CN106186006A - A kind of purifying lithium chloride method - Google Patents
A kind of purifying lithium chloride method Download PDFInfo
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- CN106186006A CN106186006A CN201610597647.6A CN201610597647A CN106186006A CN 106186006 A CN106186006 A CN 106186006A CN 201610597647 A CN201610597647 A CN 201610597647A CN 106186006 A CN106186006 A CN 106186006A
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- lithium chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/04—Halides
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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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- 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
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a kind of purifying lithium chloride method, comprise the following steps: a) dissolve: in dissolution kettle, add lithium chloride crude product, and inject a certain amount of water, after heated and stirred, carry out solid-liquid separation operation, obtain lithium chloride wet product A, collect the mother solution of isolated simultaneously；B) crystallization: mother solution is poured in evaporative crystallization still, circulation and evacuation in opening, the most slowly heat up, steamed by the water in mother solution, cool down afterwards, obtain magma；C) dry: magma is carried out solid-liquid separation operation, obtains lithium chloride wet product B, be dried after the lithium chloride wet product obtained is mixed, pack after being dried in two steps.Present invention process is simple, without any medicament, does not produce product and pollutes, and purifying lithium chloride technology yield is high, and energy consumption is low.
Description
Technical field
The present invention relates to lithium compound purification technique field, especially relate to a kind of purifying lithium chloride method.
Background technology
Highly purified lithium metal and lithium compound (purity is not less than 99.9%) have been widely used in various field, as
Lithium battery, containing lithium constructional alloy, nuclear energy high-tech, the aluminum lithium constructional alloy etc. of application in Aeronautics and Astronautics；The most nearest tens
Year, along with developing rapidly of lithium ion battery industry, the demand of high-purity lithium compound is significantly increased；Highly purified lithium metal and
It is that raw material prepares that lithium compound is presently mainly with highly purified lithium chloride (purity is not less than 99.9%)；Therefore, height is obtained
The lithium chloride of purity is it is critical that a ring.Existing lithium compound uses in environment, to impurity natrium ion in lithium compound
Existence require harsher, general requirement≤15ppm, so in some sense, remove impurity natrium ion, become this
One of key of control of product quality, and the biggest to the elimination difficulty of impurity natrium ion.
At present, purifying lithium chloride method having carried out substantial amounts of work, the method for purification of conventional chemical chemical industry, as coprecipitated
The processes such as shallow lake, fractional crystallization, solvent extraction, ion exchange, the purification to lithium chloride, or not reaching the degree of depth removes impurity
Sodium ion, though or technically feasible, but cost is high.Such as Chinese periodical " rare metal ", vol23.No2.P95～99, public affairs
Open the document of entitled " from the flow process research of Saturated with Magnesium chloride bittern extraction lithium ", wherein with Qinghai Salt Lake Bittern resource, first
After in salt, sodium, potassium, boron are separated into corresponding product, remaining mother solution contains magnesium, lithium valuable constituent, uses containing lithium aqueous solution ground
Organic solvent extractionprocess, to separate the impurity such as substantial amounts of magnesium and the sodium of residual, potassium, boron, ferrum in solution；Result shows, this technique
Can only obtain qualified industrial chlorinations lithium product, purity does not reaches pure lithium chloride standard, only with regard to impurity natrium content >=1700ppm.
Summary of the invention
For solving the problems referred to above, the invention provides one and have lithium chloride yield height, purity is more than 99.9%, impurity natrium
The effective Radix Raphani of ion remaval, purifying lithium chloride method.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of purifying lithium chloride method, comprises the following steps:
A) dissolve: in dissolution kettle, add lithium chloride crude product, and inject a certain amount of water, make the mass ratio of lithium chloride crude product and water
Being 1.5～2.0:1.0, heating keeps the temperature at 25～35 DEG C, after stirring 2～3 hours, carries out solid-liquid separation operation, obtains
Lithium chloride wet product A, collects the mother solution of isolated simultaneously；
B) crystallization: the mother solution collected in step a is poured in evaporative crystallization still, circulation and evacuation in opening, the most slowly rise
Temperature, steams the water in mother solution, stops distillation when 50 that the moisture steamed is mother solution volume～80% and stops evacuation, and
It is cooled to less than 20 DEG C, after keeping 2～3 hours, obtains magma；
C) dry: magma step b obtained carries out solid-liquid separation operation, obtains lithium chloride wet product B, by lithium chloride wet product B and
It is dried after the lithium chloride wet product A mixing prepared by step a, packs after being dried.
Step a is selected water dissolution lithium chloride crude product, it is preferred to use purified water or deionized water dissolve, and so may be used
To reduce the pollution of foreign ion, it is ensured that in purification process, the content of sodium ion reaches minimum；At a temperature of this and under amount of water, chlorine
Change lithium solution the most saturated, and sodium ion (existing as sodium chloride in crude product) unsaturation far away, then in crude product lithium chloride
Sodium chloride can be dissolved completely in water, and lithium chloride solution has reached supersaturation simultaneously, so substantial amounts of lithium chloride is the most molten
Solving, can be obtained by centrifuge dehydration, yield improves, and decreases the energy consumption of evaporation water required behind.
Step b first carries out the water of continuous print evaporative crystallization, i.e. evaporation section, separates out partial oxidation crystalline lithium, due to water
It is not vaporized completely, so the sodium ion of trace will not be precipitated, simultaneously in order to make lithium chloride as much as possible separate out, needs
Transpiring moistures the most in the case of not separating out ensureing sodium chloride；Next decrease temperature crystalline is started, along with at temperature
Fall, lithium chloride crystal can constantly separate out, but owing to the sodium ion of trace exists as sodium chloride, its dissolubility is with temperature
Degree impact is less, so sodium chloride crystal separates out hardly.
As preferably, the solid-liquid separation operation in step a and step c is precipitate and separate, centrifugation or filters separation
Operation.
As preferably, the solid-liquid separation operation in step a and step c operates for centrifugation.
Although precipitate and separate and filtration separate the effect that also can play solid-liquid separation, but due to precipitate and separate and filtration point
In wet product lithium chloride after both PROCESS FOR TREATMENT, water content is higher, can increase the operating pressure of follow-up baking operation, and from
The heart separates moisture content less in the wet product lithium chloride obtained, it is possible to reduce the pressure of baking operation.
As preferably, after lithium chloride crude product and water add dissolution kettle in step a, account for the 75～85% of dissolution kettle volume.
As preferably, in step b, after mother solution pours evaporative crystallization still into, in first opening, circulate evacuation again.
As preferably, in step b, aqueous cooling solution is used to cool down.
As preferably, in step b, using chilled brine to cool down, chilled brine concentration is 15～25wt%, freezing salt
Temperature≤-10 DEG C of water.
As preferably, in step c, the solution obtained after collecting solid-liquid separation, and upper once purify time add as raw material
Enter.
The solution that in step c, magma obtains after solid-liquid separation is also dissolved with the lithium chloride of certain content, receives for improving
Rate, using this part solution upper once purify time as raw material add, reduce waste, improve yield.
As preferably, in step c, lithium chloride wet product is dried, moisture≤0.1wt% contained therein.
Therefore, the method have the advantages that
(1) present invention process is simple, without any medicament, does not produce product and pollutes；
(2) the purifying lithium chloride technology yield in the present invention is high, and energy consumption is low.
Detailed description of the invention
Below in conjunction with detailed description of the invention, technical scheme is further described.
Embodiment 1
A kind of purifying lithium chloride method, comprises the following steps:
A) dissolve: in dissolution kettle, add lithium chloride crude product, and inject a certain amount of water, make the mass ratio of lithium chloride crude product and water
After adding dissolution kettle for 1.5:1.0, lithium chloride crude product and water, accounting for the 75% of dissolution kettle volume, heating keeps the temperature at 25 DEG C,
After stirring 2 hours, carry out solid-liquid separation operation, obtain lithium chloride wet product A, collect the mother solution of isolated simultaneously；
B) crystallization: pour in evaporative crystallization still by the mother solution collected in step a, circulates evacuation again in first opening, the most slowly
Heat up, the water in mother solution is steamed, stop distillation when 50% that the moisture steamed is mother solution volume and stop evacuation, and adopting
Carry out being cooled to 20 DEG C with aqueous cooling solution, after keeping 2 hours, obtain magma；
C) dry: magma step b obtained carries out solid-liquid separation operation, obtains lithium chloride wet product B, by lithium chloride wet product B and
Being dried after the lithium chloride wet product A mixing prepared by step a, lithium chloride wet product is dried, and moisture need contained therein≤
0.1wt%, then packs；After solid-liquid separation, collect the solution obtained after solid-liquid separation, and upper once purify time conduct
Raw material adds.
Embodiment 2
A kind of purifying lithium chloride method, comprises the following steps:
A) dissolve: in dissolution kettle, add lithium chloride crude product, and inject a certain amount of water, make the mass ratio of lithium chloride crude product and water
After adding dissolution kettle for 1.7:1.0, lithium chloride crude product and water, accounting for the 80% of dissolution kettle volume, heating keeps the temperature at 30 DEG C,
After stirring 2.5 hours, carry out solid-liquid separation operation, obtain lithium chloride wet product A, collect the mother solution of isolated simultaneously；
B) crystallization: pour in evaporative crystallization still by the mother solution collected in step a, circulates evacuation again in first opening, the most slowly
Heat up, the water in mother solution is steamed, stop distillation when 65% that the moisture steamed is mother solution volume and stop evacuation, and adopting
Carry out being cooled to 15 DEG C with aqueous cooling solution, after keeping 2.5 hours, obtain magma；
C) dry: magma step b obtained carries out solid-liquid separation operation, obtains lithium chloride wet product B, by lithium chloride wet product B and
Being dried after the lithium chloride wet product A mixing prepared by step a, lithium chloride wet product is dried, and moisture need contained therein≤
0.1wt%, then packs；After solid-liquid separation, collect the solution obtained after solid-liquid separation, and upper once purify time conduct
Raw material adds.
Embodiment 3
A kind of purifying lithium chloride method, comprises the following steps:
A) dissolve: in dissolution kettle, add lithium chloride crude product, and inject a certain amount of water, make the mass ratio of lithium chloride crude product and water
After adding dissolution kettle for 2.0:1.0, lithium chloride crude product and water, accounting for the 85% of dissolution kettle volume, heating keeps the temperature at 35 DEG C,
After stirring 3 hours, carry out solid-liquid separation operation, obtain lithium chloride wet product A, collect the mother solution of isolated simultaneously；
B) crystallization: pour in evaporative crystallization still by the mother solution collected in step a, circulates evacuation again in first opening, the most slowly
Heat up, the water in mother solution is steamed, stop distillation when 80% that the moisture steamed is mother solution volume and stop evacuation, and adopting
Carry out being cooled to 10 DEG C with aqueous cooling solution, after keeping 3 hours, obtain magma；
C) dry: magma step b obtained carries out solid-liquid separation operation, obtains lithium chloride wet product B, by lithium chloride wet product B and
Being dried after the lithium chloride wet product A mixing prepared by step a, lithium chloride wet product is dried, and moisture need contained therein≤
0.1wt%, then packs；After solid-liquid separation, collect the solution obtained after solid-liquid separation, and upper once purify time conduct
Raw material adds.
Embodiment 4
A kind of purifying lithium chloride method, comprises the following steps:
A) dissolve: in dissolution kettle, add lithium chloride crude product, and inject a certain amount of water, make the mass ratio of lithium chloride crude product and water
After adding dissolution kettle for 1.5:1.0, lithium chloride crude product and water, accounting for the 75% of dissolution kettle volume, heating keeps the temperature at 25 DEG C,
After stirring 2 hours, carry out precipitate and separate operation, obtain lithium chloride wet product A, collect the mother solution of isolated simultaneously；
B) crystallization: pour in evaporative crystallization still by the mother solution collected in step a, circulates evacuation again in first opening, the most slowly
Heat up, the water in mother solution is steamed, stop distillation when 50% that the moisture steamed is mother solution volume and stop evacuation, and adopting
Carry out being cooled to 20 DEG C with chilled brine, after keeping 2 hours, obtain magma；Wherein, chilled brine concentration is 15wt%, freezing salt
The temperature of water is-10 DEG C；
C) dry: magma step b obtained carries out precipitate and separate operation, obtains lithium chloride wet product B, by lithium chloride wet product B and
Being dried after the lithium chloride wet product A mixing prepared by step a, lithium chloride wet product is dried, and moisture need contained therein≤
0.1wt%, then packs；After precipitate and separate operation, collect the solution that obtains after separating, and upper once purify time conduct
Raw material adds.
Embodiment 5
A kind of purifying lithium chloride method, comprises the following steps:
A) dissolve: in dissolution kettle, add lithium chloride crude product, and inject a certain amount of water, make the mass ratio of lithium chloride crude product and water
After adding dissolution kettle for 1.7:1.0, lithium chloride crude product and water, accounting for the 80% of dissolution kettle volume, heating keeps the temperature at 30 DEG C,
After stirring 2.5 hours, it is centrifuged lock out operation, obtains lithium chloride wet product A, collect the mother solution of isolated simultaneously；
B) crystallization: pour in evaporative crystallization still by the mother solution collected in step a, circulates evacuation again in first opening, the most slowly
Heat up, the water in mother solution is steamed, stop distillation when 65% that the moisture steamed is mother solution volume and stop evacuation, and adopting
Carry out being cooled to 15 DEG C with chilled brine, after keeping 2.5 hours, obtain magma；Wherein, chilled brine concentration is 20wt%, freezing
The temperature of saline is-12 DEG C；
C) dry: magma step b obtained is centrifuged lock out operation operation, obtains lithium chloride wet product B, by lithium chloride wet product
B and lithium chloride wet product A prepared by step a are dried after mixing, and lithium chloride wet product is dried, and moisture need contained therein≤
0.1wt%, then packs；After centrifugation operation, collect the solution that obtains after separating, and upper once purify time conduct
Raw material adds.
Embodiment 6
A kind of purifying lithium chloride method, comprises the following steps:
A) dissolve: in dissolution kettle, add lithium chloride crude product, and inject a certain amount of water, make the mass ratio of lithium chloride crude product and water
After adding dissolution kettle for 2.0:1.0, lithium chloride crude product and water, accounting for the 85% of dissolution kettle volume, heating keeps the temperature at 35 DEG C,
After stirring 3 hours, carry out filtering lock out operation, obtain lithium chloride wet product A, collect the mother solution of isolated simultaneously；
B) crystallization: pour in evaporative crystallization still by the mother solution collected in step a, circulates evacuation again in first opening, the most slowly
Heat up, the water in mother solution is steamed, stop distillation when 80% that the moisture steamed is mother solution volume and stop evacuation, and adopting
Carry out being cooled to 10 DEG C with chilled brine, after keeping 3 hours, obtain magma；Wherein, chilled brine concentration is 25wt%, freezing salt
The temperature of water is-15 DEG C；
C) dry: magma step b obtained carries out filtering lock out operation, obtains lithium chloride wet product B, by lithium chloride wet product B and
Being dried after the lithium chloride wet product A mixing prepared by step a, lithium chloride wet product is dried, and moisture need contained therein≤
0.1wt%, then packs；Filter after lock out operation, collect the solution obtained after separating, and upper once purify time conduct
Raw material adds.
The technical grade lithium chloride that purity is 97wt% of the raw material lithium chloride crude product employed in above-described embodiment, is passing through
Above-mentioned steps purifies the purity of afterchlorinate lithium and is both greater than 99.9wt%, and sodium ions content is all not more than 15ppm, even purity and is more than
99.95wt%, sodium ions content is less than 10ppm.
Claims (9)
1. a purifying lithium chloride method, it is characterised in that comprise the following steps:
A) dissolve: in dissolution kettle, add lithium chloride crude product, and inject a certain amount of water, make the mass ratio of lithium chloride crude product and water
Being 1.5～2.0:1.0, heating keeps the temperature at 25～35 DEG C, after stirring 2～3 hours, carries out solid-liquid separation operation, obtains
Lithium chloride wet product A, collects the mother solution of isolated simultaneously；
B) crystallization: the mother solution collected in step a is poured in evaporative crystallization still, circulation and evacuation in opening, the most slowly rise
Temperature, steams the water in mother solution, stops distillation when 50 that the moisture steamed is mother solution volume～80% and stops evacuation, and
It is cooled to less than 20 DEG C, after keeping 2～3 hours, obtains magma；
C) dry: magma step b obtained carries out solid-liquid separation operation, obtains lithium chloride wet product B, by lithium chloride wet product B and
It is dried after the lithium chloride wet product A mixing prepared by step a, packs after being dried.
A kind of purifying lithium chloride method the most according to claim 1, it is characterised in that: consolidating in described step a and step c
Liquid lock out operation is precipitate and separate, centrifugation or filters lock out operation.
A kind of purifying lithium chloride method the most according to claim 1, it is characterised in that: consolidating in described step a and step c
Liquid lock out operation is centrifugation operation.
A kind of purifying lithium chloride method the most according to claim 1, it is characterised in that: lithium chloride crude product in described step a
After adding dissolution kettle with water, account for the 75～85% of dissolution kettle volume.
A kind of purifying lithium chloride method the most according to claim 1, it is characterised in that: in described step b, mother solution pours steaming into
After sending out crystallization kettle, in first opening, circulate evacuation again.
A kind of purifying lithium chloride method the most according to claim 1, it is characterised in that: in described step b, use cooling water
Solution cools down.
7. according to a kind of purifying lithium chloride method described in claim 1 or 6, it is characterised in that: in described step b, use cold
Freezing saline to cool down, chilled brine concentration is 15～25wt%, temperature≤-10 DEG C of chilled brine.
A kind of purifying lithium chloride method the most according to claim 1, it is characterised in that: in described step c, collect solid-liquid and divide
The solution obtained after from, and upper once purify time as raw material add.
A kind of purifying lithium chloride method the most according to claim 1, it is characterised in that: in described step c, lithium chloride wet product
After drying, moisture≤0.1wt% contained therein.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109662991A (en) * | 2019-02-20 | 2019-04-23 | 郑州大学第附属医院 | A kind of drug and preparation method of the treatment diabetic nephropathy based on lithium chloride |
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| CN109662991A (en) * | 2019-02-20 | 2019-04-23 | 郑州大学第附属医院 | A kind of drug and preparation method of the treatment diabetic nephropathy based on lithium chloride |
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Inventor after: Weng Min Inventor after: Bao Zhiquan Inventor before: Bao Zhiquan |
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| CB03 | Change of inventor or designer information | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A purification method of lithium chloride Effective date of registration: 20221024 Granted publication date: 20170825 Pledgee: Zhejiang Suichang Rural Commercial Bank Co.,Ltd. Pledgor: ZHEJIANG HONGHAO TECHNOLOGY CO.,LTD. Registration number: Y2022330002781 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |