CN108675358A - A kind of method for crystallising of cobalt chloride solution - Google Patents
A kind of method for crystallising of cobalt chloride solution Download PDFInfo
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- CN108675358A CN108675358A CN201810781819.4A CN201810781819A CN108675358A CN 108675358 A CN108675358 A CN 108675358A CN 201810781819 A CN201810781819 A CN 201810781819A CN 108675358 A CN108675358 A CN 108675358A
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- cobalt chloride
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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
- C01G51/08—Halides
- C01G51/085—Chlorides
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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
A kind of method for crystallising of cobalt chloride solution of the present invention includes the following steps：Cobalt chloride solution is concentrated by evaporation；Cobalt chloride solution after evaporation and concentration, which is placed in water-bath cool down, makes cobalt chloride crystal grain grow naturally, and the temperature of water-bath closes water-bath when being down to 30 DEG C 35 DEG C；Naturally it is filtered after the cobalt chloride crystal grain grown is carried out 15 h of nature growing the grain, 20 h at room temperature, obtains cobalt chloride crude product；Solid-liquor separation is carried out when cobalt chloride crude product temperature is down to 20 DEG C 25 DEG C, natural air drying will be carried out by the cobalt chloride crude product of solid-liquor separation, obtain the refined cobalt chloride product that grain size is larger, quality meets national standard, the cobalt chloride product percent crystallization in massecuite of acquisition is up to 60% 75%, while homogeneous grain size, crystal color are uniform.
Description
Technical field
The invention belongs to field of hydrometallurgy, and in particular to a kind of method for crystallising of cobalt chloride solution.
Background technology
The method for crystallising of traditional salt product is after saline solution is concentrated into certain weight proportion, to be placed in crystallizer,
It is passed through after cooling water makes saline solution be cooled to certain temperature to crystallizer and crystal seed is added, then carry out growing the grain, wait for that crystal seed is gradual
Solid-liquor separation is carried out after becoming bulky grain product, obtains product.The crystal seed being added in the crystallization process of traditional salt product at
Sub-prime amount directly determines the quality of product.Crystallization to cobalt chloride solution is produced using the cobalt chloride of traditional method for crystallising output
Product crystalline particle size is uneven, crystal color is uneven and percent crystallization in massecuite is low, influences the presentation quality and yield of cobalt chloride product,
And then improve production cost.
Invention content
For the purpose of the present invention aiming at insufficient existing for above-mentioned prior art, providing a kind of can make cobalt chloride crystalline particle
Uniform in size, grain color is uniform and the method for crystallising of the higher cobalt chloride solution of percent crystallization in massecuite.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of method for crystallising of cobalt chloride solution, which is characterized in that the method for crystallising includes the following steps：
(1) cobalt chloride solution is concentrated by evaporation；
(2) cobalt chloride solution after being concentrated by evaporation in step (1) is placed in water-bath cool down and makes cobalt chloride crystal grain
Naturally it grows, the temperature of the water-bath closes the water-bath when being down to 30 DEG C -35 DEG C；
(3) it is filtered after the cobalt chloride crystal grain grown naturally in step (2) being carried out nature growing the grain 15h-20h at room temperature,
Cobalt chloride crude product is obtained, the temperature of the suction filtration is 20 DEG C -25 DEG C；
(4) solid-liquor separation is carried out when the cobalt chloride crude product temperature in step (3) is down to 20 DEG C -25 DEG C, liquid will be passed through
Admittedly the cobalt chloride crude product detached carries out natural air drying, cobalt chloride product is obtained.
According to above-mentioned method for crystallising, which is characterized in that the proportion of the cobalt chloride solution after being concentrated by evaporation in step (1) is
1.48-1.56。
Beneficial effects of the present invention：The method for crystallising of the present invention is added without crystal seed in crystallization process, will not introduce other
Impurity makes the quality of product improve；Crystallization process cooling rate is slowly uniform, there is the growing the grain process of long period, final products
The particle of formation is larger, and preferable grain diameter can reach 3mm or so；The cobalt chloride product percent crystallization in massecuite that the method for the present invention obtains
Reach 60%-75%, reduces mother liquor amount；The proportion of cobalt chloride solution after evaporation and concentration is 1.48-1.56, the too low knot of proportion
Brilliant rate is low, and the particle of excessively high final products is small.
Specific implementation mode
A kind of method for crystallising of cobalt chloride solution of the present invention includes the following steps：(1) cobalt chloride solution is concentrated by evaporation,
The proportion of cobalt chloride solution after evaporation and concentration is 1.48-1.56；(2) the cobalt chloride solution table after being concentrated by evaporation in step (1)
When epitaxial occurs in face, being placed in water-bath cool down makes cobalt chloride crystal grain grow naturally, and rate of temperature fall is 8 DEG C/h-10 DEG C/h,
The initial temperature of water-bath is set as 85 DEG C/h-92 DEG C, and the temperature of water-bath closes water-bath when being down to 30 DEG C -35 DEG C；(3) will
The cobalt chloride crystal grain grown naturally in step (2) filters after carrying out nature growing the grain 15h-20h at room temperature, obtains cobalt chloride and slightly produces
Product, crude product particle is loose, and the temperature of suction filtration is 20 DEG C -25 DEG C；(4) when the cobalt chloride crude product temperature in step (3) is down to
Solid-liquor separation is carried out at 20 DEG C -25 DEG C, will carry out natural air drying by the cobalt chloride crude product of solid-liquor separation, it is equal to obtain particle
It is even, grain size is larger, quality meets the cobalt chloride product of national standard, cobalt chloride product percent crystallization in massecuite is higher, up to 60%-75%.
Explanation is further explained to the present invention with reference to specific embodiment.
Table 1 is the component and its mass percentage of the refined cobalt chloride product of national standard, and table 2 is chlorine before being concentrated by evaporation
Change the component and its concentration of cobalt liquor.
The component and its mass percentage (%) of the refined cobalt chloride product of 1 national standard of table
The component and its concentration (g/L) of cobalt chloride solution before table 2 is concentrated by evaporation
Embodiment 1
It takes and is evaporated concentration in cobalt chloride solution to beaker before the evaporation and concentration in 3.5L tables 2, after evaporation and concentration
When the proportion of cobalt chloride solution is 1.48, beaker, which is placed in water-bath, cool down makes cobalt chloride crystal grain grow naturally, cools down
Rate is 10 DEG C/h, and the initial temperature of water-bath is set as 92 DEG C, and the temperature of water-bath closes water-bath when being down to 30 DEG C；Room temperature
It is filtered to obtain cobalt chloride crude product after lower nature growing the grain 15h, the temperature of suction filtration is 25 DEG C；Cobalt chloride crude product temperature is down to
Solid-liquor separation is carried out at 25 DEG C, and cobalt chloride product is obtained by natural air drying is carried out by the cobalt chloride crude product of solid-liquor separation, it will
The weighing of cobalt chloride product, analysis ingredient, analysis result are shown in Table 3, and the percent crystallization in massecuite of cobalt chloride product is 60% and product quality is more than
The refined cobalt chloride product of national standard.
3 cobalt chloride product component of table and its mass percentage (%)
Embodiment 2
It takes and is evaporated concentration in cobalt chloride solution to beaker before the evaporation and concentration in 3.5L tables 2, after evaporation and concentration
When the proportion of cobalt chloride solution is 1.5, beaker, which is placed in water-bath, cool down makes cobalt chloride crystal grain grow naturally, cooling speed
Rate is 10 DEG C/h, and the initial temperature of water-bath is set as 92 DEG C, and the temperature of water-bath closes water-bath when being down to 30 DEG C；At room temperature
It is filtered to obtain cobalt chloride crude product after natural growing the grain 15h, the temperature of suction filtration is 23 DEG C；Cobalt chloride crude product temperature is down to 20
DEG C when carry out solid-liquor separation, by by solid-liquor separation cobalt chloride crude product carry out natural air drying obtain cobalt chloride product, by chlorine
Change the weighing of cobalt product, analysis ingredient, analysis result is shown in Table 4, and the percent crystallization in massecuite of cobalt chloride product is 63% and product quality is more than state
The refined cobalt chloride product of family's standard.
4 cobalt chloride product component of table and its mass percentage (%)
Embodiment 3
It takes and is evaporated concentration in cobalt chloride solution to beaker before the evaporation and concentration in 3.5L tables 2, after evaporation and concentration
When the proportion of cobalt chloride solution is 1.52, beaker, which is placed in water-bath, cool down makes cobalt chloride crystal grain grow naturally, cools down
Rate is 10 DEG C/h, and the initial temperature of water-bath is set as 92 DEG C, and the temperature of water-bath closes water-bath when being down to 30 DEG C；Room temperature
It is filtered to obtain cobalt chloride crude product after lower nature growing the grain 18h, the temperature of suction filtration is 20 DEG C；Cobalt chloride crude product temperature is down to
Solid-liquor separation is carried out at 20 DEG C, and cobalt chloride product is obtained by natural air drying is carried out by the cobalt chloride crude product of solid-liquor separation, it will
The weighing of cobalt chloride product, analysis ingredient, analysis result are shown in Table 5, and the percent crystallization in massecuite of cobalt chloride product is 67% and product quality is more than
The refined cobalt chloride product of national standard.
5 cobalt chloride product component of table and its mass percentage (%)
Embodiment 4
It takes and is evaporated concentration in cobalt chloride solution to beaker before the evaporation and concentration in 3.5L tables 2, after evaporation and concentration
When the proportion of cobalt chloride solution is 1.54, beaker, which is placed in water-bath, cool down makes cobalt chloride crystal grain grow naturally, cools down
Rate is 10 DEG C/h, and the initial temperature of water-bath is set as 92 DEG C, and the temperature of water-bath closes water-bath when being down to 30 DEG C；Room temperature
It is filtered to obtain cobalt chloride crude product after lower nature growing the grain 20h, the temperature of suction filtration is 20 DEG C；Cobalt chloride crude product temperature is down to
Solid-liquor separation is carried out at 20 DEG C, and cobalt chloride product is obtained by natural air drying is carried out by the cobalt chloride crude product of solid-liquor separation, it will
The weighing of cobalt chloride product, analysis ingredient, analysis result are shown in Table 6, and the percent crystallization in massecuite of cobalt chloride product is 71% and product quality is more than
The refined cobalt chloride product of national standard.
6 cobalt chloride product component of table and its mass percentage (%)
Embodiment 5
It takes and is evaporated concentration in cobalt chloride solution to beaker before the evaporation and concentration in 3.5L tables 2, after evaporation and concentration
When the proportion of cobalt chloride solution is 1.56, beaker, which is placed in water-bath, cool down makes cobalt chloride crystal grain grow naturally, cools down
Rate is 10 DEG C/h, and the initial temperature of water-bath is set as 92 DEG C, and the temperature of water-bath closes water-bath when being down to 30 DEG C；Room temperature
It is filtered to obtain cobalt chloride crude product after lower nature growing the grain 20h, the temperature of suction filtration is 20 DEG C；Cobalt chloride crude product temperature is down to
Solid-liquor separation is carried out at 20 DEG C, and cobalt chloride product is obtained by natural air drying is carried out by the cobalt chloride crude product of solid-liquor separation, it will
The weighing of cobalt chloride product, analysis ingredient, analysis result are shown in Table 7, and the percent crystallization in massecuite of cobalt chloride product is 75.2% and product quality is super
Cross the refined cobalt chloride product of national standard.
7 cobalt chloride product component of table and its mass percentage (%)
Claims (2)
1. a kind of method for crystallising of cobalt chloride solution, which is characterized in that the method for crystallising includes the following steps：
（1）Cobalt chloride solution is concentrated by evaporation；
（2）By step（1）Cobalt chloride solution after middle evaporation and concentration, which is placed in water-bath cool down, keeps cobalt chloride crystal grain natural
It grows, the temperature of the water-bath closes the water-bath when being down to 30 DEG C -35 DEG C；
（3）By step（2）The middle cobalt chloride crystal grain grown naturally filters after carrying out 15 h-20 h of nature growing the grain at room temperature, obtains
Temperature to cobalt chloride crude product, the suction filtration is 20 DEG C -25 DEG C；
（4）Work as step（3）In cobalt chloride crude product temperature carry out solid-liquor separation when being down to 20 DEG C -25 DEG C, will consolidate by liquid
The cobalt chloride crude product of separation carries out natural air drying, obtains cobalt chloride product.
2. method for crystallising according to claim 1, which is characterized in that step（1）Cobalt chloride solution after middle evaporation and concentration
Proportion be 1.48-1.56.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810781819.4A CN108675358A (en) | 2018-07-17 | 2018-07-17 | A kind of method for crystallising of cobalt chloride solution |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113046572A (en) * | 2021-03-11 | 2021-06-29 | 浙江中金格派锂电产业股份有限公司 | Cobalt chloride production process |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101543685A (en) * | 2009-03-30 | 2009-09-30 | 南通新玮镍钴科技发展有限公司 | Steam application technological process in the process for preparing the crystal cobalt chloride by cobalt chloride solution |
| CN101774651A (en) * | 2010-01-11 | 2010-07-14 | 广东光华化学厂有限公司 | Method for preparing reagent cobalt chloride hexahydrate |
| CN202346789U (en) * | 2011-10-19 | 2012-07-25 | 江西稀有稀土金属钨业集团有限公司 | System used for directly preparing anhydrous cobalt chloride powder from cobalt chloride solution |
| CN102910687A (en) * | 2012-11-07 | 2013-02-06 | 天津市化学试剂研究所 | Preparation method of superior pure cobalt chloride |
| CN103950905A (en) * | 2014-04-30 | 2014-07-30 | 金川集团股份有限公司 | Crystallization method of nickel aminosulfonate product |
| WO2015083406A1 (en) * | 2013-12-02 | 2015-06-11 | Jx日鉱日石金属株式会社 | High purity cobalt chloride and manufacturing method therefor |
-
2018
- 2018-07-17 CN CN201810781819.4A patent/CN108675358A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101543685A (en) * | 2009-03-30 | 2009-09-30 | 南通新玮镍钴科技发展有限公司 | Steam application technological process in the process for preparing the crystal cobalt chloride by cobalt chloride solution |
| CN101774651A (en) * | 2010-01-11 | 2010-07-14 | 广东光华化学厂有限公司 | Method for preparing reagent cobalt chloride hexahydrate |
| CN202346789U (en) * | 2011-10-19 | 2012-07-25 | 江西稀有稀土金属钨业集团有限公司 | System used for directly preparing anhydrous cobalt chloride powder from cobalt chloride solution |
| CN102910687A (en) * | 2012-11-07 | 2013-02-06 | 天津市化学试剂研究所 | Preparation method of superior pure cobalt chloride |
| WO2015083406A1 (en) * | 2013-12-02 | 2015-06-11 | Jx日鉱日石金属株式会社 | High purity cobalt chloride and manufacturing method therefor |
| CN103950905A (en) * | 2014-04-30 | 2014-07-30 | 金川集团股份有限公司 | Crystallization method of nickel aminosulfonate product |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113046572A (en) * | 2021-03-11 | 2021-06-29 | 浙江中金格派锂电产业股份有限公司 | Cobalt chloride production process |
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