CN102139928A - Production method for lithium cobalt oxide material and industrial preparation device thereof - Google Patents
Production method for lithium cobalt oxide material and industrial preparation device thereof Download PDFInfo
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- CN102139928A CN102139928A CN 201110117424 CN201110117424A CN102139928A CN 102139928 A CN102139928 A CN 102139928A CN 201110117424 CN201110117424 CN 201110117424 CN 201110117424 A CN201110117424 A CN 201110117424A CN 102139928 A CN102139928 A CN 102139928A
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Abstract
The invention relates to a production method for a lithium cobalt oxide material and an industrial preparation device thereof; the industrial preparation device solves the problems that the existing electric heating kiln has high energy consumption, big kiln temperature difference and long production cycle, and refractory materials are easily corroded. The production method comprises the following steps: cobalt containing compound and lithium containing compound are taken as raw materials and a flame kiln such as a roller kiln or a tunnel kiln or a bogie hearth kiln which adopts natural gas or coal gas or liquefied petroleum gas as fuels is taken as the industrial preparation device to synthesize the lithium cobalt oxide material. In the invention, basic refractory materials such as magnesium oxide, calcium oxide, magnesia calcium bricks, magnesia zirconia bricks, pleonaste, magnesium manganese spinels and the like are also proposed to be adopted for replacing salic refractory materials used by the original kiln or a kiln furniture so as to reduce the damage of the kiln caused by the volatilization of lithium oixde in the lithium cobalt oxide material preparation process. The invention is characterized in that the flame kiln which directly adopts natural gas or coal gas or liquefied gas as fuels and basic refractory materials as kiln building materials not only can reduce energy consumption cost, but also can ensure uniform kiln temperature, reduces production cycle, improves product quality and production efficiency, and prolongs service life of the kiln.
Description
Technical field
The present invention relates to a kind of production method and preparation of industrialization device thereof of cobalt acid lithium class material.
Background technology
Lithium ion battery have operating voltage height, specific energy big, have extended cycle life, self-discharge rate is low, memory-less effect and advantage such as environmentally friendly, be a kind of power generation assembly of new green environment protection, be widely used in fields such as mobile communication, military affairs, aerospace and automobile power.The development of lithium ion battery has driven the positive electrode material fast development that lithium ion battery is used.Cobalt acid lithium class material is to have obtained the main positive electrode material that the lithium ion battery of widespread commercial application is used.The high quality of cobalt acid lithium material is synthetic most important for the research and development of lithium ion battery.The original intellecture property of domestic cobalt acid lithium class material development is few, and synthetic technology and production equipment are comparatively backward, especially is difficult to realize the cobalt acid lithium class material of low-cost synthesized high-performance.The present invention is from the building-up process and the performance study of cobalt acid lithium class material, cobalt acid lithium class preparation methods and preparation of industrialization device thereof have been proposed, to improve the efficient of cobalt acid lithium preparation of industrialization, improve the output and the quality of cobalt acid lithium class material, improve the production domesticization level of cobalt acid lithium class material preparation.
The production process of cobalt acid lithium class positive electrode material is as follows: with lithium-containing compound and cobalt compound is main raw material.Lithium-containing compound is at least a in Quilonum Retard, lithium hydroxide, Lithium Oxide 98min, the lithium nitrate.Cobalt compound is at least a in cobaltous carbonate, cobaltous dihydroxycarbonate, cobalt oxide, cobaltous oxide, the tricobalt tetroxide.After two class raw materials mixed, reaction generated under the high temperature about 1000 ℃.Generating structure and composition all satisfy the positive electrode material of lithium ion battery demand, and this is to decompose under the hot conditions and synthetic parallel reaction.The lithium of cobalt acid now class material produce is all finished in the electric heating pushed bat kiln mostly.In order to improve the output of cobalt acid lithium class material, some enterprise's introduction of foreign technology begins to manufacture and design the electric heating roller kiln and produces cobalt acid lithium class material.The used heating components and parts material of electric heating roller kiln mainly is a silicon carbide
Use the electric heating kiln to prepare cobalt acid lithium class material, have following deficiency: the first, be heating element with the globars, inhomogeneous based on the electric heating kiln kiln temperature of radiative transfer, the interior temperature difference of kiln thorax is bigger, and the goods inequality of being heated influences the quality of product.The second, the heat recovery of electric heating kiln is insufficient, adds will guarantee not sneak into impurity in the goods, does not adopt the technology of cooling air preheating base substrate.The 3rd, lithium ion has very strong corrodibility to kiln and kiln furniture material, and the cobalt acid lithium class synthetic initial stage of material, volatility is stronger, and is therefore, bigger to producing the equipment infringement.In the electric heating kiln, often adopt the silicon carbide heating member to put the aluminum oxide sleeve pipe prolongs heating member with the method for protection heating unit work-ing life.In addition, the production cycle of electric heating kiln is long partially, influences the output of cobalt acid lithium class material.The 4th, the kiln material of building of existing electric heating kiln generally is the relatively poor sal refractory materials of alkaline resistance properties, as trichroite, mullite, quartzose and corundum matter etc., because easily decomposing, lithium-containing compound generates the stronger Lithium Oxide 98min of volatility under hot conditions, very easily form the eutectic glassy phase with the sal refractory materials, to constantly permeate and corrode refractory materials, thereby influence the life-span of kiln.The 5th, for this developing country of China, electric power resource is shortage comparatively, and electricity price is comparatively expensive.More than all situations, become the technical bottleneck that synthetic cobalt acid lithium class material presses for solution.。
Summary of the invention
At above-mentioned deficiency, the synthesis mechanism according to cobalt acid lithium class material the present invention proposes and adopts improved flame kiln, is that main raw material prepares cobalt acid lithium class material with lithium-containing compound and cobalt compound.This preparation of industrialization device can make the cobalt acid lithium class material crystalline phase of being produced form even, more reasonable structure, and more excellent performance manufactures instinct and significantly reduces.
Lithium-containing compound of the present invention is at least a in Quilonum Retard, lithium hydroxide, Lithium Oxide 98min, the lithium nitrate, cobalt compound is at least a in cobaltous carbonate, cobaltous dihydroxycarbonate, cobalt oxide, cobaltous oxide, the tricobalt tetroxide, and lithium in the batching: the cobalt mol ratio is 1: 1.
At least a in the Sweet natural gas by custom-designed filter cleaning, coal gas, the liquefied petroleum gas (LPG) of the fuel of described flame kiln, kiln type can be at the bottom of roller kiln, tunnel furnace or the step car of continous way at least a in the kiln.
Described kiln all adopts high combustion rate burner, and firing atmosphere is an oxidizing atmosphere, conducts heat by strong convection, to guarantee the even of kiln temperature.Recrystallized silicon carbide is adopted at burner bocca position, and the metalwork part adopts heat-resistance stainless steel, to guarantee not having iron filings and other impurity to sneak in the goods in the burner use.
The hot blast that is used for refrigerated product can take following several mode to utilize its waste heat by behind the special filtering cleaner, and the one, directly be evacuated to the preheating zone heating product, the 2nd, enter in the combustion system in the mode of combustion air, the 3rd, by the heat exchanger recovery waste heat.All kinds of flue gases that kiln is discharged, after purifying by private filter, emptying again guarantees to reach environmental protection requirement.
Innovation part of the present invention also is, used basic refractory to replace sal refractory materials in traditional kiln.Described basic refractory is at least a in magnesium oxide, calcium oxide, magnesia-calcium brick, magnesium zirconia block, magnesia calcium zirconium brick, pleonast(e), the magnesium galaxite.Basic refractory is used for kiln, can avoids that the volatilization because of Lithium Oxide 98min causes the kiln damage in the cobalt acid lithium class material preparation process.
The firing temperature of cobalt acid lithium class material of the present invention is 800 ℃～1200 ℃, and the sintering period is 2～24h.
The present invention has overcome the high shortcoming of electric heating kiln energy consumption, especially in the higher developed regions of electricity price, with at least a flame kiln that acts as a fuel in Sweet natural gas, coal gas and the liquefied petroleum gas (LPG), adopt high combustion rate burner, conduct heat by strong convection, strengthen waste heat recovery and utilization, both can guarantee that the kiln temperature is even, also can save energy and reduce the cost.The present invention has also overcome globars Heating element in the electric heating kiln influences kiln because of the corrosive Aging Damage that is subjected to Lithium Oxide 98min in sintering process use.Also greatly improved the work-ing life of kiln among the present invention because of the use basic refractory replaces the aluminium-silica fireproof material.
Embodiment one
The roller kiln that are used for the material preparation of cobalt acid lithium class.Long 46 meters of full kiln, burner hearth is wide 1.2 meters, and is high 0.3 meter.With the Sweet natural gas is fuel, strainer has been installed advance the main valve of kiln at Sweet natural gas after.14 meters of preheating belt lengths have been installed 12 pairs of high combustion rate burners up and down respectively at roller-way, burn till 16 meters of belt lengths, at roller-way 16 pairs of high combustion rate burners have been installed respectively up and down.Full kiln lining adopts the brick one-tenth of light magnesium oxide.Maximum sintering temperature is 1000 ℃, and firing period is 4 hours.The wind of refrigerated product also enters into kiln again through behind the strainer, as combustion air, is assigned in each high combustion rate burner of preheating zone and clinkering zone.Institute's synthetic cobalt acid lithium material is a dark gray powder, accidental caking, and tap density reaches 2.4g/cm
3, granularity D50 is 8.5 μ m, product performance are stable, high conformity.At voltage is 3.0-4.2V, and 1C discharges and recharges under the condition, and its first discharge specific capacity reaches 136mAh/g.
Embodiment two
The roller kiln that are used for the material preparation of cobalt acid lithium class.Long 46 meters of full kiln, burner hearth is wide 1.2 meters, and is high 0.3 meter.With the liquefied petroleum gas (LPG) is fuel.Volume expansion often is attended by the heat absorption phenomenon, with the gas pipeline after the liquefied petroleum gas (LPG) reducing valve, by the heat exchanger of 60～80 ℃ of hot water is housed, receives on the strainer again, is redistributed to after the purification in each burner.14 meters of preheating belt lengths have been installed 12 pairs of high combustion rate burners up and down respectively at roller-way, burn till 16 meters of belt lengths, at roller-way 16 pairs of high combustion rate burners have been installed respectively up and down.Full kiln lining adopts the brick one-tenth of lightweight calcium oxide, and firing temperature is set at 1000 ℃, and firing period is 5 hours.Cobalt acid lithium class material is a dark gray powder, does not have caking, and tap density reaches 2.6g/cm
3, granularity D50 is 8.2 μ m, and product performance are stable, and high conformity is 3.0-4.2V at voltage, and 1C discharges and recharges under the condition, and its first discharge specific capacity reaches 138mAh/g.
Embodiment three
Be used to prepare kiln at the bottom of the car of cobalt acid lithium class material.Kiln is of a size of 2.5m * 2m * 2m, and full kiln is built into the high-quality magnesia-calcium brick.Kiln car is built by laying bricks or stones with the light weight calcium magnesia brick, and kiln furnitures are the saggar of magnesium calcium zirconium material, and two pairs of isothermal high combustion rate burners are installed alternately.Act as a fuel with Sweet natural gas, advance kiln natural gas via private filter and purify.Waste heat is by the heat exchanger heats combustion air.Firing temperature is 1000 ℃, and firing period is 6 hours.Cobalt acid lithium class material is a dark gray powder, does not have caking, and tap density reaches 2.7g/cm
3, granularity D50 is 7.4 μ m, and product performance are stable, and high conformity is 3.0-4.2V at voltage, and 1C discharges and recharges under the condition, and its first discharge specific capacity reaches 143mAh/g.
Embodiment four
Be used to prepare the tunnel furnace of cobalt acid lithium class material.Long 46 meters of full kiln, burner hearth is wide 1.2 meters, and is high 1.0 meters, 14 meters of preheating zones, 16 meters of clinkering zones, 16 meters of cooling zones.12 pairs of high combustion rate burners are installed in the preheating zone, and clinkering zone has been installed 16 pairs of high combustion rate burners.With the Sweet natural gas is fuel, strainer has been installed advance the main valve of kiln at Sweet natural gas after.Full kiln adopts high-quality lightweight magnesia calcium zirconium brick to be built into, and the kiln car material adopts the surface to coat the recrystallized silicon carbide of magnesium calcium zirconium coating, and firing temperature is set at 980 ℃, and firing period is 24 hours.Cobalt acid lithium class material is a dark gray powder, does not have caking, and tap density reaches 2.9g/cm
3, D50 is 6.5 μ m, and product performance are stable, and high conformity is 3.0-4.2V at voltage, and 1C discharges and recharges under the condition, and its first discharge specific capacity reaches 145mAh/g.
Claims (9)
1. the production method and the preparation of industrialization device thereof of a cobalt acid lithium class material is characterized in that, are raw material with cobalt compound, lithium-containing compound, and adopting with the basic refractory is the synthetic cobalt acid of the flame kiln lithium material that kiln is built material.
2. the production method of cobalt as claimed in claim 1 acid lithium class material is characterized in that, lithium-containing compound is at least a in Quilonum Retard, lithium hydroxide, Lithium Oxide 98min, the lithium nitrate.
3. the production method of cobalt as claimed in claim 1 acid lithium class material is characterized in that, cobalt compound is at least a in cobaltous carbonate, cobaltous dihydroxycarbonate, cobalt oxide, cobaltous oxide, the tricobalt tetroxide.
4. the preparation of industrialization device of cobalt as claimed in claim 1 acid lithium class material is characterized in that, the used fuel of flame kiln is at least a in the Sweet natural gas that purifies after filtration, coal gas, the liquefied petroleum gas (LPG).
5. the preparation of industrialization device of cobalt as claimed in claim 1 acid lithium class material is characterized in that, kiln is at least a in the kiln at the bottom of roller kiln, tunnel furnace, the car.
6. flame kiln as claimed in claim 4 is characterized in that, adopts the high combustion rate burner of conveniently regulating and controlling fuel, air capacity and ratio thereof.
7. high combustion rate burner as claimed in claim 6 is characterized in that, the recrystallized silicon carbide preparation is adopted at burner bocca position, and the metalwork part adopts the heat-resistance stainless steel preparation.
8. flame kiln as claimed in claim 4 is characterized in that, building the kiln material is basic refractory, and basic refractory is mainly at least a in magnesium oxide, calcium oxide, magnesia-calcium brick, magnesium zirconia block, magnesia calcium zirconium brick, pleonast(e), the magnesium galaxite.
9. the production method and the preparation of industrialization device thereof of cobalt acid lithium class material as claimed in claim 1 is characterized in that cobalt acid lithium firing temperature is 800 ℃～1200 ℃, and the sintering period is 2～24h, and the preparation of industrialization device is easy to obtain above-mentioned processing condition.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583565A (en) * | 2012-02-29 | 2012-07-18 | 北京师范大学 | Preparation method for spinel-type lithium manganate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101354215A (en) * | 2008-09-19 | 2009-01-28 | 吉林市弗兰达科技股份有限公司 | Inorganic salt uniform calcination rotary kiln |
| CN101762155A (en) * | 2010-01-15 | 2010-06-30 | 南京盛和陶瓷材料有限公司 | High-efficiency energy-saving high-technology ceramic material synthesis pre-burning kiln |
| CN201611208U (en) * | 2009-12-31 | 2010-10-20 | 中国恩菲工程技术有限公司 | Nickel-containing material calcination device |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101354215A (en) * | 2008-09-19 | 2009-01-28 | 吉林市弗兰达科技股份有限公司 | Inorganic salt uniform calcination rotary kiln |
| CN201611208U (en) * | 2009-12-31 | 2010-10-20 | 中国恩菲工程技术有限公司 | Nickel-containing material calcination device |
| CN101762155A (en) * | 2010-01-15 | 2010-06-30 | 南京盛和陶瓷材料有限公司 | High-efficiency energy-saving high-technology ceramic material synthesis pre-burning kiln |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583565A (en) * | 2012-02-29 | 2012-07-18 | 北京师范大学 | Preparation method for spinel-type lithium manganate |
| CN102583565B (en) * | 2012-02-29 | 2014-10-29 | 北京师范大学 | Preparation method for spinel-type lithium manganate |
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Application publication date: 20110803 |