CN108862405A - A kind of preparation method and device of low sodium cobaltosic oxide - Google Patents
A kind of preparation method and device of low sodium cobaltosic oxide Download PDFInfo
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- CN108862405A CN108862405A CN201710339742.0A CN201710339742A CN108862405A CN 108862405 A CN108862405 A CN 108862405A CN 201710339742 A CN201710339742 A CN 201710339742A CN 108862405 A CN108862405 A CN 108862405A
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- Prior art keywords
- cobaltosic oxide
- low sodium
- washing
- centrifuge
- sodium
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- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 title claims abstract description 150
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 52
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 52
- 239000011734 sodium Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 44
- 238000001354 calcination Methods 0.000 claims abstract description 39
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 36
- 230000032683 aging Effects 0.000 claims abstract description 31
- 150000001868 cobalt Chemical class 0.000 claims abstract description 27
- 239000012266 salt solution Substances 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 11
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010941 cobalt Substances 0.000 claims abstract description 8
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 58
- 239000002244 precipitate Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000004806 packaging method and process Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 3
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 3
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 15
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 235000013495 cobalt Nutrition 0.000 description 12
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 11
- 229960001484 edetic acid Drugs 0.000 description 11
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical class [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 5
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- SAXCKUIOAKKRAS-UHFFFAOYSA-N cobalt;hydrate Chemical compound O.[Co] SAXCKUIOAKKRAS-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 159000000000 sodium salts Chemical group 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Abstract
The invention discloses a kind of preparation method of low sodium cobaltosic oxide, this method is achieved by the steps of：Step 1 mixes additive and cobalt saline solution；Sodium hydroxide solution is added in mixing cobalt salt solution and is precipitated, purified, obtained cobaltosic oxide is precipitated；Step 2 carries out centrifuge washing to above-mentioned cobaltosic oxide and takes off dry；Step 3 is sintered first time centrifugal material obtained above；Step 4 carries out ageing, washing to material after calcination obtained above；Step 5 be centrifuged taking off and be done to material after washing obtained above, and low sodium cobaltosic oxide is made.The present invention also provides a kind of preparation facilities of low sodium cobaltosic oxide.The present invention first washes out the sodium of the overwhelming majority in cobaltosic oxide with centrifuge, then makes that the structure of cobaltosic oxide changes and sodium becomes easily to flow by calcination, then carry out secondary washing and separation, has just obtained the lower cobaltosic oxide of sodium content in this way；Apparatus of the present invention structure is simple, easy to operate.
Description
Technical field
The invention belongs to the technical fields of pure phase cobaltosic oxide preparation, and in particular to a kind of system of low sodium cobaltosic oxide
Preparation Method；The invention further relates to a kind of preparation facilities of low sodium cobaltosic oxide.
Background technique
In the generating process of cobaltosic oxide, when ball cobalt forms specified size, main environment substance is sodium salt, growth
Meanwhile gradually include certain content sodium salt, and the structure of ball cobalt be it is porous, specific surface area is the index of its porous measurement,
When centrifuge washs, the decline of sodium content exponentially grade, it is poorer more to arrive washing effect below, to reach acceptance value hereinafter, often needing
Want more hot water and longer wash time.And reducing sodium is current each cobalt acid lithium factory necessary to improving quality
Family requires also be continuously improved, must do thus to the technique of the washing of sodium to unwanted impurity determining in cobaltosic oxide
It improves, to improve product quality, makes and meet the product of demand instantly and forward-looking raising.
Summary of the invention
In view of this, being solved the main purpose of the present invention is to provide a kind of preparation method of low sodium cobaltosic oxide
Sodium content height, problem at high cost in the prior art.
In order to achieve the above objectives, the technical proposal of the invention is realized in this way：A kind of preparation of low sodium cobaltosic oxide
Method, this method are achieved by the steps of：
Step 1 mixes disodium EDTA and cobalt saline solution, and mixing cobalt salt solution is made；By hydroxide
Sodium solution is added in mixing cobalt salt solution and is precipitated, and precipitates purified rear obtained cobaltosic oxide；
Step 2 carries out centrifuge washing and de- dry, obtained centrifugation object for the first time to cobaltosic oxide made from the step 1
Material；
Step 3 is sintered first time centrifugal material made from the step 2, expects after calcination is made；
Step 4 carries out ageing, washing to material after calcination made from the step 3；Expect after washing is made；
Step 5 carries out centrifuge washing again and takes off to do to material after washing made from the step 4, and low sodium four is made and aoxidizes
Three cobalts.
Preferably, the step 2 is realized especially by following steps：Extremely by cobaltosic oxide made from the step 1
It is divided into 2 parts less, 2~4 centrifuge washings of every part of progress, each 5~15min of centrifuge washing.
Preferably, in the step 3, the temperature of the sintering is 600~700 DEG C.
Preferably, the step 4 is realized especially by following steps：Into aging reactor be added 30~70 DEG C pure water and
Expect after calcination made from step 3, then stirs 0.5~1.5h.
Preferably, the mass percent expected after the pure water and calcination is (3~7):1.
Preferably, additive is one of ethylenediamine tetra-acetic acid, ammonium hydroxide, citric acid in the step 1.
What another technical solution of the invention was realized in：A kind of preparation facilities of low sodium cobaltosic oxide, packet
Include reactive tank, the first centrifuge, pushed bat kiln, aging reactor, the second centrifuge, drier mixing machine, the reactive tank, the first centrifugation
Machine, pushed bat kiln, aging reactor, the second centrifuge, drier and mixing machine pass sequentially through pipeline and are connected.
It preferably, further include filter tunnel and groove body, the filter tunnel is set to the discharge outlet of reactive tank lower end, institute
State the lower section that groove body is set to filter tunnel, the bottom end of the groove body is provided with discharge gate, the discharge gate by pipeline with from
The feed inlet of scheming upper end is connected.
Preferably, first centrifuge, aging reactor, be respectively arranged with the first water inlet, at the top of the second centrifuge
Two water inlets, third water inlet, first water inlet, the second water inlet, third water inlet pass through pipeline and water system
It is connected, is provided with flow control valve on the pipeline being connected with water system.
Preferably, further include folding type packaging bag, have and mixing machine top discharge mouth phase on the folding type packaging bag
The tightening device of cooperation.
Preferably, the pipeline that the pipeline and aging reactor that the groove body is connect with the first seperator are connect with the first seperator
On be provided with pump and control valve；On the pipeline that first seperator is connect with pushed bat kiln, pushed bat kiln and aging reactor connection
It is provided on pipeline, on the pipeline that second seperator is connect with drier and in management that drier is connect with mixing machine
Control valve.
Preferably, the discharge outlet of the mixing machine lower end is provided with butterfly switch.
Compared with prior art, the present invention first washes out the sodium of the overwhelming majority in cobaltosic oxide with centrifuge, then
Make that the structure of cobaltosic oxide changes and sodium becomes easily to flow by calcination, then carries out secondary washing and separation, so just
The lower cobaltosic oxide of sodium content is arrived；The method of the present invention not only saves water resource, reduces cost, and improves four oxidations three
The utilization rate of cobalt；Apparatus of the present invention structure is simple, easy to operate, and be worth promoting use.
Detailed description of the invention
Fig. 1 is a kind of preparation facilities structural schematic diagram of low sodium cobaltosic oxide provided in an embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The embodiment of the present invention provides a kind of preparation method of low sodium cobaltosic oxide, and this method is achieved by the steps of：
Step 1 mixes disodium EDTA and cobalt saline solution, and mixing cobalt salt solution is made；By hydroxide
Sodium solution is added in mixing cobalt salt solution and is precipitated, and precipitates purified rear obtained cobaltosic oxide；
Cobaltosic oxide made from the step 1 is at least divided into 2 parts by step 2,2~4 centrifuge washings of every part of progress,
Each 5~15min of centrifuge washing is simultaneously de- dry, and first time centrifugal material is made；
Step 3 is sintered first time centrifugal material made from the step 2 at 600~700 DEG C, and calcination is made
After expect；
Expect after calcination made from step 4, the pure water that 30~70 DEG C are added into aging reactor and step 3, then stir 0.5~
1.5h expects after washing is made；The mass percent wherein expected after pure water and calcination is (3~7):1
Step 5 carries out centrifuge washing again and de- dry (the same step 2 of method, system to material after washing made from the step 4
Obtain low sodium cobaltosic oxide.
Preliminary cobaltosic oxide material obtained is mingled with micro hydroxyl cobalt (CoOOH), this hydroxyl cobalt (CoOOH) structure
Cause sodium washing unclean, the present invention is under above-mentioned sintering condition and guarantees that the crystal structure of cobaltosic oxide does not change
In the case where, so that micro hydroxyl cobalt (CoOOH) is decomposed, so that the easy stream that sodium becomes, eventually by complete after secondary washing and centrifugation
Portion is transformed into the lower cobaltosic oxide of sodium content.
The embodiment of the invention also provides a kind of preparation facilities of low sodium cobaltosic oxide comprising reactive tank 1, first from
Scheming 2, pushed bat kiln 3, aging reactor 4, the second centrifuge 5, drier 6, mixing machine 7, the reactive tank 1, push away first centrifuge 2
Plate kiln 3, aging reactor 4, the second centrifuge 5, drier 6 and mixing machine 7 pass sequentially through pipeline and are connected.
It further, further include filter tunnel 11 and groove body 12, the filter tunnel 11 is set to going out for 1 lower end of reactive tank
At material mouth, groove body 12 is set to the lower section of filter tunnel 11, and the bottom end of groove body 12 is provided with discharge gate 121, and discharge gate 121 passes through
Pipeline is connected with the feed inlet of centrifuge upper end.
Further, the first centrifuge 2, aging reactor 4, the second centrifuge 6 top be respectively arranged with the first water inlet 21,
Second water inlet 41, third water inlet 51, the first water inlet 21, the second water inlet 41, third water inlet 51 by pipeline with
Water system 8 is connected, and is provided with flow control valve on the pipeline being connected with water system 8.
Further, further include folding type packaging bag 9, have and 7 top discharge mouth phase of mixing machine on folding type packaging bag 9
The tightening device 91 of cooperation.
Further, what the pipeline and aging reactor 4 that groove body 12 is connect with the first seperator 2 were connect with the first seperator 5
Pump and control valve are provided on pipeline；On the pipeline that first seperator 2 is connect with pushed bat kiln 3, pushed bat kiln 3 and aging reactor 4 connect
It is set on the pipeline connect, on the pipeline that the second seperator 5 is connect with drier 6 and in management that drier 6 is connect with mixing machine 7
It is equipped with control valve.
Further, the discharge outlet of 7 lower end of mixing machine is provided with butterfly switch 71.
Compared with prior art, the present invention first washes out the sodium of the overwhelming majority in cobaltosic oxide with centrifuge, then
Make that the structure of cobaltosic oxide changes and sodium becomes easily to flow by calcination, then carries out secondary washing and separation, so just
The lower cobaltosic oxide of sodium content is arrived；The method of the present invention not only saves water resource, reduces cost, and improves four oxidations three
The utilization rate of cobalt；Apparatus of the present invention structure is simple, easy to operate, and be worth promoting use.
Embodiment 1
1) cobalt salt solution and sodium hydroxide solution are prepared first, and ethylenediamine tetrem is added into configured cobalt salt solution
Acid disodium salt stirs evenly, and the cobalt salt solution containing ethylenediamine tetra-acetic acid is made；2) 3L pure water is added into reactive tank 1, and adds
Above-mentioned sodium hydroxide solution and the cobalt salt solution containing ethylenediamine tetra-acetic acid are added in reactive tank 1 and are precipitated to 73 DEG C by heat,
Precipitate purified, obtained cobaltosic oxide；3) control valve for opening 1 lower end discharge outlet of reactive tank, to four oxidation obtained
Three cobalts are filtered, and obtain filtered cobaltosic oxide, open pump will be pumped into for filtered cobaltosic oxide point 3 times first from
Scheming 2 carries out centrifuge washing, washs 10min every time, obtains first time centrifugal material；4) first time centrifugal material is sent into push plate
Kiln 3 carries out calcination at 660 DEG C, expects after calcination is made；5) a certain amount of 50 DEG C of pure water is added into aging reactor 4, then takes
Material is added in aging reactor 4 after a certain amount of calcination, guarantees that the mass percent expected after pure water and calcination is 5:1 (the present embodiment is pure
The amount of water is 10m3, the amount expected after calcination is 2000kg), 60min is stirred, is expected after being washed；6) will expect to divide 3 again after washing
Secondary second centrifuge that is pumped into carries out centrifuge washing, washs 10min every time, low sodium cobaltosic oxide is made.
The cobaltosic oxide that embodiment 1 obtains is dried, is closed and is criticized and detect, the content for obtaining sodium is 0.015%, water
The material of part≤0.1%.
Embodiment 2
1) cobalt salt solution and sodium hydroxide solution are prepared first, and ethylenediamine tetrem is added into configured cobalt salt solution
Acid disodium salt stirs evenly, and the cobalt salt solution containing ethylenediamine tetra-acetic acid is made；2) 3L pure water is added into reactive tank 1, and adds
Above-mentioned sodium hydroxide solution and the cobalt salt solution containing ethylenediamine tetra-acetic acid are added in reactive tank 1 and are precipitated to 73 DEG C by heat,
Precipitate purified, obtained cobaltosic oxide；3) control valve for opening 1 lower end discharge outlet of reactive tank, to four oxidation obtained
Three cobalts are filtered, and obtain filtered cobaltosic oxide, open pump will be pumped into for filtered cobaltosic oxide point 4 times first from
Scheming 2 carries out centrifuge washing, washs 5min every time, obtains first time centrifugal material；4) first time centrifugal material is sent into push plate
Kiln 3 carries out calcination at 600 DEG C, expects after calcination is made；5) a certain amount of 30 DEG C of pure water is added into aging reactor 4, then takes
Material is added in aging reactor 4 after a certain amount of calcination, guarantees that the mass percent expected after pure water and calcination is 3:1 (the present embodiment is pure
The amount of water is 6m3, the amount expected after calcination is 2000kg), 30min is stirred, is expected after being washed；6) will expect to divide 4 again after washing
Secondary second centrifuge that is pumped into carries out centrifuge washing, washs 5min every time, low sodium cobaltosic oxide is made.
The cobaltosic oxide that embodiment 1 obtains is dried, is closed and is criticized and detect, the content for obtaining sodium is 0.021%, water
The material of part≤0.1%.
Embodiment 3
1) cobalt salt solution and sodium hydroxide solution are prepared first, and ethylenediamine tetrem is added into configured cobalt salt solution
Acid disodium salt stirs evenly, and the cobalt salt solution containing ethylenediamine tetra-acetic acid is made；2) 3L pure water is added into reactive tank 1, and adds
Above-mentioned sodium hydroxide solution and the cobalt salt solution containing ethylenediamine tetra-acetic acid are added in reactive tank 1 and are precipitated to 73 DEG C by heat,
Precipitate purified, obtained cobaltosic oxide；3) control valve for opening 1 lower end discharge outlet of reactive tank, to four oxidation obtained
Three cobalts are filtered, and obtain filtered cobaltosic oxide, open pump will be pumped into for filtered cobaltosic oxide point 2 times first from
Scheming 2 carries out centrifuge washing, washs 15min every time, obtains first time centrifugal material；4) first time centrifugal material is sent into push plate
Kiln 3 carries out calcination at 700 DEG C, expects after calcination is made；5) a certain amount of 70 DEG C of pure water is added into aging reactor 4, then takes
Material is added in aging reactor 4 after a certain amount of calcination, guarantees that the mass percent expected after pure water and calcination is 7:1 (the present embodiment is pure
The amount of water is 14m3, the amount expected after calcination is 2000kg), 120min is stirred, is expected after being washed；6) will expect to divide again after washing
It is pumped into the second centrifuge for 2 times and carries out centrifuge washing, wash 15min every time, low sodium cobaltosic oxide is made.
The cobaltosic oxide that embodiment 1 obtains is dried, is closed and is criticized and detect, the content for obtaining sodium is 0.019%, water
The material of part≤0.1%.
Embodiment 4
1) cobalt salt solution and sodium hydroxide solution are prepared first, and ethylenediamine tetrem is added into configured cobalt salt solution
Acid disodium salt stirs evenly, and the cobalt salt solution containing ethylenediamine tetra-acetic acid is made；2) 3L pure water is added into reactive tank 1, and adds
Above-mentioned sodium hydroxide solution and the cobalt salt solution containing ethylenediamine tetra-acetic acid are added in reactive tank 1 and are precipitated to 73 DEG C by heat,
Precipitate purified, obtained cobaltosic oxide；3) control valve for opening 1 lower end discharge outlet of reactive tank, to four oxidation obtained
Three cobalts are filtered, and obtain filtered cobaltosic oxide, open pump will be pumped into for filtered cobaltosic oxide point 3 times first from
Scheming 2 carries out centrifuge washing, washs 10min every time, obtains first time centrifugal material；4) first time centrifugal material is sent into push plate
Kiln 3 carries out calcination at 700 DEG C, expects after calcination is made；5) a certain amount of 70 DEG C of pure water is added into aging reactor 4, then takes
Material is added in aging reactor 4 after a certain amount of calcination, guarantees that the mass percent expected after pure water and calcination is 5:1 (the present embodiment is pure
The amount of water is 10m3, the amount expected after calcination is 2000kg), 60min is stirred, is expected after being washed；6) will expect to divide 3 again after washing
Secondary second centrifuge that is pumped into carries out centrifuge washing, washs 10min every time, low sodium cobaltosic oxide is made.
The cobaltosic oxide that embodiment 1 obtains is dried, is closed and is criticized and detect, the content for obtaining sodium is 0.016%, water
The material of part≤0.1%.
Embodiment 5
1) cobalt salt solution and sodium hydroxide solution are prepared first, and ethylenediamine tetrem is added into configured cobalt salt solution
Acid disodium salt stirs evenly, and the cobalt salt solution containing ethylenediamine tetra-acetic acid is made；2) 3L pure water is added into reactive tank 1, and adds
Above-mentioned sodium hydroxide solution and the cobalt salt solution containing ethylenediamine tetra-acetic acid are added in reactive tank 1 and are precipitated to 73 DEG C by heat,
Precipitate purified, obtained cobaltosic oxide；3) control valve for opening 1 lower end discharge outlet of reactive tank, to four oxidation obtained
Three cobalts are filtered, and obtain filtered cobaltosic oxide, open pump will be pumped into for filtered cobaltosic oxide point 3 times first from
Scheming 2 carries out centrifuge washing, washs 10min every time, obtains first time centrifugal material；4) first time centrifugal material is sent into push plate
Kiln 3 carries out calcination at 600 DEG C, expects after calcination is made；5) a certain amount of 70 DEG C of pure water is added into aging reactor 4, then takes
Material is added in aging reactor 4 after a certain amount of calcination, guarantees that the mass percent expected after pure water and calcination is 7:1 (the present embodiment is pure
The amount of water is 14m3, the amount expected after calcination is 2000kg), 120min is stirred, is expected after being washed；6) will expect to divide again after washing
It is pumped into the second centrifuge for 3 times and carries out centrifuge washing, wash 10min every time, low sodium cobaltosic oxide is made.
The cobaltosic oxide that embodiment 1 obtains is dried, is closed and is criticized and detect, the content for obtaining sodium is 0.022%, water
The material of part≤0.1%.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention.
Claims (10)
1. a kind of preparation method of low sodium cobaltosic oxide, which is characterized in that this method is achieved by the steps of：
Step 1 mixes disodium EDTA and cobalt saline solution, and mixing cobalt salt solution is made；Sodium hydroxide is molten
Liquid is added in mixing cobalt salt solution and is precipitated, and precipitates purified rear obtained cobaltosic oxide；
Step 2 carries out centrifuge washing and de- dry, obtained first time centrifugal material to cobaltosic oxide made from the step 1；
Step 3 is sintered first time centrifugal material made from the step 2, expects after calcination is made；
Step 4 carries out ageing, washing to material after calcination made from the step 3；Expect after washing is made；
Step 5 carries out centrifuge washing again and takes off to do to material after washing made from the step 4, and low sodium cobaltosic oxide is made.
2. a kind of preparation method of low sodium cobaltosic oxide according to claim 1, which is characterized in that step 2 tool
Body is realized by following steps：Cobaltosic oxide made from the step 1 is at least divided into 2 parts, every part carry out 2~4 times from
Heart washing, each 5~15min of centrifuge washing.
3. a kind of preparation method of low sodium cobaltosic oxide according to claim 1, which is characterized in that in the step 3,
The temperature of the sintering is 600~700 DEG C.
4. a kind of preparation method of low sodium cobaltosic oxide according to claim 1, which is characterized in that step 4 tool
Body is realized by following steps：Be added into aging reactor 30~70 DEG C pure water and step 3 made from expect after calcination, then stir
Mix 0.5~1.5h.
5. a kind of preparation method of low sodium cobaltosic oxide according to claim 1, which is characterized in that the pure water and burn
The mass percent expected after burning is (3~7):1.
6. a kind of preparation facilities of low sodium cobaltosic oxide, which is characterized in that it include reactive tank, the first centrifuge, pushed bat kiln,
Aging reactor, the second centrifuge, drier, mixing machine, the reactive tank, the first centrifuge, pushed bat kiln, aging reactor, the second centrifugation
Machine, drier and mixing machine pass sequentially through pipeline and are connected.
7. a kind of preparation facilities of low sodium cobaltosic oxide according to claim 6, which is characterized in that further include filtering leakage
Bucket and groove body, the filter tunnel are set to the discharge outlet of reactive tank lower end, and the groove body is set to the lower section of filter tunnel,
The bottom end of the groove body is provided with discharge gate, and the discharge gate is connected by pipeline with the feed inlet of centrifuge upper end.
8. a kind of preparation facilities of low sodium cobaltosic oxide according to claim 7, which is characterized in that first centrifugation
Machine, aging reactor are respectively arranged with the first water inlet, the second water inlet, third water inlet at the top of the second centrifuge, and described first
Water inlet, the second water inlet, third water inlet pass through pipeline and be connected with water system, described to be connected with water system
Flow control valve is provided on pipeline.
9. a kind of preparation facilities of low sodium cobaltosic oxide according to claim 8, which is characterized in that it further includes folding
Formula packaging bag has the tightening device matched with mixing machine top discharge mouth on the folding type packaging bag.
10. according to a kind of preparation facilities of any low sodium cobaltosic oxide of claim 6-9, which is characterized in that described
Pump and control valve are provided on the pipeline that the pipeline and aging reactor that groove body is connect with the first seperator are connect with the first seperator
Door；On the pipeline that first seperator is connected with pushed bat kiln, on the pipeline that pushed bat kiln is connected with aging reactor, described second separate
Control valve is provided on the pipeline that machine is connect with drier and in management that drier is connect with mixing machine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710339742.0A CN108862405A (en) | 2017-05-15 | 2017-05-15 | A kind of preparation method and device of low sodium cobaltosic oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710339742.0A CN108862405A (en) | 2017-05-15 | 2017-05-15 | A kind of preparation method and device of low sodium cobaltosic oxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408500A (en) * | 2020-11-26 | 2021-02-26 | 格林美（江苏）钴业股份有限公司 | Production method of battery-grade cobalt oxide |
| CN112645393A (en) * | 2020-12-21 | 2021-04-13 | 格林美（江苏）钴业股份有限公司 | Preparation method of cobaltosic oxide |
Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20010046015A (en) * | 1999-11-09 | 2001-06-05 | 김원배 | Manufacturig method of alumina powder |
| JP2007055817A (en) * | 2005-08-22 | 2007-03-08 | Dainichiseika Color & Chem Mfg Co Ltd | Particulate tricobalt tetroxide pigment, and method for producing the same |
| CN101434416A (en) * | 2008-11-28 | 2009-05-20 | 宁波金和新材料有限公司 | Hydroxy spherical cobaltosic oxide and preparation thereof |
| CN102259934A (en) * | 2011-05-17 | 2011-11-30 | 周红阳 | Process for producing high-density spherical cobaltosic oxide by virtue of low temperature liquid phase precipitation oxidization |
| CN103224257A (en) * | 2012-11-28 | 2013-07-31 | 江苏大学 | Method for preparing Co3O4 from waste and old lithium ion batteries |
| CN103255288A (en) * | 2012-02-17 | 2013-08-21 | 苏州艾默特材料技术有限公司 | Purification method of industrial molybdenum powder |
| CN103506127A (en) * | 2012-06-30 | 2014-01-15 | 中国石油化工股份有限公司 | Preparation method of low-sodium copper zinc aluminum hydrogenation catalyst |
| CN103771442A (en) * | 2012-10-19 | 2014-05-07 | 中国石油化工股份有限公司 | Y-type molecular sieve modification method and catalytic cracking catalyst preparation method |
| CN103803663A (en) * | 2012-11-06 | 2014-05-21 | 宁波科博特钴镍有限公司 | Production method of spherical tricobalt tetroxide |
| CN104134786A (en) * | 2014-07-28 | 2014-11-05 | 宁波金和新材料股份有限公司 | Method for preparing small-particle size high-density spherical cobalt (II,III) oxide |
| CN104986807A (en) * | 2015-04-23 | 2015-10-21 | 金川集团股份有限公司 | Spherical tricobalt tetraoxide preparation method |
| CN105668650A (en) * | 2016-03-23 | 2016-06-15 | 荆门市格林美新材料有限公司 | Method for preparing low-sodium cobaltosic oxide |
| CN105776356A (en) * | 2016-03-22 | 2016-07-20 | 阳江市联邦金属化工有限公司 | Preparation method of spherical compact tricobalt tetroxide |
| CN106082358A (en) * | 2016-06-22 | 2016-11-09 | 荆门市格林美新材料有限公司 | The preparation method of Cobalto-cobaltic oxide |
-
2017
- 2017-05-15 CN CN201710339742.0A patent/CN108862405A/en active Pending
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20010046015A (en) * | 1999-11-09 | 2001-06-05 | 김원배 | Manufacturig method of alumina powder |
| JP2007055817A (en) * | 2005-08-22 | 2007-03-08 | Dainichiseika Color & Chem Mfg Co Ltd | Particulate tricobalt tetroxide pigment, and method for producing the same |
| CN101434416A (en) * | 2008-11-28 | 2009-05-20 | 宁波金和新材料有限公司 | Hydroxy spherical cobaltosic oxide and preparation thereof |
| CN102259934A (en) * | 2011-05-17 | 2011-11-30 | 周红阳 | Process for producing high-density spherical cobaltosic oxide by virtue of low temperature liquid phase precipitation oxidization |
| CN103255288A (en) * | 2012-02-17 | 2013-08-21 | 苏州艾默特材料技术有限公司 | Purification method of industrial molybdenum powder |
| CN103506127A (en) * | 2012-06-30 | 2014-01-15 | 中国石油化工股份有限公司 | Preparation method of low-sodium copper zinc aluminum hydrogenation catalyst |
| CN103771442A (en) * | 2012-10-19 | 2014-05-07 | 中国石油化工股份有限公司 | Y-type molecular sieve modification method and catalytic cracking catalyst preparation method |
| CN103803663A (en) * | 2012-11-06 | 2014-05-21 | 宁波科博特钴镍有限公司 | Production method of spherical tricobalt tetroxide |
| CN103224257A (en) * | 2012-11-28 | 2013-07-31 | 江苏大学 | Method for preparing Co3O4 from waste and old lithium ion batteries |
| CN104134786A (en) * | 2014-07-28 | 2014-11-05 | 宁波金和新材料股份有限公司 | Method for preparing small-particle size high-density spherical cobalt (II,III) oxide |
| CN104986807A (en) * | 2015-04-23 | 2015-10-21 | 金川集团股份有限公司 | Spherical tricobalt tetraoxide preparation method |
| CN105776356A (en) * | 2016-03-22 | 2016-07-20 | 阳江市联邦金属化工有限公司 | Preparation method of spherical compact tricobalt tetroxide |
| CN105668650A (en) * | 2016-03-23 | 2016-06-15 | 荆门市格林美新材料有限公司 | Method for preparing low-sodium cobaltosic oxide |
| CN106082358A (en) * | 2016-06-22 | 2016-11-09 | 荆门市格林美新材料有限公司 | The preparation method of Cobalto-cobaltic oxide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408500A (en) * | 2020-11-26 | 2021-02-26 | 格林美（江苏）钴业股份有限公司 | Production method of battery-grade cobalt oxide |
| CN112645393A (en) * | 2020-12-21 | 2021-04-13 | 格林美（江苏）钴业股份有限公司 | Preparation method of cobaltosic oxide |
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