CN104117686B - A kind of preparation method of cobalt powder - Google Patents

A kind of preparation method of cobalt powder Download PDF

Info

Publication number
CN104117686B
CN104117686B CN201410378434.5A CN201410378434A CN104117686B CN 104117686 B CN104117686 B CN 104117686B CN 201410378434 A CN201410378434 A CN 201410378434A CN 104117686 B CN104117686 B CN 104117686B
Authority
CN
China
Prior art keywords
cobalt
powder
preparation
sulfate solution
cobalt powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201410378434.5A
Other languages
Chinese (zh)
Other versions
CN104117686A (en
Inventor
冯小龙
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
NINGBO YANMEN NEW ENERGY Co Ltd
Original Assignee
NINGBO YANMEN NEW ENERGY Co Ltd
Filing date
Publication date
Application filed by NINGBO YANMEN NEW ENERGY Co Ltd filed Critical NINGBO YANMEN NEW ENERGY Co Ltd
Priority to CN201410378434.5A priority Critical patent/CN104117686B/en
Publication of CN104117686A publication Critical patent/CN104117686A/en
Application granted granted Critical
Publication of CN104117686B publication Critical patent/CN104117686B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The present invention relates to industrial chemicals production field, particularly to the preparation method of a kind of cobalt powder, comprise the following steps: in lithium cobalt paper, add sulphuric acid carry out acidolysis;Regulation pH value, to after 13, removes cupra matter;Adding hydrogen peroxide, then regulation pH value is to 25, and the removal of impurity is gone in filter pressing;Purification, and react prepared cobalt nitrate solution;To react with ammonium carbonate, obtain cobalt carbonate;Cobalt carbonate is dried, roasting, cooling, obtain cobalt powder.This preparation method, it is not necessary to liquid caustic soda processes lithium cobalt paper, also without adding reducing agent sulfur dioxide in acidization, replaces soda with ammonium carbonate in heavy cobalt;Use lithium cobalt paper production to prepare cobalt powder, greatly reduce production cost, and will not be to environment;And the cobalt powder prepared, has the highest hardness, high comprcssive strength, acts not only as the catalyst of secondary cell, and may apply to hard alloy additive, have, than cobalt protoxide, the scope that is more widely applied.

Description

A kind of preparation method of cobalt powder
Technical field
The present invention relates to industrial chemicals production field, in particular to the preparation method of a kind of cobalt powder.
Background technology
At present, owing to metallic cobalt price is high, so that producing ni-mh, nickel chromium triangle secondary battery catalyst-cobalt protoxide one-tenth This is prohibitively expensive, and uses lithium cobalt paper (being mainly derived from scrapping material and leftover pieces and tearing material open of man of Battery Plant generation) to do former Material, it is the most cheap that cobalt protoxide is prepared in production, moreover it is possible to reducing the pollution to environment of the lithium cobalt paper, therefore, it is by market Heat is held in both hands.Prior art produces concretely comprising the following steps of cobalt protoxide with lithium cobalt paper: first by molten for raw material alkali, then acidolysis, then carry out Purify, extract, precipitate and roasting, obtain cobalt protoxide.But, during alkali in this process for producing is molten, because having Liquid caustic soda remains in cobalt slag, causes in acid is molten, and sulfuric acid dosage increases, and production cost increases;Further, in acid is molten, because of difficult Molten cobalt exists, in addition it is also necessary to add reducing agent, and in general production process, reducing agent is sulfur dioxide, and sulfur dioxide is poisonous Gas, brings atmospheric pollution, and the physical condition of workman is also brought along impact.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of cobalt powder, to solve above-mentioned problem.
Provide the preparation method of a kind of cobalt powder in an embodiment of the present invention, comprise the following steps:
(a), in lithium cobalt paper add sulphuric acid carry out acidolysis, obtain cobalt sulfate solution;
(b), by described cobalt sulfate solution regulation pH value to 1-3, then remove cupra matter;
(c), will remove cupra matter cobalt sulfate solution add hydrogen peroxide, then regulation pH value go remove impurity to 2-5, filter pressing Matter, the cobalt sulfate solution being purified;
(d), the cobalt sulfate solution purification that will purify, and react prepared cobalt nitrate solution;
(e), by described cobalt nitrate solution heated and stirred, and add ammonium carbonate, after reaction, obtain cobalt carbonate precipitation;
(f), by described cobalt carbonate dry after in hydrogen reduction system, carry out roasting, the temperature of described roasting is 400- 600 DEG C, after roasting completes, cool down under the protection of noble gas, obtain cobalt powder.
Preferably, in described step (a), also include the filtering residue obtained after lithium cobalt paper acidolysis is carried out acidolysis again.
Preferably, in described step (a), described lithium cobalt paper is 1:0.5-8 with the mass ratio of described sulphuric acid.
Preferably, in described step (a), described filtering residue is 1:2-3 with the mass ratio of described sulphuric acid.
Preferably, in described step (c), the addition of described hydrogen peroxide is that the cobalt sulfate solution of every cubic metre adds 0.08-0.20kg hydrogen peroxide.
Preferably, in described step (d), cobalt sulfate solution is by preparing cobalt nitrate solution after P204, P507 extraction box.
Preferably, in described step (e), described ammonium carbonate is solution state, and the mass percent of sal volatile is 13- 15%, described cobalt nitrate is 1:0.4-4 with the volume ratio of described ammonium carbonate.
Preferably, in described step (f), the temperature of described drying is 115-125 DEG C.
Preferably, the preparation method of described cobalt powder also includes: under the protection of noble gas, uses vacuum pneumatic pulverizer Described cobalt powder is crushed, prepares even-grained cobalt powder.
Preferably, any one during described noble gas includes nitrogen, carbon dioxide.
The preparation method of a kind of cobalt powder that the embodiment of the present invention provides, it is not necessary to liquid caustic soda processes lithium cobalt paper, acidified In journey also without add reducing agent sulfur dioxide, in heavy cobalt, replace soda with ammonium carbonate, make cobalt sulfate solution and carbon In acid ammonium reaction, obtain rod-like crystal, beneficially the uniform cobalt powder of prepared sizes.The preparation method of the cobalt powder that the present invention provides is adopted Prepare cobalt powder with lithium cobalt paper production, greatly reduce production cost, and will not be to environment;And the cobalt powder prepared, There is the highest hardness, high comprcssive strength, act not only as the catalyst of secondary cell, and may apply to hard Alloy addition, has, than cobalt protoxide, the scope that is more widely applied.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail.
Provide the preparation method of a kind of cobalt powder in an embodiment of the present invention, comprise the following steps:
(a), in lithium cobalt paper add sulphuric acid carry out acidolysis, obtain cobalt sulfate solution;
(b), by described cobalt sulfate solution regulation pH value to 1-3, then remove cupra matter;
(c), will remove cupra matter cobalt sulfate solution add hydrogen peroxide, then regulation pH value go remove impurity to 2-5, filter pressing Matter, the cobalt sulfate solution being purified;
(d), the cobalt sulfate solution purification that will purify, and react prepared cobalt nitrate solution;
(e), by described cobalt nitrate solution heated and stirred, and add ammonium carbonate, after reaction, obtain cobalt carbonate precipitation;
(f), by described cobalt carbonate dry after in hydrogen reduction system, carry out roasting, the temperature of described roasting is 400- 600 DEG C, after roasting completes, cool down under the protection of noble gas, obtain cobalt powder.
The preparation method of a kind of cobalt powder that the embodiment of the present invention provides, it is not necessary to liquid caustic soda processes lithium cobalt paper, acidified In journey also without add reducing agent sulfur dioxide, in heavy cobalt, replace soda with ammonium carbonate, make cobalt sulfate solution and carbon In acid ammonium reaction, obtain rod-like crystal, beneficially the uniform cobalt powder of prepared sizes.The preparation method of the cobalt powder that the present invention provides is adopted Prepare cobalt powder with lithium cobalt paper production, greatly reduce production cost, and will not be to environment;And the cobalt powder prepared, There is the highest hardness, high comprcssive strength, act not only as the catalyst of secondary cell, and may apply to hard Alloy addition, has, than cobalt protoxide, the scope that is more widely applied.
The most thorough in order to extracted by the cobalt in lithium cobalt paper, the impurity obtained is less, to reduce the pollution of environment, preferably Ground, in described step (a), also includes the filtering residue obtained after lithium cobalt paper acidolysis is carried out acidolysis again.
In order to by the more preferable acidolysis of cobalt composition in lithium cobalt paper, it is preferable that in described step (a), described lithium cobalt paper with The mass ratio of described sulphuric acid is 1:0.5-8.It is highly preferred that the mass ratio of described lithium cobalt paper and described sulphuric acid is 1:2-4.Such as may be used To select 1:0.5,1:1,1:2,1:3,1:4,1:5,1:6,1:7,1:8 etc..
In order to by the more preferable acidolysis of cobalt composition in filtering residue, it is preferable that in described step (a), described filtering residue is with described The mass ratio of sulphuric acid is 1:2-3.
Specifically, in described step (b), described removal cupra matter is by copper extraction box by cobalt sulfate solution.Pass through The multitple extraction of copper extraction box, removes the cupra matter in cobalt sulfate solution.Copper extraction box concretely comprises the following steps: copper extraction box has 13 grades, the 1st, 2 grades of saponification sections, 3rd level feed clarification, the 4th, 5,6 grades of extractions, the 7th grade of spent acid settling section, wash cobalt section for the 8th, 9 grades, 10th grade of copper clarification of water, washes copper section for the 11st, 12 grades, the 13rd grade of organic clarification level.
Concrete principle is: be first high-efficiency copper extractant and liquid caustic soda generation saponification in copper extraction box, then will acidifying After cobalt sulfate solution in copper absorption on copper extractant;It is adsorbed with the high-efficiency copper extractant of a large amount of copper at 1.0mol/L Sulphuric acid in wash, during high-efficiency copper is extracted, the cobalt liquid that is mingled with washs;The high-efficiency copper extractant bringing a large amount of copper afterwards exists The sulphuric acid of 4mol/L washs, substantial amounts of copper ion is washed, form copper-bath.
The component content of the cobalt sulfate solution before and after entrance copper extraction box is as shown in Table 1 and Table 2.
Table 1 enters the component content of the cobalt sulfate solution before copper extraction box
Table 2 enters the component content of the cobalt sulfate solution after copper extraction box
As can be seen from Table 1 and Table 2, the copper content in cobalt sulfate solution is after copper extraction box processes, and its content is the lowest.
Preferably, in described step (c), the addition of described hydrogen peroxide is that the cobalt sulfate solution of every cubic metre adds 0.08-0.20kg hydrogen peroxide.Such as hydrogen peroxide can select 0.08kg, 0.10kg, 0.12kg, 0.15kg, 0.18kg, 0.20kg Deng.Hydrogen peroxide is to be ferric ion by the oxidation of divalent iron ion in cobalt sulfate solution, and then the going of follow-up iron ion Remove.
Preferably, in described step (d), cobalt sulfate solution is by preparing cobalt nitrate solution after P204, P507 extraction box.
Wherein, P204 extraction box has 34 grades, and dominant response flow process is: 2 grades of saponification, 3 grades of feed clarifications, 9 grades of extractions, and 7 Level washing, 1 grade of spent acid clarification, wash copper, manganese, 1 grade of spent acid clarification, 4 grades of washed metals, 3 grades of extractant clarifications for 4 grades.Concrete principle is: P204 extractant and liquid caustic soda generation saponification, saponification rate about 70%, the copper in the extraction section of 9 grades, P204 and solution, manganese Big quantitative response;The cobalt being mingled with the salt acid elution of 1mol/L in 7 grades of washing sections, washes copper for 4 grades, and the sulphuric acid of manganese section 2.5mol/L is washed Copper and manganese, at 4 grades with the hydrochloric acid washed metal washed metal of 6mol/L.The purpose of purification of sulphuric acids cobalt liquor is reached with this.
As shown in table 3 by component content each in cobalt sulfate solution after P204 extraction box.
Table 3 enters the component content of the cobalt sulfate solution after P204 extraction box
Element Cobalt Nickel Copper Ferrum Manganese Calcium Magnesium
Concentration (g/L) 15.7 0.68 0.0004 0.001 0.0006 0.002 0.002
P507 extraction box has 32 grades, and dominant response flow process is: 2 grades of saponification, 3 grades of feed clarifications, 7 grades of extractions, washes for 5 grades Wash, 1 grade of finished product clarification, 4 grades of washings, 1 grade of spent acid clarification, 4 grades of washed metals, 3 grades of extractant clarifications.Concrete principle is: P507 extracts Agent and liquid caustic soda generation saponification, saponification rate about 65%;7 grades of extraction sections, the big quantitative response of nickel in P507 and feed liquid, 5 grades Washing section, washs the cobalt being mingled with the nitric acid of 1.2mol/L;At 4 grades of washing sections, wash cobalt with the nitric acid of 3mol/L, form nitric acid Cobalt;4 grades of washed metal sections, with the hydrochloric acid washed metal of 6mol/L.
As shown in table 4 by component content each in cobalt nitrate solution after P507 extraction box.
Table 4 enters the component content of the cobalt nitrate solution after P507 extraction box
Element Cobalt Nickel Copper Ferrum Manganese Calcium Magnesium
Concentration (g/L) 73.5 0.001 0.001 0.001 0.001 0.006 0.003
Cobalt sulfate solution is by after P204, P507 extraction box, and its composition obtains purification and purification, and cobaltous sulfate generates nitre Acid cobalt.Using P204, P507 extraction box, cobalt sulfate solution directly carries out multitple extraction, method is easy, in the cobalt nitrate obtained Cobalt composition is the purest.
In order to preferably be reacted with ammonium carbonate by cobalt nitrate, it is preferable that in described step (e), described ammonium carbonate is molten Liquid, the mass percent of sal volatile is 13-15%, and described cobalt nitrate is 1:0.4-4 with the volume ratio of described ammonium carbonate, Prepare solid carbonic acid cobalt.Wherein, cobalt nitrate can select 1:0.4,1:1,1:2,1:3,1:4 etc. with the volume ratio of ammonium carbonate.
In the step that cobalt nitrate and ammonium carbonate react, both are 65-75 DEG C at the temperature of reaction, keep stirring in course of reaction Mixing, the speed of stirring is 25-35r/min.
In order to reduce the hardness of the cobalt carbonate obtained, empirical tests, the sal volatile of interpolation is preheated to 75-85 DEG C, then Mixing with the cobalt nitrate being heated to 70-80 DEG C, control temperature, to 65-75 DEG C, is kept stirring in course of reaction, stirring Speed is 25-35r/min, is 7.8-8.2 to pH, and reaction completes, and the cobalt carbonate hardness obtained is suitable.
In order to be evaporated faster by the moisture in cobalt carbonate, prevent the cobalt in cobalt carbonate oxidized again, it is preferable that In described step (f), the temperature of described drying is 115-125 DEG C.
Cobalt carbonate is 400-600 DEG C in temperature and carries out roasting, and cobalt carbonate can be decomposed under the reduction of hydrogen, by Step decomposition obtains metallic cobalt, empirical tests, it is preferable that the hydrogen flowing quantity being passed through in hydrogen reduction system is 4-6L/h, it is possible to very well Meet its reduction.But metallic cobalt is prone to oxidation in atmosphere, therefore, uses lazy after roasting completes during cooling Property gas is protected.Wherein, sintering temperature can select 400 DEG C, 450 DEG C, 500 DEG C, 520 DEG C, 550 DEG C, 580 DEG C, 600 DEG C Etc..
In order to prevent the cobalt powder granularity that temperature is the highest and prepared too big, it is unfavorable for follow-up crushing.Preferably, described roasting Temperature be 470-540 DEG C.Further, described roasting uses the mode being gradually lowered temperature to carry out roasting.As roasting uses Metal powder reduction stove is carried out, 470-540 DEG C is arranged to 530-540 DEG C, 515-525 DEG C, 495-505 DEG C, 475-485 DEG C, 465-470 DEG C, 465-470 DEG C of temperature section, respectively at each temperature section roasting 40-80min, i.e. can get granule size suitable Cobalt powder.Roasting enters cooling zone cooling after completing, cool down 2.5-3.5h, obtain the cobalt powder that temperature is 32-38 DEG C.
Cobalt powder granularity owing to obtaining in step (f) is uneven, in order to obtain uniform cobalt powder, needs to enter it Crushing of one step.In order to prevent cobalt powder in shattering process oxidized, it is preferable that the preparation method of described cobalt powder also includes: lazy Property gas protection under, use vacuum pneumatic pulverizer described cobalt powder is crushed, prepare even-grained cobalt powder.
Empirical tests, when noble gas is any one in nitrogen, carbon dioxide, its protected effect is good, and nitrogen and dioxy Changing carbon gas is common gas, low cost.Preferably, any one during described noble gas includes nitrogen, carbon dioxide.
Being below the preparation method specific embodiment of cobalt powder, wherein, the amount containing cobalt in the lithium cobalt paper that embodiment uses is at 35- 45%.
Embodiment 1
The preparation method of cobalt powder, comprises the following steps:
(a), in lithium cobalt paper, add sulphuric acid, the mass ratio of lithium cobalt paper and sulphuric acid is 1:0.5, and it is molten that acidolysis obtains cobaltous sulfate Liquid;Cobalt sulfate solution being crossed pressure filter, again adds sulphuric acid in filtering residue, filtering residue is 1:2 with the ratio of sulphuric acid;
(b), add mass percent be the soda ash solution of 6% as nertralizer, cobalt sulfate solution is regulated pH value to 1, Then by cobalt sulfate solution by copper extraction box, cupra matter is removed;
(c), will remove cupra matter cobalt sulfate solution add hydrogen peroxide, the addition of hydrogen peroxide is the sulphuric acid of every cubic metre Cobalt liquor adds 0.08kg hydrogen peroxide, is subsequently adding the soda ash solution that mass percent is 6%, and regulation pH value is to 2, and filter pressing is removed Impurity, the cobalt sulfate solution being purified;
(d), by the cobalt sulfate solution purified by preparing cobalt nitrate solution after P204, P507 extraction box;
(e), cobalt nitrate solution is put into heated and stirred in reactor, and add sal volatile, the matter of sal volatile Amount percent is 13%, and cobalt nitrate is 1:4 with the volume ratio of ammonium carbonate, obtains cobalt carbonate precipitation after reaction;
(f), cobalt carbonate is dried at 115 DEG C, be then placed in metal powder reduction stove, carry out in hydrogen reduction system Roasting, carries out roasting through temperature below section: 530 DEG C, 515 DEG C, 495 DEG C, 475 DEG C, 465 DEG C, 465 DEG C, each temperature section successively Roasting 80min, roasting enters cooling zone after completing and cools down under the protection of nitrogen, cools down 2.5h, obtain the cobalt that temperature is 38 DEG C Powder;
Under the protection of nitrogen, using vacuum pneumatic pulverizer to be crushed by cobalt powder, preparing even-grained, granularity is Cobalt powder about 1.2 μm.
With in lithium cobalt paper containing cobalt gauge, the yield of cobalt powder is 92%.
Prepared cobalt powder atomic absorption spectrophotometer is calculated the various impurity contents in cobalt powder;With carbon, sulfur Analyser, analyzes carbon therein, sulfur content;The purity calculating cobalt powder with minusing is 99.95%.
Embodiment 2
The preparation method of cobalt powder, comprises the following steps:
(a), in lithium cobalt paper, add sulphuric acid, the mass ratio of lithium cobalt paper and sulphuric acid is 1:4, and acidolysis obtains cobalt sulfate solution; Cobalt sulfate solution being crossed pressure filter, again adds sulphuric acid in filtering residue, filtering residue is 1:2.5 with the ratio of sulphuric acid;
(b), add mass percent be the soda ash solution of 7% as nertralizer, cobalt sulfate solution is regulated pH value to 2, Then by cobalt sulfate solution by copper extraction box, cupra matter is removed;
(c), will remove cupra matter cobalt sulfate solution add hydrogen peroxide, the addition of hydrogen peroxide is the sulphuric acid of every cubic metre Cobalt liquor adds 0.15kg hydrogen peroxide, is subsequently adding the soda ash solution that mass percent is 7%, and regulation pH value is to 3.5, and filter pressing is gone The removal of impurity, the cobalt sulfate solution being purified;
(d), by the cobalt sulfate solution purified by preparing cobalt nitrate solution after P204, P507 extraction box;
(e), cobalt nitrate solution is put into heated and stirred in reactor, and add sal volatile, the matter of sal volatile Amount percent is 14%, and cobalt nitrate is 1:0.4-4 with the volume ratio of ammonium carbonate, obtains cobalt carbonate precipitation after reaction;
(f), cobalt carbonate is dried at 120 DEG C, be then placed in metal powder reduction stove, carry out in hydrogen reduction system Roasting, carries out roasting through temperature below district: 540 DEG C, 525 DEG C, 500 DEG C, 480 DEG C, 470 DEG C, 470 DEG C, each temperature section successively Roasting 60min, roasting enters cooling zone after completing and cools down under the protection of carbon dioxide, cools down 3h, and obtaining temperature is 35 DEG C Cobalt powder;
Under the protection of carbon dioxide, use vacuum pneumatic pulverizer to be crushed by cobalt powder, prepare even-grained, grain Degree is the cobalt powder about 1.2 μm.
With in lithium cobalt paper containing cobalt gauge, the yield of cobalt powder is 95%.
Prepared cobalt powder atomic absorption spectrophotometer is calculated the various impurity contents in cobalt powder;With carbon, sulfur Analyser, analyzes carbon therein, sulfur content;The purity calculating cobalt powder with minusing is 99.98%.
Embodiment 3
The preparation method of cobalt powder, comprises the following steps:
(a), in lithium cobalt paper, add sulphuric acid, the mass ratio of lithium cobalt paper and sulphuric acid is 1:8, and acidolysis obtains cobalt sulfate solution; Cobalt sulfate solution being crossed pressure filter, again adds sulphuric acid in filtering residue, filtering residue is 1:3 with the ratio of sulphuric acid;
(b), add mass percent be the soda ash solution of 7% as nertralizer, cobalt sulfate solution is regulated pH value to 3, Then by cobalt sulfate solution by copper extraction box, cupra matter is removed;
(c), will remove cupra matter cobalt sulfate solution add hydrogen peroxide, the addition of hydrogen peroxide is the sulphuric acid of every cubic metre Cobalt liquor adds 0.20kg hydrogen peroxide, is subsequently adding the soda ash solution that mass percent is 7%, and regulation pH value is to 5, and filter pressing is removed Impurity, the cobalt sulfate solution being purified;
(d), by the cobalt sulfate solution purified by preparing cobalt nitrate solution after P204, P507 extraction box;
(e), cobalt nitrate solution is put into heated and stirred in reactor, and add sal volatile, the matter of sal volatile Amount percent is 15%, and cobalt nitrate is 1:0.4-4 with the volume ratio of ammonium carbonate, obtains cobalt carbonate precipitation after reaction;
(f), cobalt carbonate is dried at 125 DEG C, be then placed in metal powder reduction stove, carry out in hydrogen reduction system Roasting, carries out roasting through temperature below district: 540 DEG C, 525 DEG C, 505 DEG C, 485 DEG C, 470 DEG C, 470 DEG C, each temperature section successively Roasting 40min, roasting enters cooling zone after completing and cools down under the protection of nitrogen, cools down 3.5h, obtain the cobalt that temperature is 32 DEG C Powder;
Under the protection of nitrogen, using vacuum pneumatic pulverizer to be crushed by cobalt powder, preparing even-grained, granularity is Cobalt powder about 1.2 μm.
With in lithium cobalt paper containing cobalt gauge, the yield of cobalt powder is 92%.
Prepared cobalt powder atomic absorption spectrophotometer is calculated the various impurity contents in cobalt powder;With carbon, sulfur Analyser, analyzes carbon therein, sulfur content;The purity calculating cobalt powder with minusing is 99.96%.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, that is made any repaiies Change, equivalent, improvement etc., should be included within the scope of the present invention.

Claims (7)

1. the preparation method of a cobalt powder, it is characterised in that comprise the following steps:
(a), in lithium cobalt paper add sulphuric acid carry out acidolysis, obtain cobalt sulfate solution;
(b), by described cobalt sulfate solution regulation pH value to 1-3, then remove cupra matter;
(c), will remove cupra matter cobalt sulfate solution add hydrogen peroxide, then regulation pH value go the removal of impurity to 2-5, filter pressing, To the cobalt sulfate solution purified;
(d), the cobalt sulfate solution purification that will purify, and react prepared cobalt nitrate solution;
(e), by described cobalt nitrate solution heated and stirred, and add ammonium carbonate, the ammonium carbonate of interpolation is preheated to 75-85 DEG C, reaction Temperature is 65-75 DEG C, and the speed of stirring is 25-35r/min, is 7.8-8.2 to pH, and reaction completes, and obtains cobalt carbonate after reaction Precipitation;
(f), by described cobalt carbonate dry after in hydrogen reduction system, carry out roasting, the temperature of described roasting is 400-600 DEG C, After roasting completes, cool down under the protection of noble gas, obtain cobalt powder;
Under the protection of noble gas, use vacuum pneumatic pulverizer to be crushed by described cobalt powder, prepare even-grained cobalt Powder;
In described step (c), the addition of described hydrogen peroxide is that the cobalt sulfate solution of every cubic metre adds 0.08-0.20kg pair Oxygen water;
In described step (e), described ammonium carbonate is solution state, and the mass percent of sal volatile is 13%-15%, described Cobalt nitrate is 1:0.4-4 with the volume ratio of described ammonium carbonate.
The preparation method of cobalt powder the most according to claim 1, it is characterised in that in described step (a), also includes lithium The filtering residue obtained after cobalt paper acidolysis carries out acidolysis again.
The preparation method of cobalt powder the most according to claim 2, it is characterised in that in described step (a), described lithium cobalt paper It is 1:0.5-8 with the mass ratio of described sulphuric acid.
The preparation method of cobalt powder the most according to claim 3, it is characterised in that in described step (a), described filtering residue with The mass ratio of described sulphuric acid is 1:2-3.
The preparation method of cobalt powder the most according to claim 2, it is characterised in that in described step (d), cobalt sulfate solution By preparing cobalt nitrate solution after P204, P507 extraction box.
The preparation method of cobalt powder the most according to claim 2, it is characterised in that in described step (f), described drying Temperature is 115-125 DEG C.
The preparation method of cobalt powder the most according to claim 1, it is characterised in that described noble gas includes nitrogen, dioxy Change any one in carbon.
CN201410378434.5A 2014-08-01 A kind of preparation method of cobalt powder Active CN104117686B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410378434.5A CN104117686B (en) 2014-08-01 A kind of preparation method of cobalt powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410378434.5A CN104117686B (en) 2014-08-01 A kind of preparation method of cobalt powder

Publications (2)

Publication Number Publication Date
CN104117686A CN104117686A (en) 2014-10-29
CN104117686B true CN104117686B (en) 2017-01-04

Family

ID=

Similar Documents

Publication Publication Date Title
CN102206755B (en) Method for separating and recovering valuable elements from neodymium-iron-boron wastes
CN101736153B (en) Method for extracting ammonium molybdate from molybdenum concentrate by pressure ammonia leaching
Liu et al. A new process of extracting vanadium from stone coal
CN111057876B (en) Method for preparing high-purity vanadium pentoxide by microemulsion extraction
WO2015161659A1 (en) Method for simultaneously preparing high-purity vanadium and heteropolyacid catalyst
CN110284004B (en) Method for synergistically recycling copper slag and sodium sulfate waste slag
CN102560100A (en) Process for preparing high-purity superfine cobalt powder from copper-cobalt-iron alloy
CN102876896B (en) Method for recovering vanadium by decomposing vanadium extraction tailings by using sodium hydroxide solution
CN102492858A (en) Method for separating enriched nickel and cobalt from battery waste leaching solution
CN101323914A (en) Process for extracting vanadic anhydride by high calcium calcination
CN114058853B (en) Method for recovering titanium, vanadium and tungsten from waste SCR denitration catalyst
CN101956070A (en) Recovery method of molybdenum concentrates
CN101585553B (en) Method for producing vanadium pentoxide by ore containing vanadium and intermediate material containing vanadium
CN103290223A (en) Comprehensive recovery method for multiple metals of waste catalyst
CN101983925B (en) Preparation method of cerium oxide powder
CN104261473B (en) A kind of preparation method of Vanadium Pentoxide in FLAKES
CN111778398A (en) Method for extracting vanadium and tungsten from waste SCR denitration catalyst
CN102303908A (en) Method for preparing high-solubility industrial molybdenum oxide
CN112626348A (en) Method for recycling metal nickel and cobalt and preparation method of nickel-cobalt-manganese ternary solution
CN102485922A (en) Method for extracting nickel, cobalt, magnesium and iron from laterite-nickel ore under conditions of normal temperature and normal pressure and using waste residues
CN102643986A (en) Method for producing electrolytic manganese by taking pyrolusite as raw material through wet method reduction leaching
CN101705377B (en) Method for extracting vanadium from stone coal by wet-process enrichment and pyrogenic-process conversion
CN105861836B (en) A method of collecting noble metal from more metal alloy materials
CN113387387A (en) Method for preparing sodium tungstate solution by utilizing tungsten-containing waste in short process
CN104117686B (en) A kind of preparation method of cobalt powder

Legal Events

Date Code Title Description
PB01 Publication
SE01 Entry into force of request for substantive examination
GR01 Patent grant