CN106629857A - Separation method for impurity magnesium in manganese sulfate solution - Google Patents
Separation method for impurity magnesium in manganese sulfate solution Download PDFInfo
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- CN106629857A CN106629857A CN201710003818.2A CN201710003818A CN106629857A CN 106629857 A CN106629857 A CN 106629857A CN 201710003818 A CN201710003818 A CN 201710003818A CN 106629857 A CN106629857 A CN 106629857A
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- manganese sulfate
- separation method
- sulfate solution
- magnesium
- sulfuric acid
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- 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
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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
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a separation method for impurity magnesium in a manganese sulfate solution. The method comprises the following steps: adding sulfuric acid into the manganese sulfate solution to be processed, carrying out a reaction under stirring until no longer producing precipitates and performing solid-fluid separation. The separation method is high in operability and simple in technological process; the separation efficiency of magnesium reaches 60-92%, and the recycling rate of manganese sulfate reaches 60-85%; furthermore, the separation method helps to reduce the cost of a subsequent impurity-removing process of a cell-grade high-purity manganese sulfate solution.
Description
Technical field
The present invention relates to fine inorganic chemicals technical field, in particular it relates to impurity in a kind of manganese sulfate solution
The separation method of magnesium.
Background technology
With the extension and the development of power vehicle of field of lithium battery application, anode material of lithium battery industry is becoming most
The industry of tool development potentiality and investment value.But due to the scarcity of high-grade manganese resource in recent years, low-grade manganese is opened
Send out using of great interest and attention.The impurity content such as calcium, magnesium is higher in manganese sulfate solution prepared by low-grade manganese,
The requirement for preparing high-purity sulphuric acid manganese solution necessary to the high-purity manganese based raw material of LITHIUM BATTERY is not reached completely.Calcium in manganese sulfate solution
Removal technology is quite ripe, and manganese magnesium separates the big technical barrier being always in manganese sulfate production.Industrially, it is general to adopt
The method that all kinds of fluorides generate fluorination magnesium precipitate is added to remove the magnesium in manganese sulfate solution, but this method needs strict control
The addition of fluoride processed, it is exceeded to easily cause fluorine ion, and consumes a large amount of high-purity cleaners.Therefore, in the urgent need to proposing one
The detached new method of the simple manganese magnesium of efficient, workable, technological process is planted, to realize effective removal of magnesium.
The content of the invention
The goal of the invention of the present invention is the defect for prior art, there is provided impurity magnesium divides in a kind of manganese sulfate solution
From method.The targeted pending manganese sulfate solution of the method for the present invention is primarily referred to as the low-grade manganese of rich magnesium, and (manganese content is
10wt%-19wt%) the manganese sulfate solution of the high magnesium for preparing.
The separation method of impurity magnesium in the manganese sulfate solution that the present invention is provided, adds including in pending manganese sulfate solution
The step of sulfuric acid.
Aforesaid separation method, comprises the steps：
Sulfuric acid is added in pending manganese sulfate solution, stirring reaction is until no longer produce precipitation；
Separation of solid and liquid, reclaims solid, you can obtain the manganese sulfate solid of low magnesium and the manganese sulfate mother liquor of high magnesium.
Aforesaid separation method, the concentration of manganese sulfate is 300-700g/L in the pending manganese sulfate solution.
Aforesaid separation method, the concentration of magnesium is 300-6000mg/L in the pending manganese sulfate solution.
Aforesaid separation method, the sulfuric acid is the concentrated sulfuric acid, preferably the technical grade concentrated sulfuric acid, and more preferably concentration is
The technical grade concentrated sulfuric acid of 98wt%.
Aforesaid separation method, the pending manganese sulfate solution and the volume ratio of the sulfuric acid are 4:0.8-1.5.
Aforesaid separation method, the stirring reaction is reacted 0.5 hour to 16 hours under 25-95 DEG C, normal pressure.
Aforesaid separation method, the separative efficiency of impurity magnesium is 60wt%-92wt%.
Aforesaid separation method, the rate of recovery of manganese sulfate is 60wt%-85wt%.
Had the advantages that using above-mentioned technical proposal：At manganese sulfate solution of the present invention to high magnesium
Reason, can efficiently separate magnesium sulfate and manganese sulfate, and the separative efficiency of magnesium reaches 60%-92%, and the rate of recovery of manganese sulfate is 60%-
85%, it is further battery level high-purity sulphuric acid manganese solution removal of impurities reduces cost.And workable, technological process of the invention is simply,
Low production cost, it is easy to accomplish industrial-scale production, will not cause secondary pollution to further battery level high-purity sulphuric acid manganese product,
The deficiency of the method presence of existing separation manganese sulfate and magnesium sulfate is overcome completely.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to described reality
Among applying a scope.The experimental technique of unreceipted actual conditions in the following example, conventionally and condition, or according to business
Product specification is selected.
Following manganese sulfate solutions are prepared using the rich magnesium low-grade sulfuric acid manganese ore that manganese content is 10wt%-19wt%, Gao Mei
The rate of recovery of the content of each material and manganese sulfate, the separative efficiency of magnesium are obtained using this area conventional method in manganese sulfate solution
Arrive.
Embodiment 1：
325mL concentration is added to into 1300mL containing MnSO for the 98.0wt% concentrated sulfuric acids4385.11g/L, Mg 391mg/L's
In manganese sulfate solution, stirring is incubated 0.5h after being heated to 90 DEG C, suction filtration draws after separation of solid and liquid：The volume of mother liquor is
1045mL, containing MnSO4158.11g/L, Mg 438mg/L, the rate of recovery of manganese sulfate is 67%, and the separative efficiency of magnesium is
90.05%.
Embodiment 2：
250mL concentration is added to into 1000mL containing MnSO for the 98.0wt% concentrated sulfuric acids4494.21g/L, Mg1062mg/L's
In manganese sulfate solution, stirring is incubated 0.5h after being heated to 90 DEG C, suction filtration draws after separation of solid and liquid：The volume of mother liquor is
1060mL, containing MnSO4151.73g/L, Mg 909.8mg/L, the rate of recovery of manganese sulfate is 67.46%, and the separative efficiency of magnesium is
90.81%.
Embodiment 3：
650mL concentration is added to into 2600mL containing MnSO for the 98.0wt% concentrated sulfuric acids4484.2g/L, Mg701.4mg/L's
In manganese sulfate solution, after stirring at normal temperature 16h, suction filtration draws after separation of solid and liquid：The volume of mother liquor is 2630mL, is contained
MnSO4115.95g/L, Mg 624.1mg/L, the rate of recovery of manganese sulfate is 75.78%, and the separative efficiency of magnesium is 90.01%.
Embodiment 4：
250mL concentration is added to into 1000mL containing MnSO for the 98.0wt% concentrated sulfuric acids4580.37g/L, Mg5518mg/L's
In manganese sulfate solution, stirring is incubated 1.5h after being heated to 95 DEG C, suction filtration draws after separation of solid and liquid：The volume of mother liquor is
1030mL, containing MnSO4168.35g/L, Mg 4173mg/L, the rate of recovery of manganese sulfate is 70.12%, and the separative efficiency of magnesium is
77.89%.
Embodiment 5：
250mL concentration is added to into 1000mL containing MnSO for the 98.0wt% concentrated sulfuric acids4580.37g/L, Mg5518mg/L's
In manganese sulfate solution, stirring is incubated 6h after being heated to 95 DEG C, suction filtration draws after separation of solid and liquid：The volume of mother liquor is 980mL, is contained
MnSO4132.91g/L, Mg 4155mg/L, the rate of recovery of manganese sulfate is 77.59%, and the separative efficiency of magnesium is 73.79%.
Embodiment 6：
375mL concentration is added to into 1000mL containing MnSO for the 98.0wt% concentrated sulfuric acids4449.37g/L, Mg3121mg/L's
In manganese sulfate solution, stirring is incubated 0.7h after being heated to 90 DEG C, suction filtration draws after separation of solid and liquid：The volume of mother liquor is
1080mL, containing MnSO465.36g/L, Mg 1871mg/L, the rate of recovery of manganese sulfate is 84.29%, and the separative efficiency of magnesium is
64.74%.
Embodiment 7：
200mL concentration is added to into 1000mL containing MnSO for the 98.0wt% concentrated sulfuric acids4526.53g/L, Mg2881mg/L's
In manganese sulfate solution, stirring is incubated 0.5h after being heated to 90 DEG C, suction filtration draws after separation of solid and liquid：The volume of mother liquor is
1040mL, containing MnSO4178.38g/L, Mg 2552mg/L, the rate of recovery of manganese sulfate is 64.77%, and the separative efficiency of magnesium is
92.12%.
Claims (9)
1. in a kind of manganese sulfate solution impurity magnesium separation method, it is characterised in that include in pending manganese sulfate solution plus
The step of entering sulfuric acid.
2. separation method according to claim 1, it is characterised in that comprise the steps：
Sulfuric acid is added in pending manganese sulfate solution, stirring reaction is until no longer produce precipitation；
Separation of solid and liquid, reclaims solid.
3. separation method according to claim 1 and 2, it is characterised in that manganese sulfate in the pending manganese sulfate solution
Concentration be 300-700g/L.
4. the separation method according to any one of claim 1-3, it is characterised in that magnesium in the pending manganese sulfate solution
Concentration be 300-6000mg/L.
5. the separation method according to any one of claim 1-4, it is characterised in that the sulfuric acid is the concentrated sulfuric acid, preferably
The technical grade concentrated sulfuric acid, more preferably concentration are the technical grade concentrated sulfuric acid of 98wt%.
6. the separation method according to any one of claim 1-5, it is characterised in that the pending manganese sulfate solution and institute
The volume ratio for stating sulfuric acid is 4:0.8-1.5.
7. the separation method according to any one of claim 2-6, it is characterised in that the stirring reaction be 25-95 DEG C,
React 0.5 hour to 16 hours under normal pressure.
8. the separation method according to any one of claim 1-7, it is characterised in that the separative efficiency of impurity magnesium is
60wt%-92wt%.
9. the separation method according to any one of claim 1-8, it is characterised in that the rate of recovery of manganese sulfate is 60wt%-
85wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710003818.2A CN106629857A (en) | 2017-01-04 | 2017-01-04 | Separation method for impurity magnesium in manganese sulfate solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710003818.2A CN106629857A (en) | 2017-01-04 | 2017-01-04 | Separation method for impurity magnesium in manganese sulfate solution |
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| CN106629857A true CN106629857A (en) | 2017-05-10 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107963669A (en) * | 2018-01-08 | 2018-04-27 | 中南大学 | A kind of calcium removal methods of technical grade sulfuric acid manganese |
| CN111170367A (en) * | 2020-02-20 | 2020-05-19 | 中国恩菲工程技术有限公司 | Method for purifying manganese sulfate in magnesium-rich manganese sulfate solution |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508467A (en) * | 2008-11-18 | 2009-08-19 | 湖北开元化工科技股份有限公司 | Preparation of high purity manganese sulfate |
| CN101875507A (en) * | 2010-08-04 | 2010-11-03 | 湖南汇通科技有限责任公司 | High purity manganese sulfate monohydrate and preparation method thereof |
| CN104947154A (en) * | 2015-07-08 | 2015-09-30 | 长沙矿冶研究院有限责任公司 | Method for demagging anolyte of electrolytic manganese |
-
2017
- 2017-01-04 CN CN201710003818.2A patent/CN106629857A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508467A (en) * | 2008-11-18 | 2009-08-19 | 湖北开元化工科技股份有限公司 | Preparation of high purity manganese sulfate |
| CN101875507A (en) * | 2010-08-04 | 2010-11-03 | 湖南汇通科技有限责任公司 | High purity manganese sulfate monohydrate and preparation method thereof |
| CN104947154A (en) * | 2015-07-08 | 2015-09-30 | 长沙矿冶研究院有限责任公司 | Method for demagging anolyte of electrolytic manganese |
Non-Patent Citations (2)
| Title |
|---|
| M.E.波任 等: "《无机盐工艺学 上册》", 30 September 1982 * |
| 伍福智 等: "酸解法制备硫酸锰的研究", 《无机盐工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107963669A (en) * | 2018-01-08 | 2018-04-27 | 中南大学 | A kind of calcium removal methods of technical grade sulfuric acid manganese |
| CN111170367A (en) * | 2020-02-20 | 2020-05-19 | 中国恩菲工程技术有限公司 | Method for purifying manganese sulfate in magnesium-rich manganese sulfate solution |
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Application publication date: 20170510 |