CN114405053A - Method for crystallizing manganese sulfate solution based on ethanol method - Google Patents
Method for crystallizing manganese sulfate solution based on ethanol method Download PDFInfo
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- CN114405053A CN114405053A CN202210095066.8A CN202210095066A CN114405053A CN 114405053 A CN114405053 A CN 114405053A CN 202210095066 A CN202210095066 A CN 202210095066A CN 114405053 A CN114405053 A CN 114405053A
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- CN
- China
- Prior art keywords
- manganese sulfate
- sulfate solution
- crystallizing
- ethanol
- ethyl alcohol
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 235000007079 manganese sulphate Nutrition 0.000 title claims abstract description 81
- 239000011702 manganese sulphate Substances 0.000 title claims abstract description 81
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 title claims abstract description 81
- 229940099596 manganese sulfate Drugs 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 60
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 235000019441 ethanol Nutrition 0.000 claims abstract description 22
- 238000002425 crystallisation Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000003825 pressing Methods 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 230000008025 crystallization Effects 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 7
- 238000005070 sampling Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 4
- SQUHHTBVTRBESD-UHFFFAOYSA-N Hexa-Ac-myo-Inositol Natural products CC(=O)OC1C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C1OC(C)=O SQUHHTBVTRBESD-UHFFFAOYSA-N 0.000 claims 1
- CDAISMWEOUEBRE-GPIVLXJGSA-N inositol Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@@H]1O CDAISMWEOUEBRE-GPIVLXJGSA-N 0.000 claims 1
- 229960000367 inositol Drugs 0.000 claims 1
- CDAISMWEOUEBRE-UHFFFAOYSA-N scyllo-inosotol Natural products OC1C(O)C(O)C(O)C(O)C1O CDAISMWEOUEBRE-UHFFFAOYSA-N 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 125000004122 cyclic group Chemical group 0.000 abstract description 3
- 238000004821 distillation Methods 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 238000009854 hydrometallurgy Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 9
- 230000007547 defect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000008040 ionic compounds Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/10—Sulfates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
- B01D2009/009—Separation of organic compounds by selective or extractive crystallisation with the aid of auxiliary substances forming complex or molecular compounds, e.g. with ureum, thioureum or metal salts
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for crystallizing a manganese sulfate solution based on an ethanol method, and relates to the technical field of hydrometallurgy. The method for crystallizing the manganese sulfate solution based on the ethanol method comprises the following steps: the method for crystallizing the manganese sulfate solution by the ethanol method comprises the following steps: s1, putting a certain amount of manganese sulfate solution into a reaction container, and fully stirring at normal temperature; s2, slowly adding absolute ethyl alcohol into the reaction container, and stopping adding the absolute ethyl alcohol when the supernatant is colorless and transparent; and S3, after being fully and uniformly mixed in the reaction container, carrying out filter pressing on the mixture by using a filter press to obtain manganese sulfate crystals. Adding absolute ethanol which is an organic solvent with weak polarity into the manganese sulfate solution to separate solid manganese sulfate from the solution. Compared with the existing manganese sulfate crystallization method, the method is simple and convenient to operate, almost has no energy consumption, has low requirements on equipment, and can continuously add the subsequent filter-pressed solution into the manganese sulfate solution after distillation, thereby realizing the cyclic utilization of absolute ethyl alcohol.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a method for crystallizing a manganese sulfate solution based on an ethanol method.
Background
Manganese sulfate is increasingly regarded as the most important and basic manganese source material of the positive electrode material of the manganese-series power lithium battery. The traditional manganese sulfate solution crystallization mainly comprises methods such as evaporation concentration, high-temperature crystallization, recrystallization and the like. For preparing manganese sulfate crystals by a concentration method, the aim of concentrating and crystallizing manganese sulfate is mainly achieved by heating a solution to continuously evaporate a solvent. However, when isothermal crystallization is carried out, fine manganese sulfate crystal particles are formed on the heat transfer surface, the heat conductivity coefficient is reduced, and the subsequent energy consumption is obviously increased. Meanwhile, the content of impurities such as calcium, magnesium and the like in the solution can be increased along with the reduction of the solvent, so that the subsequent manganese sulfate is not completely crystallized, and a residual part of high-concentration manganese sulfate mother liquor needs to be further treated, thereby increasing the production cost. In the case of the high-temperature crystallization method, the solubility of manganese sulfate is sharply reduced when the temperature exceeds 100 ℃, and the solution can be heated by direct steam with certain pressure in an autoclave to separate out the manganese sulfate. Only a small amount of manganese sulfate remains in the mother liquor, which is discharged through a filter installed under the autoclave, and then another new batch of solution is injected into the autoclave, and the salt is discharged after two or three crystallization operations. However, the method needs to be carried out at high temperature and high pressure, the requirements on the material and quality of equipment are high, otherwise, the safe operation of the system is influenced, and further, serious production accidents are caused.
Manganese sulfate crystallization in the existing market mainly adopts a concentration method and a high-temperature crystallization method, and has the disadvantages of great defect, high energy consumption, long process flow and low production efficiency under the condition of heating.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for crystallizing a manganese sulfate solution based on an ethanol method, which solves the problems of large energy consumption, long process flow and low production efficiency of manganese sulfate crystallization production.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a method for crystallizing a manganese sulfate solution based on an ethanol method comprises the following steps:
the method for crystallizing the manganese sulfate solution by the ethanol method comprises the following steps:
s1, putting a certain amount of manganese sulfate solution into a reaction container, and fully stirring at normal temperature;
s2, slowly adding absolute ethyl alcohol into the reaction container, and stopping adding the absolute ethyl alcohol when the supernatant is colorless and transparent;
and S3, after being fully and uniformly mixed in the reaction container, carrying out filter pressing on the mixture by using a filter press to obtain manganese sulfate crystals.
Preferably, the concentration of the manganese sulfate solution in S1 is more than 150 g/L.
Preferably, the volume ratio of the addition amount of the absolute ethyl alcohol to the addition amount of the manganese sulfate solution in the S2 is more than 1.0.
Preferably, the reaction vessel is one of a beaker and a reaction kettle
Preferably, the method for crystallizing the manganese sulfate solution based on the ethanol method specifically comprises the following steps:
s101, adding 200ml of manganese sulfate solution into a beaker, and stirring at normal temperature;
s102, slowly adding 200 and 350ml of absolute ethyl alcohol;
s103, after fully and uniformly stirring, performing filter pressing and drying;
s104, sampling and detecting. The crystallization rate of the manganese sulfate is measured to be 68.75-88.49%.
Preferably, the normal temperature stirring in the step S101 is performed at a normal temperature of 20-28 ℃, and the normal temperature stirring in the step S101 may be performed under a sealed condition.
(III) advantageous effects
The invention provides a method for crystallizing a manganese sulfate solution based on an ethanol method. The method has the following beneficial effects:
in the invention, as can be seen from the principle of similar phase solubility, ionic compounds with strong polarity are hardly dissolved in organic solvents with weak polarity, and solid manganese sulfate is separated out of the solution by adding absolute ethanol which is an organic solvent with weak polarity into the manganese sulfate solution. Compared with the existing manganese sulfate crystallization method, the method is simple and convenient to operate, almost has no energy consumption, has low requirements on equipment, and can continuously add the subsequent filter-pressed solution into the manganese sulfate solution after distillation, thereby realizing the cyclic utilization of absolute ethyl alcohol. Short process flow, high production efficiency and high production and application values.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
the embodiment of the invention provides a method for crystallizing a manganese sulfate solution based on an ethanol method, which comprises the following steps:
the method for crystallizing the manganese sulfate solution by the ethanol method comprises the following steps:
s1, putting a certain amount of manganese sulfate solution into a reaction container, and fully stirring at normal temperature;
s2, slowly adding absolute ethyl alcohol into the reaction container, and stopping adding the absolute ethyl alcohol when the supernatant is colorless and transparent;
s3, after fully and uniformly mixing the manganese sulfate solution and the manganese sulfate solution in the reaction container, carrying out filter pressing on the manganese sulfate solution by using a filter press to obtain manganese sulfate crystals, wherein according to the principle of similarity and intermiscibility, ionic compounds with strong polarity are almost insoluble in organic solvents with weak polarity, and solid manganese sulfate is separated out of the manganese sulfate solution by adding absolute ethyl alcohol which is an organic solvent with weak polarity into the manganese sulfate solution. Compared with the existing manganese sulfate crystallization method, the method is simple and convenient to operate, almost has no energy consumption, has low requirements on equipment, and can continuously add the subsequent filter-pressed solution into the manganese sulfate solution after distillation, thereby realizing the cyclic utilization of absolute ethyl alcohol. Short process flow, high production efficiency and high production and application values.
The concentration of the manganese sulfate solution in the S1 is more than 150 g/L.
The volume ratio of the addition of the absolute ethyl alcohol to the addition of the manganese sulfate solution in the S2 is more than 1.0.
The reaction vessel is one of a beaker and a reaction kettle
A method for crystallizing a manganese sulfate solution based on an ethanol method specifically comprises the following steps:
s101, adding 200ml of manganese sulfate solution into a beaker, and stirring at normal temperature;
s102, slowly adding 240ml of absolute ethyl alcohol;
s103, after fully and uniformly stirring, performing filter pressing and drying;
s104, sampling and detecting to obtain the manganese sulfate crystallization rate of 75.84%.
And the normal-temperature stirring in the step S101 is carried out at the normal temperature of 25 ℃, and the normal-temperature stirring in the step S101 can also be carried out under the sealing condition.
Example two:
the embodiment of the invention provides a method for crystallizing a manganese sulfate solution based on an ethanol method, which comprises the following steps:
s101, adding 200ml of manganese sulfate solution into a beaker, and stirring at normal temperature;
s102, slowly adding 210ml of absolute ethyl alcohol;
s103, after fully and uniformly stirring, performing filter pressing and drying;
s104, sampling and detecting to obtain the manganese sulfate crystallization rate of 68.12%.
Example three:
the embodiment of the invention provides a method for crystallizing a manganese sulfate solution based on an ethanol method, which specifically comprises the following steps:
s101, adding 200ml of manganese sulfate solution into a beaker, and stirring at normal temperature;
s102, slowly adding 200ml of absolute ethyl alcohol;
s103, after fully and uniformly stirring, performing filter pressing and drying;
s104, sampling and detecting to obtain the manganese sulfate crystallization rate of 68.75%.
Example four:
the embodiment of the invention provides a crystallization method of a manganese sulfate solution, which specifically comprises the following steps:
s101, adding 200ml of manganese sulfate solution into a beaker, sealing and stirring at normal temperature;
s102, slowly adding 250ml of absolute ethyl alcohol;
s103, after fully and uniformly stirring, performing filter pressing and drying;
s104, sampling and detecting to obtain 80.03% of manganese sulfate crystallization rate.
Example five:
the embodiment of the invention provides a crystallization method of a manganese sulfate solution, which specifically comprises the following steps:
s101, adding 200ml of manganese sulfate solution into a beaker, sealing and stirring at normal temperature;
s102, slowly adding 350ml of absolute ethyl alcohol;
s103, after fully and uniformly stirring, performing filter pressing and drying;
s104, sampling and detecting to obtain 88.49% of manganese sulfate crystallization rate.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A method for crystallizing a manganese sulfate solution based on an ethanol method is characterized by comprising the following steps: comprises an ethanol method:
the method for crystallizing the manganese sulfate solution by the ethanol method comprises the following steps:
s1, putting a certain amount of manganese sulfate solution into a reaction container, and fully stirring at normal temperature;
s2, slowly adding absolute ethyl alcohol into the reaction container, and stopping adding the absolute ethyl alcohol when the supernatant is colorless and transparent;
and S3, after being fully and uniformly mixed in the reaction container, carrying out filter pressing on the mixture by using a filter press to obtain manganese sulfate crystals.
2. The method for crystallizing a manganese sulfate solution based on the ethanol method as claimed in claim 1, wherein: the concentration of the manganese sulfate solution in the S1 is more than 150 g/L.
3. The method for crystallizing a manganese sulfate solution based on the ethanol method as claimed in claim 1, wherein: the volume ratio of the addition of the absolute ethyl alcohol to the addition of the manganese sulfate solution in the S2 is more than 1.0.
4. The method for crystallizing a manganese sulfate solution based on the inositol method as set forth in claim 1, wherein: the reaction vessel is one of a beaker and a reaction kettle.
5. A method for crystallisation of manganese sulphate solution based on the ethanol process according to any of claims 1-3, characterised in that: the method specifically comprises the following steps:
s101, adding 200ml of manganese sulfate solution into a beaker, and stirring at normal temperature;
s102, slowly adding 200 and 350ml of absolute ethyl alcohol;
s103, after fully and uniformly stirring, performing filter pressing and drying;
s104, sampling and detecting. The crystallization rate of the manganese sulfate is measured to be 68.75-88.49%.
6. The method for crystallizing a manganese sulfate solution based on the ethanol method as claimed in claim 4, wherein: and the normal-temperature stirring in the step S101 is carried out at the normal temperature of 20-28 ℃, and the normal-temperature stirring in the step S101 can also be carried out under the sealing condition.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210095066.8A CN114405053A (en) | 2022-01-26 | 2022-01-26 | Method for crystallizing manganese sulfate solution based on ethanol method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210095066.8A CN114405053A (en) | 2022-01-26 | 2022-01-26 | Method for crystallizing manganese sulfate solution based on ethanol method |
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| CN114405053A true CN114405053A (en) | 2022-04-29 |
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| CN202210095066.8A Pending CN114405053A (en) | 2022-01-26 | 2022-01-26 | Method for crystallizing manganese sulfate solution based on ethanol method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115571920A (en) * | 2022-10-18 | 2023-01-06 | 南京南环水务科技有限公司 | Method for obtaining manganese sulfate crystals from solution containing manganese sulfate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939090A (en) * | 2021-05-14 | 2021-06-11 | 蜂巢能源科技有限公司 | Manganese sulfate purification and crystallization method |
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2022
- 2022-01-26 CN CN202210095066.8A patent/CN114405053A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939090A (en) * | 2021-05-14 | 2021-06-11 | 蜂巢能源科技有限公司 | Manganese sulfate purification and crystallization method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115571920A (en) * | 2022-10-18 | 2023-01-06 | 南京南环水务科技有限公司 | Method for obtaining manganese sulfate crystals from solution containing manganese sulfate |
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Application publication date: 20220429 |