CN101786672A

CN101786672A - Production method of cobaltous oxide for power battery

Info

Publication number: CN101786672A
Application number: CN200910226696A
Authority: CN
Inventors: 周红阳
Original assignee: Individual
Current assignee: Zhou Hongyang
Priority date: 2009-12-18
Filing date: 2009-12-18
Publication date: 2010-07-28
Anticipated expiration: 2029-12-18
Also published as: CN101786672B

Abstract

The invention relates to a production method of cobaltous oxide for a power battery, comprising the following steps of: firstly reacting a cobalt chloride solution with an ammonium acid carbonate precipitant through a third-order reaction tank to generate basic cobaltous carbonate slurries; then filtering the slurries, slurrying, washing, drying, and protecting and crashing by an inert gas to obtain basic cobaltous carbonate powder; then decomposing through a positive pressure atmosphere, wherein a decomposing furnace is internally provided with 10 computer temperature control areas, air inside the decomposing furnace is driven by the inert gas before feeding, then a CO2 gas is continuously charged, and a material boat loaded with the basic cobaltous carbonate powder passes through the 10 computer temperature control areas at the speed of 5 minutes per time so that basic cobaltous carbonate is decomposed to generate the cobaltous oxide for the power battery in the positive pressure atmosphere. The invention saves the energy and has low production cost; in addition, the cobaltous oxide has great high chemical purity and physical performance and can be used as powder materials of the power high-performance and high-power battery.

Description

Production method of cobaltous oxide for power battery

Technical field

The present invention relates to the powder body material production method that battery industry is used, especially prepare the production method of cobaltous oxide for power battery powder, international classification number is C01G51/04.

Background technology

Publication number is that 101200309 patent of invention " method for producing cobaltous oxide " is though can produce the high cobaltous oxide of a kind of cobalt contents, but the product chemical purity is not good enough, the content of elements such as nickel, iron, calcium, copper, manganese, zinc, magnesium is higher in the product, does not reach the every index request of high-performance high-power drive pond to battery material.In addition, one will be 50-55 ℃ to reactive tank heating and the controlled temperature that generates the intermediates cobaltous carbonate, need expend the more energy; Two will constantly fill pilot-gas---hydrogen toward decomposing in the reduction furnace that generates cobaltous oxide, and hydrogen is relatively more expensive, so also there is the high weak point of production cost in this patent of invention.

Summary of the invention

The purpose of this invention is to provide a kind of production method of cobaltous oxide for power battery, accomplish that the product chemical purity is high and satisfy the every index request of high-performance high-power electric battery to battery material, and production cost is low.

Production stage of the present invention is as follows:

1, preparation cobalt oxide solution

The hot pure water 1.5m that in configured slot, adds 25-35 ℃ ³, open agitating vane, the limit evenly adds cobalt chloride, and the limit adds hot pure water to 3m ³, added 3 liters of the aviation kerosenes of emulsifying effect simultaneously, stir after 25-35 minute, sampling analysis when cobalt oxide concentration reaches 45-50g/L, is warming up to 40 ℃, adding acid or alkali, to adjust pH value be 2.0-2.5, pumps into cobalt liquid storage tank then.

2, synthetic food carbon ammonium precipitation agent

The hot pure water 1.5m that in configured slot, adds 45-50 ℃ ³, open agitating vane, slowly add food carbon ammonium, add hot pure water simultaneously to 3m ³, dissolving back sampling and measuring when food carbon ammonium concentration reaches 200-220g/L, is warming up to 60 ℃ fully, pumps into the alkali lye storage tank.

3, heavy cobalt

The normal temperature pure water that adds high 20CM in first and second order reaction groove in advance adds high 30CM in advance in third stage reactive tank, temperature 55-60 ℃ hot pure water; Open the agitating vane of first step reactive tank, with the 1000L/h flow, enter first step reactive tank simultaneously with the 1000-1200L/h flow from the alkali lye of alkali lye storage tank from the cobalt liquid of cobalt liquid storage tank; When the pH of first step reactive tank value is 6.7-7.0, open the valve of first step reactive tank overflow port, the beginning discharge is opened the agitating vane of second stage reactive tank simultaneously to second stage reactive tank; When the slip liquid level reaches second stage reactive tank overflow port height and pH value for 7.75-7.85, be in the groove material chemical reaction better, when generating cobaltous dihydroxycarbonate, the valve discharge of opening second stage reactive tank overflow port is to third stage reactive tank, open third stage reactive tank agitating vane simultaneously, and press the 2000-2200L/h flow and add 5 liters of 55-60 ℃ hot pure water and alcohol.Alcohol further disperses crystalline particle, thereby reduces granularity, improves the physicals of intermediates.

4, filtration, pulp, washing

When third stage reactive tank slip volume reaches 4m ³The time, be pressed into pressure filter; At first compress filter plate, make slip become filter cake behind squeeze and filter, washing filter Pie unclamps filter plate and unloads filter Pie then; Add the normal temperature pure water toward the pulp groove earlier when pulp begins, open agitating vane and slowly add filter cake simultaneously in the pulp groove, the limit adds 55-60 ℃ of hot pure water limit pulp stirred 30 minutes, accomplished pulp cmpletely; The material that pulp is good is pressed into and carries out filtration washing in the pressure filter, and till washing no white precipitate, should be less than 0.005g/L with the chlorion that silver nitrate titration detects in the filtrate this moment.

5, protection of inert gas fragmentation

The wet cobalt carbonate hydroxide filter cake that washing of precipitate is the good oven drying at low temperature room of packing into, storing temperature 65-80 ℃; After the oven dry, material is sent into crusher in crushing, feed rare gas element simultaneously in crusher, obtaining granularity is the following cobaltous dihydroxycarbonate powder of 4um.

6, malleation atmosphere is decomposed production

Series arrangement has 10 computer temperature-controlled areas in the decomposing furnace, and the temperature in every district is respectively 200,260,300,350,400,480,480,400,300,250; Drove furnace air 1.5-2.5 hour with rare gas element earlier before the charging, successively in stove, charge into CO then ₂Gas, the material boat that the cobaltous dihydroxycarbonate powder is housed passes through 10 temperature-controlled areas in the stove by each 5 minutes speed, and cobaltous dihydroxycarbonate decomposes generation cobaltous oxide for power battery product, filling with inert gas during discharging in malleation atmosphere.

7, rare gas element passivation and packing

The product bucket of rapidly product being packed into, and in the product bucket filling with inert gas, after rare gas element passivation for some time, product is carried out the double-layer vacuum packing, the lining bag be the vacuum packaging of aluminium platinum, packs with composite plastic film for outer bag.

Compared with the prior art, the present invention has following characteristics:

1, owing to adopts food carbon ammonium as precipitation agent, the chemical purity and the physicals of product have been improved, therefore after this product joins and can fill nickel metal hydride battery, can improve the charge-discharge performance of active substance effectively, fully improve the energy storage utilization ratio of active substance, thereby can increase the specific storage that to fill Ni-MH power cell, improve and charge into electric cycle index, prolong battery work-ing life.

2, owing in cobalt chloride solution preparation journey, added the aviation spirit of emulsifying effect, improve the speed of cobalt liquid and alkaline reaction, reduced the temperature requirement that generates the cobaltous dihydroxycarbonate reaction, so first and second order reaction groove need not heating, but save energy reduces production costs.

3, produce cobaltous oxide owing to adopt malleation atmosphere that cobaltous dihydroxycarbonate is decomposed, only need in decomposing furnace, to charge into CO than hydrogen cheapness ₂Therefore gas further reduce production costs.

4, owing to adopt 20 temperature controls, low-temperature decomposition technology, make material in malleation atmosphere decomposition course, react balanced, the temperature difference, granularity are effectively controlled, material reaction grows, no longer occurs out of control no longer arbitrarily, so the finished product---and every chemistry of cobaltous oxide for power battery and physical index are good.

Description of drawings

Fig. 1 is the cobaltous oxide for power battery chemical component table

Fig. 2 is a cobaltous oxide for power battery physicals table

Embodiment

Embodiment one

Production stage is the same, repeats no more herein.The inert gas that this example adopts is a nitrogen.

Embodiment two

Basic identical with example one, different is that inert gas is a helium.

Embodiment three

Basic identical with example one, different is that inert gas is a neon.

Embodiment four

Basic identical with example one, different is that inert gas is an argon gas.

Embodiment five

Basic identical with example one, different is that inert gas is a krypton gas.

Embodiment six

Basic identical with example one, different is that inert gas is an xenon.

Embodiment seven

Basic identical with example one, different is that inert gas is a radon gas.

Claims

1. production method of cobaltous oxide for power battery, production stage is as follows:

A, preparation cobalt chloride solution

The hot pure water 1.5m that in configured slot, adds 25-35 ℃ ³, open agitating vane, the limit evenly adds cobalt chloride, and the limit adds hot pure water to 3m ³, add 3 liters of aviation kerosenes simultaneously, stir after 25-35 minute, sampling analysis when cobalt chloride concentration reaches 45-50g/L, is warming up to 40 ℃, adding acid or alkali, to adjust pH value be 2.0-2.5, pumps into cobalt liquid storage tank then;

B, the agent of synthetic food carbon ammonium precipitation

The hot pure water 1.5m that in configured slot, adds 45-50 ℃ ³, open agitating vane, slowly add food carbon ammonium, add hot pure water simultaneously to 3m ³, dissolving back sampling and measuring when food carbon ammonium concentration reaches 200-220g/L, is warming up to 60 ℃ fully, pumps into the alkali lye storage tank;

C, heavy cobalt

The normal temperature pure water that adds high 20CM in first and second order reaction groove in advance adds the hot pure water of 55～60 ℃ of high 30CM, temperature in advance in third stage reactive tank; Open the agitating vane of first step reactive tank, from the cobalt liquid of cobalt liquid storage tank with the 1000L/h flow, enter first step reactive tank simultaneously with 1000～1200L/ up-flow amount from the alkali lye of alkali lye storage tank; When the pH of first step reactive tank value is 6.7～7.0, open the valve of first step reactive tank overflow port, the beginning discharge is opened the agitating vane of second stage reactive tank simultaneously to second stage reactive tank; When the slip liquid level reaches second stage reactive tank overflow port height and pH value and is 7.75～7.85, be in the groove material chemical reaction better, when generating cobaltous dihydroxycarbonate, the valve discharge of opening second stage reactive tank overflow port is to third stage reactive tank, open third stage reactive tank agitating vane simultaneously, and add 5 liters of 55～60 ℃ hot pure water and alcohol by 2000～2200L/h flow;

D, filtration, pulp, washing

When third stage reactive tank slip volume reaches 4M ³The time, be pressed into pressure filter, at first compress filter plate, make slip behind squeeze and filter, become filter cake, washing leaching cake unclamps filter plate and unloads filter cake then; When beginning, pulp adds the normal temperature pure water toward the pulp groove earlier, open agitating vane and in the pulp groove, slowly add filter cake simultaneously, the limit adds 55～60 ℃ of hot pure water limit pulps and stirred 30 minutes, accomplish pulp cmpletely, the material that pulp is good is pressed into once more and carries out filtration washing in the pressure filter, till washing no white precipitate, should be less than 0.005g/L with the chlorion that silver nitrate titration detects in the filtrate this moment;

E, protection of inert gas fragmentation

The wet cobalt carbonate hydroxide filter cake that washing of precipitate is the good oven drying at low temperature room of packing into, 65～80 ℃ of storing temperatures; After the oven dry, material is sent into crusher in crushing, feed rare gas element simultaneously in crusher, obtaining granularity is the following cobaltous dihydroxycarbonate powder of 4um;

F, malleation atmosphere are decomposed production

Series arrangement has 10 computer temperature-controlled areas in the decomposing furnace, and the controlled temperature in every district is respectively 200,260,300,350,400,480,480,400,300,250; Earlier drove furnace air 1.5～2.5 hours before the charging, successively in stove, charge into CO then with rare gas element ₂Gas, the material boat that the cobaltous dihydroxycarbonate powder is housed passes through 10 temperature-controlled areas in the stove by each 5 minutes speed, and cobaltous dihydroxycarbonate decomposes generation cobaltous oxide for power battery product, filling with inert gas during discharging in malleation atmosphere;

G, rare gas element passivation and packing