml/min, the control pH value is 9, the precipitation that reaction generates overflows to washing and filtering equipment, washing of precipitate is qualified to foreign matter content, and washing water PH filters 7.5, filter cake was 150 ℃ of bakings 6 hours, the spheric manganese carbonate powder that 80 mesh sieves get purity Wei ≧ 99% is crossed in the oven dry back, and spheric manganese carbonate is positioned in the atmosphere furnace, feeds 2.0m
3The nitrogen and hydrogen mixture of/h, wherein, nitrogen volume 90%, hydrogen volume 10% are warming up to 600 ℃ of calcining 10h, synthetic spherical manganese monoxide.
Embodiment 4:
With deionized water manganous sulfate is made into 7.5M, ammonium oxalate is made into the A solution of 5.2M, with deionized water yellow soda ash is made into 7.5M, the EDTA disodium is made into the B solution of 5.2M, open the stirring of reaction vessel, drop into container 1/5 volumetrical deionized water as end water, end water is heated to 90 ℃, A solution joins in the reaction vessel with the flow velocity of 10ml/min, B solution joins in the reaction vessel with the flow velocity of 75ml/min, the control pH value is 10.5, the precipitation that reaction generates overflows to washing and filtering equipment, washing of precipitate is qualified to foreign matter content, and washing water PH filters 7.5, filter cake was 180 ℃ of bakings 4 hours, the spheric manganese carbonate powder that 80 mesh sieves get purity Wei ≧ 99% is crossed in the oven dry back, and spheric manganese carbonate is positioned in the atmosphere furnace, feeds 1m
3The nitrogen and hydrogen mixture of/h, wherein, nitrogen volume 95%, hydrogen volume 5% are warming up to 650 ℃ of calcining 9h, synthetic spherical manganese monoxide.
Embodiment 5:
With deionized water manganous nitrate is made into 10M, ammonium oxalate is made into the A solution of 7M, with deionized water bicarbonate of ammonia is made into 10M, ammoniacal liquor is made into the B solution of 7M, open the stirring of reaction vessel, drop into container 1/3 volumetrical deionized water as end water, end water is heated to 100 ℃, A solution joins in the reaction vessel with the flow velocity of 5ml/min, B solution joins in the reaction vessel with the flow velocity of 50ml/min, the control pH value is 12, the precipitation that reaction generates overflows to washing and filtering equipment, washing of precipitate is qualified to foreign matter content, and washing water PH filters 7, filter cake advances for a short time 200 ℃ of bakings 2, the spheric manganese carbonate powder that 80 mesh sieves get purity Wei ≧ 99% is crossed in the oven dry back, and spheric manganese carbonate is positioned in the atmosphere furnace, feeds 2m
3The nitrogen and hydrogen mixture of/h, wherein nitrogen volume 90%, hydrogen volume 10% are warming up to 700 ℃ of calcining 8h, synthetic spherical manganese monoxide.
The spherical manganese monoxide that embodiment 1-5 makes is a spheroidal crystal, median size 2～30 μ m, loose density 1.6～2.2g/cm
3, tap density reaches 2.2g/cm
3More than, Chun Du ≧ 99.5%.
Claims (6)
1. the preparation method of spherical manganese monoxide is characterized in that: this preparation method is earlier synthetic precursor spheric manganese carbonate, spheric manganese carbonate calcining synthesizing spherical manganese monoxide then, and concrete steps are as follows:
1. with deionized water the manganese salt and the additive of technical grade is mixed with A solution, the manganese salt concn is that 0.1M～10M, additive concentration are 0.05M～7M in the A solution;
2. with deionized water alkaline precipitating agent, the complexing agent of technical grade is made into B solution, B solution neutral and alkali precipitation agent concentration is that 0.1M～10M, complexing agent concentration are 0.05M～7M;
3. open the stirring of reaction vessel, drop into container 1/10～2/3 volumetrical deionized water as end water, Jiang Dishui is heated to 30 ℃～100 ℃, under violent stirring, A solution and B solution carry out replacement(metathesis)reaction, control pH value 5～12 in 1:1～1:10 adding reactor by volume;
4. the precipitation of reaction generation overflows to washing and filtering equipment, washing of precipitate is qualified to foreign matter content, and washing water PH filters 7 ± 0.5, filter cake dried by the fire in 50～200 ℃ baking oven 2～10 hours, and the spheric manganese carbonate powder that 80 mesh sieves get purity Wei ≧ 99% is crossed in the oven dry back;
5. spheric manganese carbonate is positioned in the atmosphere furnace, feeds 1～2m
3The nitrogen and hydrogen mixture of/h is warming up to 400～700 ℃ of calcining 8～15h, synthetic spherical manganese monoxide.
2. the preparation method of spherical manganese monoxide according to claim 1 is characterized in that: described cobalt salt is a kind of in Manganous chloride tetrahydrate, manganous sulfate, the manganous nitrate.
3. the preparation method of spherical manganese monoxide according to claim 1 is characterized in that: described additive is a kind of in ammonium citrate, the ammonium oxalate.
4. the preparation method of spherical manganese monoxide according to claim 1 is characterized in that; Described alkaline precipitating agent is a kind of in yellow soda ash, sodium bicarbonate, the bicarbonate of ammonia.
5. the preparation method of spherical manganese monoxide according to claim 1 is characterized in that: described complexing agent is a kind of among ammoniacal liquor, citric acid, the EDTA.
6. the preparation method of spherical manganese monoxide according to claim 1, it is characterized in that: the nitrogen volume is 80-90% in the described nitrogen and hydrogen mixture, hydrogen volume is 10-20%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491422A (en) * | 2011-12-26 | 2012-06-13 | 湖南汇通科技有限责任公司 | Spherical manganic manganous oxide and its preparation method |
| CN103035902A (en) * | 2012-12-07 | 2013-04-10 | 上海空间电源研究所 | Preparation method of modified manganese oxide material for lithium ion batteries |
| CN103700830A (en) * | 2013-12-30 | 2014-04-02 | 湖南汇通科技有限责任公司 | Manganese sesquioxide micro powder and preparation method and application thereof |
| CN107546374A (en) * | 2017-03-27 | 2018-01-05 | 广西科技师范学院 | A kind of preparation method of C/MnO combination electrode materials |
| CN108408757A (en) * | 2018-03-15 | 2018-08-17 | 益阳鸿源稀土有限责任公司 | A kind of preparation method of high pure and ultra-fine scandium oxide powder |
| CN109638277A (en) * | 2018-12-10 | 2019-04-16 | 桂林理工大学 | A kind of preparation method of Magnesium ion battery manganous oxide negative electrode material |
| CN112259715A (en) * | 2020-10-14 | 2021-01-22 | 安徽益佳通电池有限公司 | MnO-loaded graphitized mesocarbon microbeads and preparation method and application thereof |
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| CN101269840A (en) * | 2008-03-05 | 2008-09-24 | 广州融捷材料科技有限公司 | Spherical manganese carbonate and preparing method thereof |
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- 2011-01-26 CN CN 201110027508 patent/CN102070197A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101269840A (en) * | 2008-03-05 | 2008-09-24 | 广州融捷材料科技有限公司 | Spherical manganese carbonate and preparing method thereof |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491422A (en) * | 2011-12-26 | 2012-06-13 | 湖南汇通科技有限责任公司 | Spherical manganic manganous oxide and its preparation method |
| CN103035902A (en) * | 2012-12-07 | 2013-04-10 | 上海空间电源研究所 | Preparation method of modified manganese oxide material for lithium ion batteries |
| CN103035902B (en) * | 2012-12-07 | 2015-04-15 | 上海空间电源研究所 | Preparation method of modified manganese oxide material for lithium ion batteries |
| CN103700830A (en) * | 2013-12-30 | 2014-04-02 | 湖南汇通科技有限责任公司 | Manganese sesquioxide micro powder and preparation method and application thereof |
| CN103700830B (en) * | 2013-12-30 | 2016-01-20 | 湖南汇通科技有限责任公司 | A kind of manganese sesquioxide managnic oxide micro mist and its preparation method and application |
| CN107546374A (en) * | 2017-03-27 | 2018-01-05 | 广西科技师范学院 | A kind of preparation method of C/MnO combination electrode materials |
| CN107546374B (en) * | 2017-03-27 | 2019-10-25 | 广西科技师范学院 | A kind of preparation method of C/MnO combination electrode material |
| CN108408757A (en) * | 2018-03-15 | 2018-08-17 | 益阳鸿源稀土有限责任公司 | A kind of preparation method of high pure and ultra-fine scandium oxide powder |
| CN109638277A (en) * | 2018-12-10 | 2019-04-16 | 桂林理工大学 | A kind of preparation method of Magnesium ion battery manganous oxide negative electrode material |
| CN112259715A (en) * | 2020-10-14 | 2021-01-22 | 安徽益佳通电池有限公司 | MnO-loaded graphitized mesocarbon microbeads and preparation method and application thereof |
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Application publication date: 20110525 |