CN106830103A - A kind of production method of basic cobaltous carbonate - Google Patents
A kind of production method of basic cobaltous carbonate Download PDFInfo
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- CN106830103A CN106830103A CN201710233832.1A CN201710233832A CN106830103A CN 106830103 A CN106830103 A CN 106830103A CN 201710233832 A CN201710233832 A CN 201710233832A CN 106830103 A CN106830103 A CN 106830103A
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- deionized water
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- press filtration
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- filter cake
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/06—Carbonates
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- 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
Abstract
The invention discloses a kind of production method of basic cobaltous carbonate, the method has been achieved by the steps of the efficient pollution-free production of basic cobaltous carbonate：A, preparation Na2CO3Solution；B, synthesis；C, ageing；D, a press filtration and washing；E, secondary press filtration and washing；F, drying.The method technical matters is simple, can quickly produce basic cobaltous carbonate, meanwhile, can be good at adjusting the quality of product by controlling mixing speed, reaction temperature, the adding speed of cobalt chloride, evengranular effect is reached, cobalt content is reached 52%.Meanwhile, add additive sodium ascorbate to prevent the oxidation of product, easy press filtration, and deionized water from repeatedly washing impurity content in reduction product during reaction and in wash water, liquid is by sewage disposal reusable edible after wash water.So so that whole production procedure is simple to operate, low cost, while reducing labour intensity, production efficiency, and non-environmental-pollution are improve again, can be used for spread.
Description
Technical field
The present invention relates to chemicals preparation field, and in particular to a kind of production method of basic cobaltous carbonate.
Background technology
Basic cobaltous carbonate [2CoCO3·3Co(OH)2·H2O] it is a kind of aubergine prism sprills, it is dissolved in diluted acid and liquid
Ammonia, is practically insoluble in cold water, decomposes in the hot water, and its water solubility has much relations with pattern source.For catalyst and cobalt processed
Salt raw material, ceramic industry colouring agent, electronics, the additive of magnetic material.
Basic cobaltous carbonate is heated and easily decompose, and the product that it is decomposed is cobaltosic oxide, carbon dioxide and water.Hold due to decomposing
Easily, impurity in products is few, and will not decompose the problem that can bring nitrogen oxides as cobalt nitrate etc., is highly suitable for various cobalt materials
Processing and manufacturing.
In the evolution of the basic cobaltous carbonate mode of production, most original is to carry out production Co by semi-mechanized operation
[(OH)2]a[CO3] 1-a, but the production technology cycle is long, and washing step is time-consuming to take 3-4 days at the soonest, and technological parameter is cumbersome
Complexity, is difficult to grasp, meanwhile, drying time is long in the production technology, and temperature distributing disproportionation is even, easily causes local temperature mistake
Height, so as to influence product quality.So, then being replaced by a kind of quick basic cobaltous carbonate production technology, the processing step is big
Cause be：Dissolve, synthesize, filter, wash, dry.Wherein, cobalt chloride and sodium carbonate dissolving ratio be in mass ratio in course of dissolution
Example be：CoCl2:H2O=1:4-8, Na2CO3:H2O=1:4-8；Wherein, aqueous slkali and cobalt chloride solution are taken in building-up process
Spray mode is added, and synthesising reacting time is 2-4 hours.This technological operation is simple, with short production cycle；But the product produced
Product unstable properties, it is oxidizable, and also product particle is uneven, and cobalt tenor can only achieve 46%-50%, therefore be unfavorable for
Efficiently become more meticulous production, easily produces and greatly wastes.Now, develop again and a kind of produce alkali by way of nanometer synthesizes
Formula cobalt carbonate material, the technology is although more advanced, guaranteed to product quality, but, production cost is but very high, to equipment instrument
Device requirement is accurate, costly, therefore, the popularization of large area is also done without condition now.
The content of the invention
(1) technical problem to be solved
In view of the shortcomings of the prior art, the technical problem to be solved in the present invention is to provide a kind of producer of basic cobaltous carbonate
Method, the method has the advantages that simple to operate, low cost, while reducing labour intensity, production efficiency is improve again, and
Non-environmental-pollution, can be used for spread.
(2) technical scheme
In order to solve the above-mentioned technical problem, the invention provides the production method of such a basic cobaltous carbonate, including such as
Lower step：
A. Na is prepared2CO3Solution；Na is prepared with soda ash2CO3Solution, then by Na2CO3Solution removes deliming, magnesium through ion exchange
Ion, the Na gone after deliming, magnesium ion2CO3Solution concentration is controlled in 150g/L-200g/L, wherein, Ca<0.001g/L、Mg<
0.001g/L, then by Na2CO3Solution and deionized water are by volume 1:In 1 addition reactor, it is warming up to 75 DEG C and stirs；
B. synthesize；By CoCl2Solution is added in reactor, and is stirred, and controls the pH of reaction end in 7.7-7.9,
CoCl2With Na2CO3Mass ratio be 2.3：1, and to adding sodium ascorbate in reactor, by sodium ascorbate preventing from closing
It is oxidized in；
C. it is aged；Ripening is carried out in a kettle., and digestion time is 1.2-1.4 hours, need to be stirred continuously during ageing,
Temperature keeps constant temperature；
D. a press filtration and washing；First time press filtration is carried out after ageing, is washed with deionized after first time press filtration, washed
After the completion of take and wash the constituent contents such as water sample analysis Na, Cl, Co, to control to wash quality, until Na, Cl, Co content are controlled respectively
In ＜ 0.3g/L, ＜ 1.3g/L, ＜ 0.05g/L, filter cake is sized mixing with deionized water, the volume ratio of deionized water and filter cake is 7:
2, reactive tank is pumped into after adding sodium ascorbate, 85 DEG C are warming up to, and continue stirring 75 minutes；
E. two press filtrations and washing；Second press filtration being carried out again, being washed with deionized after second press filtration, washing is completed
After take and wash the constituent contents such as water sample analysis Na, Cl, Co, to control to wash quality, until Na, Cl, Co content are controlled in ＜ respectively
0.001g/L；
F. dry；Filter cake after second is washed is sized mixing with deionized water, and the volume ratio of deionized water and filter cake is 7:
2, it is spray-dried after adding sodium ascorbate, at 95-105 DEG C, charging rate control control is in 45- for drying temperature control
49L/min。
Preferably, in step a, Na2CO3The mixing speed of solution and deionized water is controlled in 65-75rpm.
Preferably, in stepb, the CoCl in reactor is added2Solution concentration is controlled in 100g/L-105g/L, its matter
Amount standard is required：Cu<0.001g/L、Mg<0.001g/L、Na<0.001g/L、Mn<0.001g/L、Zn<0.001g/L、Cd<
0.001g/L、Cr<0.001g/L、Pb<0.001g/L、Ni<0.001g/L、Ca<0.001g/L、Fe<0.001g/L、Al<
0.001g/L。
Preferably, in step f, the filter cake after second is washed is sized mixing with deionized water, deionized water and filter cake
Volume ratio is 7:2, it is spray-dried after adding sodium ascorbate, drying temperature control is in 100 DEG C, charging rate control control
In 47L/min.
(3) beneficial effect
Compared with prior art, the method technical matters is simple, can quickly produce basic cobaltous carbonate for the present invention, meanwhile, lead to
The quality that control mixing speed, reaction temperature, the adding speed of cobalt chloride can be good at adjusting product is crossed, particle is reached uniform
Effect, cobalt content is reached 52%.Meanwhile, add additive sodium ascorbate to prevent product during reaction and in wash water
Oxidation, easy press filtration, and deionized water repeatedly wash impurity content in reduction product, and liquid is recyclable by sewage disposal after wash water
Utilize.Product quality can reach following standard：Co52% ± 0.5, H2O≤3%, Fe≤10ppm, Mg≤10ppm, NH4≤
300ppm、Na≤100ppm、Cl≤300ppm、Ca≤10ppm、Al≤5.0ppm、Cu≤5.0ppm、Mn≤5.0ppm、Ni≤
5.0ppm, Zn≤5.0ppm, pine ratio >=0.30g/cm3.So so that whole production procedure is simple to operate, low cost, reduce
While labour intensity, production efficiency, and non-environmental-pollution are improve again, can be used for spread.
Specific embodiment
Below, clear, complete description will be carried out to the technical scheme in the embodiment of the present invention, it is clear that described reality
It is only a part of embodiment of the invention to apply example, rather than whole embodiments.Based on the embodiment in the present invention, this area
The every other embodiment that those of ordinary skill is obtained on the premise of creative work is not made, belongs to guarantor of the present invention
The scope of shield.
Embodiment 1
A kind of production method of basic cobaltous carbonate, comprises the following steps：
A. Na is prepared2CO3Solution；Na is prepared with soda ash2CO3Solution, then by Na2CO3Solution removes deliming, magnesium through ion exchange
Ion, the Na gone after deliming, magnesium ion2CO3Solution concentration is controlled in 150g/L, wherein, Ca<0.001g/L、Mg<0.001g/L,
Again by Na2CO3Solution and deionized water are by volume 1:In 1 addition reactor, it is warming up to 75 DEG C and stirs, Na2CO3Solution
Mixing speed with deionized water is controlled in 65rpm；
B. synthesize；By CoCl2Solution is added in reactor, and is stirred, and adds the CoCl in reactor2Solution concentration
In 100g/Lg/L, its quality criteria requirements is for control：Cu<0.001g/L、Mg<0.001g/L、Na<0.001g/L、Mn<
0.001g/L、Zn<0.001g/L、Cd<0.001g/L、Cr<0.001g/L、Pb<0.001g/L、Ni<0.001g/L、Ca<
0.001g/L、Fe<0.001g/L、Al<0.001g/L, controls the pH of reaction end 7.7, CoCl2With Na2CO3Mass ratio be
2.3：1, and to sodium ascorbate is added in reactor, it is oxidized in synthesizing to prevent by sodium ascorbate；
C. it is aged；Ripening is carried out in a kettle., and digestion time is 1.2 hours, need to be stirred continuously during ageing, temperature
Keep constant temperature；
D. a press filtration and washing；First time press filtration is carried out after ageing, is washed with deionized after first time press filtration, washed
After the completion of take and wash the constituent contents such as water sample analysis Na, Cl, Co, to control to wash quality, until Na, Cl, Co content are controlled respectively
In ＜ 0.3g/L, ＜ 1.3g/L, ＜ 0.05g/L, filter cake is sized mixing with deionized water, the volume ratio of deionized water and filter cake is 7:
2, reactive tank is pumped into after adding sodium ascorbate, 85 DEG C are warming up to, and continue stirring 75 minutes；
E. two press filtrations and washing；Second press filtration being carried out again, being washed with deionized after second press filtration, washing is completed
After take and wash the constituent contents such as water sample analysis Na, Cl, Co, to control to wash quality, until Na, Cl, Co content are controlled in ＜ respectively
0.001g/L；
F. dry；Filter cake after second is washed is sized mixing with deionized water, and the volume ratio of deionized water and filter cake is 7:
2, it is spray-dried after adding sodium ascorbate, at 95 DEG C, charging rate control control is in 45L/min for drying temperature control.
Embodiment 2
A kind of production method of basic cobaltous carbonate, comprises the following steps：
A. Na is prepared2CO3Solution；Na is prepared with soda ash2CO3Solution, then by Na2CO3Solution removes deliming, magnesium through ion exchange
Ion, the Na gone after deliming, magnesium ion2CO3Solution concentration is controlled in 175g/L, wherein, Ca<0.001g/L、Mg<0.001g/L,
Again by Na2CO3Solution and deionized water are by volume 1:In 1 addition reactor, it is warming up to 75 DEG C and stirs, Na2CO3Solution
Mixing speed with deionized water is controlled in 70rpm；
B. synthesize；By CoCl2Solution is added in reactor, and is stirred, and adds the CoCl in reactor2Solution concentration
In 103g/L, its quality criteria requirements is for control：Cu<0.001g/L、Mg<0.001g/L、Na<0.001g/L、Mn<0.001g/
L、Zn<0.001g/L、Cd<0.001g/L、Cr<0.001g/L、Pb<0.001g/L、Ni<0.001g/L、Ca<0.001g/L、Fe<
0.001g/L、Al<0.001g/L, controls the pH of reaction end 7.8, CoCl2With Na2CO3Mass ratio be 2.3：1, and to anti-
Answer and add sodium ascorbate in kettle, by sodium ascorbate preventing from being oxidized in synthesis；
C. it is aged；Ripening is carried out in a kettle., and digestion time is 1.3 hours, need to be stirred continuously during ageing, temperature
Keep constant temperature；
D. a press filtration and washing；First time press filtration is carried out after ageing, is washed with deionized after first time press filtration, washed
After the completion of take and wash the constituent contents such as water sample analysis Na, Cl, Co, to control to wash quality, until Na, Cl, Co content are controlled respectively
In ＜ 0.3g/L, ＜ 1.3g/L, ＜ 0.05g/L, filter cake is sized mixing with deionized water, the volume ratio of deionized water and filter cake is 7:
2, reactive tank is pumped into after adding sodium ascorbate, 85 DEG C are warming up to, and continue stirring 75 minutes；
E. two press filtrations and washing；Second press filtration being carried out again, being washed with deionized after second press filtration, washing is completed
After take and wash the constituent contents such as water sample analysis Na, Cl, Co, to control to wash quality, until Na, Cl, Co content are controlled in ＜ respectively
0.001g/L；
F. dry；Filter cake after second is washed is sized mixing with deionized water, and the volume ratio of deionized water and filter cake is 7:
2, it is spray-dried after adding sodium ascorbate, at 100 DEG C, charging rate control control is in 47L/min for drying temperature control.
Embodiment 3
A kind of production method of basic cobaltous carbonate, comprises the following steps：
A. Na is prepared2CO3Solution；Na is prepared with soda ash2CO3Solution, then by Na2CO3Solution removes deliming, magnesium through ion exchange
Ion, the Na gone after deliming, magnesium ion2CO3Solution concentration is controlled in 200g/L, wherein, Ca<0.001g/L、Mg<0.001g/L,
Again by Na2CO3Solution and deionized water are by volume 1:In 1 addition reactor, it is warming up to 75 DEG C and stirs, Na2CO3Solution
Mixing speed with deionized water is controlled in 75rpm；
B. synthesize；By CoCl2Solution is added in reactor, and is stirred, and adds the CoCl in reactor2Solution concentration
In 105g/L, its quality criteria requirements is for control：Cu<0.001g/L、Mg<0.001g/L、Na<0.001g/L、Mn<0.001g/
L、Zn<0.001g/L、Cd<0.001g/L、Cr<0.001g/L、Pb<0.001g/L、Ni<0.001g/L、Ca<0.001g/L、Fe<
0.001g/L、Al<0.001g/L, controls the pH of reaction end 7.9, CoCl2With Na2CO3Mass ratio be 2.3：1, and to anti-
Answer and add sodium ascorbate in kettle, by sodium ascorbate preventing from being oxidized in synthesis；
C. it is aged；Ripening is carried out in a kettle., and digestion time is 1.4 hours, need to be stirred continuously during ageing, temperature
Keep constant temperature；
D. a press filtration and washing；First time press filtration is carried out after ageing, is washed with deionized after first time press filtration, washed
After the completion of take and wash the constituent contents such as water sample analysis Na, Cl, Co, to control to wash quality, until Na, Cl, Co content are controlled respectively
In ＜ 0.3g/L, ＜ 1.3g/L, ＜ 0.05g/L, filter cake is sized mixing with deionized water, the volume ratio of deionized water and filter cake is 7:
2, reactive tank is pumped into after adding sodium ascorbate, 85 DEG C are warming up to, and continue stirring 75 minutes；
E. two press filtrations and washing；Second press filtration being carried out again, being washed with deionized after second press filtration, washing is completed
After take and wash the constituent contents such as water sample analysis Na, Cl, Co, to control to wash quality, until Na, Cl, Co content are controlled in ＜ respectively
0.001g/L；
F. dry；Filter cake after second is washed is sized mixing with deionized water, and the volume ratio of deionized water and filter cake is 7:
2, it is spray-dried after adding sodium ascorbate, at 105 DEG C, charging rate control control is in 49L/min for drying temperature control.
The method technical matters is simple, can quickly produce basic cobaltous carbonate, meanwhile, by controlling mixing speed, reaction temperature
Degree, the adding speed of cobalt chloride can be good at adjusting the quality of product, reach evengranular effect, cobalt content is reached
52%.Meanwhile, add during reaction and in wash water additive sodium ascorbate to prevent the oxidation of product, easy press filtration, and go from
Sub- water repeatedly washs impurity content in reduction product, and liquid is by sewage disposal reusable edible after wash water.Product quality can reach
Following standard：Co52% ± 0.5, H2O≤3%, Fe≤10ppm, Mg≤10ppm, NH4≤300ppm, Na≤100ppm, Cl≤
300ppm, Ca≤10ppm, Al≤5.0ppm, Cu≤5.0ppm, Mn≤5.0ppm, Ni≤5.0ppm, Zn≤5.0ppm, pine ratio
≥0.30g/cm3.So so that whole production procedure is simple to operate, low cost, while reducing labour intensity, improve again
Production efficiency, and non-environmental-pollution, can be used for spread.
Embodiment described above only expresses the preferred embodiment of the present invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, technical scheme that can be as described above and design can also make other various corresponding changes and deformation, and
All these changes and deformation should all belong within the protection domain of the claims in the present invention.
Claims (4)
1. a kind of production method of basic cobaltous carbonate, it is characterised in that comprise the following steps：
A. Na is prepared2CO3Solution；Na is prepared with soda ash2CO3Solution, then by Na2CO3Solution through ion exchange go deliming, magnesium from
Son, the Na gone after deliming, magnesium ion2CO3Solution concentration is controlled in 150g/L-200g/L, wherein, Ca<0.001g/L、Mg<
0.001g/L, then by Na2CO3Solution and deionized water are by volume 1:In 1 addition reactor, it is warming up to 75 DEG C and stirs；
B. synthesize；By CoCl2Solution is added in reactor, and is stirred, and controls the pH of reaction end in 7.7-7.9, CoCl2
With Na2CO3Mass ratio be 2.3：1, and to adding sodium ascorbate in reactor, by sodium ascorbate with preventing synthesis
It is oxidized；
C. it is aged；Ripening is carried out in a kettle., and digestion time is 1.2-1.4 hours, need to be stirred continuously during ageing, temperature
Keep constant temperature；
D. a press filtration and washing；First time press filtration is carried out after ageing, is washed with deionized after first time press filtration, washing is completed
After take and wash the constituent contents such as water sample analysis Na, Cl, Co, to control to wash quality, until Na, Cl, Co content are controlled in ＜ respectively
0.3g/L, ＜ 1.3g/L, ＜ 0.05g/L, filter cake is sized mixing with deionized water, and the volume ratio of deionized water and filter cake is 7:2, plus
Reactive tank is pumped into after entering sodium ascorbate, 85 DEG C is warming up to, and continue stirring 75 minutes；
E. two press filtrations and washing；Second press filtration is carried out again, is washed with deionized after second press filtration, taken after the completion of washing
The constituent contents such as water sample analysis Na, Cl, Co are washed, to control to wash quality, until Na, Cl, Co content are controlled in ＜ respectively
0.001g/L；
F. dry；Filter cake after second is washed is sized mixing with deionized water, and the volume ratio of deionized water and filter cake is 7:2, plus
It is spray-dried after entering sodium ascorbate, at 95-105 DEG C, charging rate control control is in 45-49L/ for drying temperature control
min。
2. the production method of a kind of basic cobaltous carbonate according to claim 1, it is characterised in that in step a, Na2CO3
The mixing speed of solution and deionized water is controlled in 65-75rpm.
3. the production method of a kind of basic cobaltous carbonate according to claim 1, it is characterised in that in stepb, adds anti-
Answer the CoCl in kettle2Solution concentration is controlled in 100g/L-105g/L, and its quality criteria requirements is：Cu<0.001g/L、Mg<
0.001g/L、Na<0.001g/L、Mn<0.001g/L、Zn<0.001g/L、Cd<0.001g/L、Cr<0.001g/L、Pb<
0.001g/L、Ni<0.001g/L、Ca<0.001g/L、Fe<0.001g/L、Al<0.001g/L。
4. the production method of a kind of basic cobaltous carbonate according to claim 1, it is characterised in that in step f, by second
Filter cake after secondary washing is sized mixing with deionized water, and the volume ratio of deionized water and filter cake is 7:2, carried out after adding sodium ascorbate
Spray drying, at 100 DEG C, charging rate control control is in 47L/min for drying temperature control.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110028110A (en) * | 2019-05-16 | 2019-07-19 | 赣州逸豪优美科实业有限公司 | A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore |
| CN110092421A (en) * | 2019-04-30 | 2019-08-06 | 江西理工大学 | A kind of production method of the spherical basic cobaltous carbonate of size tunable |
| CN111892094A (en) * | 2020-06-22 | 2020-11-06 | 荆门市格林美新材料有限公司 | Mass production method of low-impurity and high-solubility basic cobalt carbonate |
| CN113292109A (en) * | 2020-02-24 | 2021-08-24 | 荆门市格林美新材料有限公司 | Preparation method of low-sodium superfine cobalt carbonate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701293A (en) * | 2012-06-13 | 2012-10-03 | 赣州逸豪优美科实业有限公司 | Production method of basic cobalt carbonate |
-
2017
- 2017-04-11 CN CN201710233832.1A patent/CN106830103A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701293A (en) * | 2012-06-13 | 2012-10-03 | 赣州逸豪优美科实业有限公司 | Production method of basic cobalt carbonate |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110092421A (en) * | 2019-04-30 | 2019-08-06 | 江西理工大学 | A kind of production method of the spherical basic cobaltous carbonate of size tunable |
| CN110028110A (en) * | 2019-05-16 | 2019-07-19 | 赣州逸豪优美科实业有限公司 | A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore |
| CN113292109A (en) * | 2020-02-24 | 2021-08-24 | 荆门市格林美新材料有限公司 | Preparation method of low-sodium superfine cobalt carbonate |
| CN113292109B (en) * | 2020-02-24 | 2023-11-07 | 荆门市格林美新材料有限公司 | Preparation method of low-sodium superfine cobalt carbonate |
| CN111892094A (en) * | 2020-06-22 | 2020-11-06 | 荆门市格林美新材料有限公司 | Mass production method of low-impurity and high-solubility basic cobalt carbonate |
| CN111892094B (en) * | 2020-06-22 | 2024-04-12 | 荆门市格林美新材料有限公司 | Mass production method of low-impurity high-solubility basic cobalt carbonate |
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Application publication date: 20170613 |