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CN107902679A - A kind of industrial method for producing battery-level lithium carbonate - Google Patents

A kind of industrial method for producing battery-level lithium carbonate Download PDF

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Publication number
CN107902679A
CN107902679A CN201711119014.5A CN201711119014A CN107902679A CN 107902679 A CN107902679 A CN 107902679A CN 201711119014 A CN201711119014 A CN 201711119014A CN 107902679 A CN107902679 A CN 107902679A
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CN
China
Prior art keywords
lithium
solution
carbonate
sulfate
lithium carbonate
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201711119014.5A
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Chinese (zh)
Inventor
谭运全
谭子峻
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Dayu County Rising Mining Technology Co Ltd
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Dayu County Rising Mining Technology Co Ltd
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Publication date
Application filed by Dayu County Rising Mining Technology Co Ltd filed Critical Dayu County Rising Mining Technology Co Ltd
Priority to CN201711119014.5A priority Critical patent/CN107902679A/en
Publication of CN107902679A publication Critical patent/CN107902679A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00Lithium compounds
    • C01D15/08Carbonates; Bicarbonates

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of industrial method for producing battery-level lithium carbonate, include the following steps:(1):Lepidolite ore is crushed, obtains lepidolite powder, pours into rotary furnace and is sintered after then lepidolite powder is mixed with technical pure lithium sulfate, the lepidolite after sintering obtains crude product solution with appropriate purifying water extraction;(2):Sodium hydroxide solution and solution of potassium carbonate are added into the crude product solution obtained by step (1), then filter, evaporate, being centrifugally separating to obtain lithium sulfate solution and potassium sulfate sodium sulfate crystal, the potassium sulfate sodium sulfate crystal returns to step (1);(3):Lithium sulfate solution and saturated sodium carbonate solution are slowly added into reactor, carbonic acid crystalline lithium is then obtained by filtration;(4):Carbonic acid crystalline lithium obtained by step (3) is washed by hot water, is then dried to obtain battery-level lithium carbonate.Preparation method of the present invention is simple, and lithium carbonate purity is high;Production cost is low;Present invention process mild condition, operating process is stablized, with short production cycle, and utilization rate of equipment and installations is high.

Description

A kind of industrial method for producing battery-level lithium carbonate
Technical field
The present invention relates to a kind of industrial method for producing battery-level lithium carbonate.
Background technology
Lithium, it is known that most light, the silvery white alkali metal of nuclear radius minimum, because lithium and its compound have it is many distinctive excellent Benign energy, they are widely used in the fields such as glass, ceramics, lubrication, electronics, metallurgy, medicine, refrigeration, aerospace.With clear Clean energy demand it is surging, the lithium energy will likely deep effect human lives, its also referred to as " energy upstart of 21 century ".
Lithium carbonate is a kind of important industrial chemicals, and with national new energy development plan, lithium electricity new energy is as country Emphasis supports one of development energy industry;And lithium carbonate develops important foundation raw material as lithium electricity new energy, it is produced and demand Measure increasing, price is also higher and higher.
Mainly liquid ore deposit, liquid ore deposit are mainly using salt lake bittern as original to the preparation method of lithium carbonate from the point of view of raw material at present Material extracted, this method is easy to extract since cost of material is low, but due in bittern magnesium ion content it is higher, its give birth to The industrial level lithium carbonate of production is easier to, but if its production cost of the lithium carbonate of production LITHIUM BATTERY is also higher.
Yichuan tantalum niobium lithium ore deposit is the tantalum niobium lithium ore deposit of current Fia, and tantalum niobium lithium resource enriches, dioxy in lepidolite Change lithium content up to 4.5%, there is extraction lithium carbonate resources advantage condition, and have in lepidolite containing potassium, rubidium, caesium, aluminium etc. are a variety of The metallic element of value, comprehensively utilizes these resources, can greatly improve the utility value that lithium carbonate is extracted from lepidolite, from And lithium carbonate production cost is greatly reduced.Therefore carrying out extraction lithium carbonate as raw material using lepidolite has broader market prospects And preferable economic benefit.
The method of traditional liquid ore deposit production battery-level lithium carbonate has technological process complicated, and of high cost, yield is low, high energy consumption The features such as, improve the production method of battery-level lithium carbonate also become whole industry there is an urgent need for.
The content of the invention
The purpose of the present invention is overcome the shortcomings of in existing product, there is provided a kind of industrialization side for producing battery-level lithium carbonate Method.
In order to achieve the above object, the present invention is achieved by the following technical solutions:
A kind of industrial method for producing battery-level lithium carbonate, includes the following steps:
(1):Lepidolite ore is crushed, obtains lepidolite powder, then mixes lepidolite powder with technical pure lithium sulfate After pour into rotary furnace be 920-1100 DEG C in temperature at be sintered a period of time, the appropriate purified water of the lepidolite after sintering Crude product solution is leached to obtain, described a period of time is 7-10 hour;
(2):Sodium hydroxide solution and solution of potassium carbonate are added into the crude product solution obtained by step (1), then filters, steam Send out, be centrifugally separating to obtain lithium sulfate solution and potassium sulfate sodium sulfate crystal, the potassium sulfate sodium sulfate crystal returns to step (1);
(3):Lithium sulfate solution and saturated sodium carbonate solution are slowly added into reactor, lithium carbonate is then obtained by filtration Crystal;
(4):Carbonic acid crystalline lithium obtained by step (3) is washed by hot water, is then dried to obtain LITHIUM BATTERY carbonic acid Lithium.
Preferably, the temperature is 920 DEG C.
Preferably, the temperature is 1100 DEG C.
Preferably, described a period of time is 7 hours.
Preferably, described a period of time is 10 hours.
Preferably, by saturated sodium carbonate solution when lithium sulfate solution is slowly added into reactor in the step (3) Atomized spray is to the surface of lithium sulfate solution.
Beneficial effects of the present invention are as follows:
1st, the present invention use lepidolite ore of low cost its technical process is simpler for raw material, production efficiency height;
2nd, method of the invention is easy to carry out quality control, and its cost of raw material is cheap, is very suitable for large-scale industry Production;
3rd, workflow of the present invention is simple, good product quality;
4th, present invention process mild condition, operating process is stablized, with short production cycle, and utilization rate of equipment and installations is high, and production cost is low, Lithium carbonate yield is high, and effect on environment is small, and energy consumption is low.
Embodiment
Technical scheme is described further below:
Embodiment 1:
A kind of industrial method for producing battery-level lithium carbonate, includes the following steps:
(1):Lepidolite ore is crushed, obtains lepidolite powder, then mixes lepidolite powder with technical pure lithium sulfate After pour into rotary furnace be 920-1100 DEG C in temperature at be sintered a period of time, the appropriate purified water of the lepidolite after sintering Crude product solution is leached to obtain, described a period of time is 7-10 hour;
(2):Sodium hydroxide solution and solution of potassium carbonate are added into the crude product solution obtained by step (1), then filters, steam Send out, be centrifugally separating to obtain lithium sulfate solution and potassium sulfate sodium sulfate crystal, the potassium sulfate sodium sulfate crystal returns to step (1);
(3):Lithium sulfate solution and saturated sodium carbonate solution are slowly added into reactor, lithium carbonate is then obtained by filtration Crystal;
(4):Carbonic acid crystalline lithium obtained by step (3) is washed by hot water, is then dried to obtain LITHIUM BATTERY carbonic acid Lithium.
Saturated sodium carbonate solution atomized spray is arrived when lithium sulfate solution is slowly added into reactor in the step (3) The surface of lithium sulfate solution.
1st, the present invention use lepidolite ore of low cost its technical process is simpler for raw material, production efficiency height;
2nd, method of the invention is easy to carry out quality control, and its cost of raw material is cheap, is very suitable for large-scale industry Production;
3rd, workflow of the present invention is simple, good product quality;
4th, present invention process mild condition, operating process is stablized, with short production cycle, and utilization rate of equipment and installations is high, and production cost is low, Lithium carbonate yield is high, and effect on environment is small, and energy consumption is low.
Embodiment 2:
A kind of industrial method for producing battery-level lithium carbonate, includes the following steps:
(1):Lepidolite ore is crushed, obtains lepidolite powder, then mixes lepidolite powder with technical pure lithium sulfate After pour into rotary furnace be 1100 DEG C in temperature at be sintered a period of time, the appropriate purifying water extraction of the lepidolite after sintering Crude product solution is obtained, described a period of time is 10 hours;
(2):Sodium hydroxide solution and solution of potassium carbonate are added into the crude product solution obtained by step (1), then filters, steam Send out, be centrifugally separating to obtain lithium sulfate solution and potassium sulfate sodium sulfate crystal, the potassium sulfate sodium sulfate crystal returns to step (1);
(3):Lithium sulfate solution and saturated sodium carbonate solution are slowly added into reactor, lithium carbonate is then obtained by filtration Crystal;
(4):Carbonic acid crystalline lithium obtained by step (3) is washed by hot water, is then dried to obtain LITHIUM BATTERY carbonic acid Lithium.
Saturated sodium carbonate solution atomized spray is arrived when lithium sulfate solution is slowly added into reactor in the step (3) The surface of lithium sulfate solution.
1st, the present invention use lepidolite ore of low cost its technical process is simpler for raw material, production efficiency height;
2nd, method of the invention is easy to carry out quality control, and its cost of raw material is cheap, is very suitable for large-scale industry Production;
3rd, workflow of the present invention is simple, good product quality;
4th, present invention process mild condition, operating process is stablized, with short production cycle, and utilization rate of equipment and installations is high, and production cost is low, Lithium carbonate yield is high, and effect on environment is small, and energy consumption is low.
Embodiment 3:
A kind of industrial method for producing battery-level lithium carbonate, includes the following steps:
(1):Lepidolite ore is crushed, obtains lepidolite powder, then mixes lepidolite powder with technical pure lithium sulfate After pour into rotary furnace be 920-1100 DEG C in temperature at be sintered a period of time, the appropriate purified water of the lepidolite after sintering Crude product solution is leached to obtain, described a period of time is 7-10 hour;
(2):Sodium hydroxide solution and solution of potassium carbonate are added into the crude product solution obtained by step (1), then filters, steam Send out, be centrifugally separating to obtain lithium sulfate solution and potassium sulfate sodium sulfate crystal, the potassium sulfate sodium sulfate crystal returns to step (1);
(3):Lithium sulfate solution and saturated sodium carbonate solution are slowly added into reactor, lithium carbonate is then obtained by filtration Crystal;
(4):Carbonic acid crystalline lithium obtained by step (3) is washed by hot water, is then dried to obtain LITHIUM BATTERY carbonic acid Lithium.
Saturated sodium carbonate solution atomized spray is arrived when lithium sulfate solution is slowly added into reactor in the step (3) The surface of lithium sulfate solution.
1st, the present invention use lepidolite ore of low cost its technical process is simpler for raw material, production efficiency height;
2nd, method of the invention is easy to carry out quality control, and its cost of raw material is cheap, is very suitable for large-scale industry Production;
3rd, workflow of the present invention is simple, makees process stabilization, with short production cycle, and utilization rate of equipment and installations is high, and production cost is low, carbon Sour lithium yield is high, and effect on environment is small.Energy consumption is low.
It should be noted that listed above is only a kind of specific embodiment of the invention.It is clear that the invention is not restricted to Upper embodiment, can also there is many deformations, in short, those of ordinary skill in the art can directly lead from present disclosure All deformations for going out or associating, are considered as protection scope of the present invention.

Claims (6)

1. a kind of industrial method for producing battery-level lithium carbonate, it is characterised in that include the following steps:
(1):Lepidolite ore is crushed, obtains lepidolite powder, is fallen after then lepidolite powder is mixed with technical pure lithium sulfate Enter and be sintered a period of time in rotary furnace in the case where temperature is 920-1100 DEG C, the appropriate purifying water extraction of the lepidolite after sintering Crude product solution is obtained, described a period of time is 7-10 hour;
(2):Sodium hydroxide solution and solution of potassium carbonate are added into the crude product solution obtained by step (1), then filter, evaporate, Lithium sulfate solution and potassium sulfate sodium sulfate crystal are centrifugally separating to obtain, the potassium sulfate sodium sulfate crystal returns to step (1);
(3):Lithium sulfate solution and saturated sodium carbonate solution are slowly added into reactor, lithium carbonate crystalline substance is then obtained by filtration Body;
(4):Carbonic acid crystalline lithium obtained by step (3) is washed by hot water, is then dried to obtain battery-level lithium carbonate.
2. the industrial method of the 1 production battery-level lithium carbonate is wanted according to right, it is characterised in that the temperature is 920 DEG C.
3. the industrial method of the 1 production battery-level lithium carbonate is wanted according to right, it is characterised in that the temperature is 1100 ℃。
4. the industrial method of the 1 production battery-level lithium carbonate is wanted according to right, it is characterised in that described a period of time is 7 A hour.
5. the industrial method of the 1 production battery-level lithium carbonate is wanted according to right, it is characterised in that described a period of time is 10 A hour.
6. the industrial method of the 1 production battery-level lithium carbonate is wanted according to right, it is characterised in that sulphur in the step (3) By the surface of saturated sodium carbonate solution atomized spray to lithium sulfate solution when sour lithium solution is slowly added into reactor.
CN201711119014.5A 2017-11-14 2017-11-14 A kind of industrial method for producing battery-level lithium carbonate Pending CN107902679A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112850758A (en) * 2021-01-29 2021-05-28 中国恩菲工程技术有限公司 Lithium extraction system and method for salt lake brine
CN113636578A (en) * 2021-09-10 2021-11-12 宜春银锂新能源有限责任公司 Process for preparing lithium carbonate from lepidolite to improve quality

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1003008B (en) * 1985-04-01 1989-01-04 广州有色金属研究院 Process for preparing lithium carbonate by treating lepidolite with potassium sulfate method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1003008B (en) * 1985-04-01 1989-01-04 广州有色金属研究院 Process for preparing lithium carbonate by treating lepidolite with potassium sulfate method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112850758A (en) * 2021-01-29 2021-05-28 中国恩菲工程技术有限公司 Lithium extraction system and method for salt lake brine
CN113636578A (en) * 2021-09-10 2021-11-12 宜春银锂新能源有限责任公司 Process for preparing lithium carbonate from lepidolite to improve quality

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Application publication date: 20180413