CN108017072A - A kind of preparation method of lithium carbonate - Google Patents
A kind of preparation method of lithium carbonate Download PDFInfo
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- CN108017072A CN108017072A CN201610960397.8A CN201610960397A CN108017072A CN 108017072 A CN108017072 A CN 108017072A CN 201610960397 A CN201610960397 A CN 201610960397A CN 108017072 A CN108017072 A CN 108017072A
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- Prior art keywords
- lithium
- spodumene
- lithium carbonate
- sulfuric acid
- carbonate
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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
- C01D15/08—Carbonates; Bicarbonates
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of preparation method of lithium carbonate, including：By the enrichment of natural spodumene into concentrate, revolution kiln roasting is sent into, the α spodumenes in ore is changed into beta spodumene, stops heating, natural cooling；When spodumene temperature is down to 80 120 DEG C, crushed, sieved, added in excessive concentrated sulfuric acid feeding converter and sinter, water-soluble lithium sulfate is made with water extraction again in sulfuric acid sintering block；It is 5.5 6.5 that excessive sulfuric acid is neutralized to pH, and filtering, removes calcium, magnesium, iron, aluminium by filtrate, then decolourize, and saturation lithium sulfate solution is made after feed liquid is concentrated；Saturated sodium carbonate solution is added in saturation lithium sulfate solution, generation lithium carbonate precipitation, precipitation and separation, obtains the lithium carbonate that product purity is more than 70%, repeats hot water washing, obtains the lithium carbonate that purity is 96 97%, dry, to obtain the final product；Preparation method of the present invention is simple, and energy consumption substantially reduces, and improves the economic benefit of enterprise.
Description
Technical field
The present invention relates to lithium compound preparing technical field, is specifically a kind of preparation method of lithium carbonate.
Background technology
Lithium carbonate is the raw material of lithium metal and various lithium compounds, mainly for the preparation of various lithium chemicals and aluminium metallurgy work
Industry, is also used for heat resistant glass, cellular glass and sedative etc., and pure Lithium Carbonate is the electricity such as magnetic material, optical instrument, dielectric
The necessity of sub- industry.
The preparation method of lithium carbonate has several at present, and one kind is to utilize liquid fossil, such as salt lake bittern, mineral spring and well halogen
In, its content only has some thousandths of, and calcium phosphate precipitation-ion-exchange or solvent extraction is usually used.Also one kind is
Using solid mineral, such as spodumene, wherein oxide containing lithium reaches as high as 8%, the method that lithium carbonate is prepared currently with solid mineral
There are sulfating roasting method, chloride roasting method etc., but use the block after roasting method firing still to contain many impurity, locate
Managing the big and current roast method of difficulty requires temperature high, and energy waste is big, therefore, researches and develops a kind of preparation of new lithium carbonate
Method is very necessary.
The content of the invention
The purpose of the present invention is high aiming at temperature requirement during preparing lithium carbonate using roasting method at present, energy waste
Greatly, a kind of the problem of and later stage impurity is not easy to remove, there is provided preparation method of lithium carbonate.
A kind of preparation method of lithium carbonate of the present invention, comprises the following steps：
（1）Natural spodumene is sent into rotary furnace, at 600-800 DEG C through beneficiation enrichment into the concentrate that oxide containing lithium is 3-5%
At a temperature of carry out vacuum baking, α-spodumene in ore is changed into β-spodumene, stop heating, natural cooling；
（2）When spodumene temperature is down to 80-120 DEG C, crushed, sieved, added the excessive concentrated sulfuric acid, be sent into after mixing
Sulphation sintering is carried out in converter, sulfuric acid sintering block is used into water extraction again, water-soluble lithium sulfate is made；
（3）It is 5.5-6.5 that the sulfuric acid of leaching liquid excess is neutralized to pH with calcium carbonate, filtering, by filtrate with chemical method remove calcium,
Magnesium, iron, aluminium, are then decolourized with carbon black again, and are filtered after feed liquid is concentrated, and saturation lithium sulfate solution is made；
（4）Saturated sodium carbonate solution, generation lithium carbonate precipitation, completely rear filtering point to be precipitated are added in saturation lithium sulfate solution
From, the lithium carbonate that product purity is more than 70% is obtained, repeats hot water washing, obtains the lithium carbonate that purity is 96-97%, it is dry,
To obtain the final product.
Spodumene is carried out vacuum and low temperature roasting by the present invention using spodumene as waste lithium carbonate in preparation process
Afterwards, then crush again, concentrated sulfuric acid oxidation removes a part of impurity and generates lithium sulfate at the same time, then the impurity in lithium sulfate is chemical
Impurity removal method is decolourized after removing using carbon black, and addition saturated sodium carbonate generation lithium carbonate precipitation after saturation lithium sulfate solution is made,
Washing, obtains the lithium carbonate that purity is 96-97%, and energy consumption substantially reduces in whole process, improves the economic effect of enterprise
Benefit.
Embodiment
Embodiment 1
A kind of preparation method of lithium carbonate, comprises the following steps：
（1）Natural spodumene is sent into rotary furnace, at a temperature of 600 DEG C through beneficiation enrichment into the concentrate that oxide containing lithium is 3%
Roasted, α-spodumene in ore is changed into β-spodumene, stop heating, natural cooling；
（2）When spodumene temperature is down to 80 DEG C, crushed, sieved, added the excessive concentrated sulfuric acid, be sent into converter after mixing
Middle progress sulphation sintering, uses water extraction by sulfuric acid sintering block, water-soluble lithium sulfate is made again；
（3）The sulfuric acid of leaching liquid excess is neutralized to pH as 5.5 with calcium carbonate, filtering, by filtrate with chemical method remove calcium, magnesium,
Iron, aluminium, are then decolourized with carbon black again, and are filtered after feed liquid is concentrated, and saturation lithium sulfate solution is made；
（4）Saturated sodium carbonate solution, generation lithium carbonate precipitation, completely rear filtering point to be precipitated are added in saturation lithium sulfate solution
From, the lithium carbonate that product purity is more than 70% is obtained, repeats hot water washing, obtains the lithium carbonate that purity is 96%, it is dry, i.e.,
.
Embodiment 2
A kind of preparation method of lithium carbonate, comprises the following steps：
（1）Natural spodumene is sent into rotary furnace, at a temperature of 800 DEG C through beneficiation enrichment into the concentrate that oxide containing lithium is 5%
Roasted, α-spodumene in ore is changed into β-spodumene, stop heating, natural cooling；
（2）When spodumene temperature is down to 120 DEG C, crushed, sieved, add the excessive concentrated sulfuric acid, be sent into turn after mixing
Sulphation sintering is carried out in stove, sulfuric acid sintering block is used into water extraction again, water-soluble lithium sulfate is made；
（3）The sulfuric acid of leaching liquid excess is neutralized to pH as 6.5 with calcium carbonate, filtering, by filtrate with chemical method remove calcium, magnesium,
Iron, aluminium, are then decolourized with carbon black again, and are filtered after feed liquid is concentrated, and saturation lithium sulfate solution is made；
（4）Saturated sodium carbonate solution, generation lithium carbonate precipitation, completely rear filtering point to be precipitated are added in saturation lithium sulfate solution
From, the lithium carbonate that product purity is more than 70% is obtained, repeats hot water washing, obtains the lithium carbonate that purity is 97%, it is dry, i.e.,
.
Claims (1)
1. a kind of preparation method of lithium carbonate, it is characterised in that comprise the following steps：
（1）Natural spodumene is sent into rotary furnace, at 600-800 DEG C through beneficiation enrichment into the concentrate that oxide containing lithium is 3-5%
At a temperature of roasted, α-spodumene in ore is changed into β-spodumene, stop heating, natural cooling；
（2）When spodumene temperature is down to 80-120 DEG C, crushed, sieved, added the excessive concentrated sulfuric acid, be sent into after mixing
Sulphation sintering is carried out in converter, sulfuric acid sintering block is used into water extraction again, water-soluble lithium sulfate is made；
（3）It is 5.5-6.5 that the sulfuric acid of leaching liquid excess is neutralized to pH with calcium carbonate, filtering, by filtrate with chemical method remove calcium,
Magnesium, iron, aluminium, are then decolourized with carbon black again, and are filtered after feed liquid is concentrated, and saturation lithium sulfate solution is made；
（4）Saturated sodium carbonate solution, generation lithium carbonate precipitation, completely rear filtering point to be precipitated are added in saturation lithium sulfate solution
From, the lithium carbonate that product purity is more than 70% is obtained, repeats hot water washing, obtains the lithium carbonate that purity is 96-97%, it is dry,
To obtain the final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610960397.8A CN108017072A (en) | 2016-10-28 | 2016-10-28 | A kind of preparation method of lithium carbonate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610960397.8A CN108017072A (en) | 2016-10-28 | 2016-10-28 | A kind of preparation method of lithium carbonate |
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| CN108017072A true CN108017072A (en) | 2018-05-11 |
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| CN201610960397.8A Pending CN108017072A (en) | 2016-10-28 | 2016-10-28 | A kind of preparation method of lithium carbonate |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793205A (en) * | 2018-09-18 | 2018-11-13 | 萍乡市拓源实业有限公司 | A kind of technique that spodumene sulfuric acid process prepares lithium carbonate |
| CN109371227A (en) * | 2018-12-19 | 2019-02-22 | 王永成 | The sulfuric acid process of spodumene magnetic material proposes lithium technique |
| CN110372016A (en) * | 2019-09-04 | 2019-10-25 | 泉州市缘创环保科技有限公司 | A kind of technique synthesizing battery-level lithium carbonate from amblygonite using acidization |
| CN112624159A (en) * | 2020-12-22 | 2021-04-09 | 成都大川锂电科技有限公司 | Method for extracting spodumene by adopting sulfuric acid nano atomization process |
| CN113046548A (en) * | 2021-04-07 | 2021-06-29 | 重庆天海电池材料有限公司 | Beneficiation method for low-grade spodumene raw ore |
| CN113104868A (en) * | 2021-04-07 | 2021-07-13 | 重庆天海电池材料有限公司 | Method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene |
| CN114349031A (en) * | 2020-03-16 | 2022-04-15 | 东北大学 | Suspension roasting method for spodumene concentrate and method for extracting lithium by suspension roasting of spodumene concentrate |
-
2016
- 2016-10-28 CN CN201610960397.8A patent/CN108017072A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793205A (en) * | 2018-09-18 | 2018-11-13 | 萍乡市拓源实业有限公司 | A kind of technique that spodumene sulfuric acid process prepares lithium carbonate |
| CN109371227A (en) * | 2018-12-19 | 2019-02-22 | 王永成 | The sulfuric acid process of spodumene magnetic material proposes lithium technique |
| CN110372016A (en) * | 2019-09-04 | 2019-10-25 | 泉州市缘创环保科技有限公司 | A kind of technique synthesizing battery-level lithium carbonate from amblygonite using acidization |
| CN114349031A (en) * | 2020-03-16 | 2022-04-15 | 东北大学 | Suspension roasting method for spodumene concentrate and method for extracting lithium by suspension roasting of spodumene concentrate |
| CN112624159A (en) * | 2020-12-22 | 2021-04-09 | 成都大川锂电科技有限公司 | Method for extracting spodumene by adopting sulfuric acid nano atomization process |
| CN112624159B (en) * | 2020-12-22 | 2023-05-02 | 成都大川锂电科技有限公司 | Method for extracting spodumene by adopting sulfuric acid nano atomization process |
| CN113046548A (en) * | 2021-04-07 | 2021-06-29 | 重庆天海电池材料有限公司 | Beneficiation method for low-grade spodumene raw ore |
| CN113104868A (en) * | 2021-04-07 | 2021-07-13 | 重庆天海电池材料有限公司 | Method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180511 |
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