CN110643832A - Method for extracting lithium from fly ash - Google Patents

Method for extracting lithium from fly ash Download PDF

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Publication number
CN110643832A
CN110643832A CN201911070888.5A CN201911070888A CN110643832A CN 110643832 A CN110643832 A CN 110643832A CN 201911070888 A CN201911070888 A CN 201911070888A CN 110643832 A CN110643832 A CN 110643832A
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Prior art keywords
fly ash
drying
steps
following
crystal
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CN201911070888.5A
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Inventor
廖家隆
韦梦蝶
梁兴东
唐胜群
潘艳明
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Guangxi Chinese Coal Geology Co Ltd
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Guangxi Chinese Coal Geology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10Obtaining alkali metals
    • C22B26/12Obtaining lithium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006Wet processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/02Working-up flue dust
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention relates to the technical field of extracting lithium from fly ash, and discloses a method for extracting lithium from fly ash, which comprises the following steps: taking fly ash; step two: leaching treatment; step three: acidifying the leachate; step four: filtering; step five: heating and crystallizing; step six: drying treatment; step seven: carbon dioxide is added. The method for extracting lithium from fly ash can avoid resource waste, save production cost and increase enterprise benefits.

Description

Method for extracting lithium from fly ash
Technical Field
The invention relates to the technical field of lithium extraction from fly ash, in particular to a method for extracting lithium from fly ash.
Background
Along with the development of the coal-electricity industry in China, the yield of the fly ash is rapidly increased year by year, so that the utilization of the fly ash also becomes a problem of comprehensive utilization of environmental protection resources which needs to be solved urgently. In recent years, with the intensive research on fly ash, particularly high-alumina fly ash, the coal and fly ash in inner Mongolia, Shanxi and other places contain high-content lithium, and the content of lithium oxide in part of fly ash is up to 8000g/t, so that the industrial grade of pegmatite independent lithium ore is achieved, and the pegmatite independent lithium ore has high extraction value.
Lithium is the lightest metal in nature and has extremely strong electrochemical activity, and the metal and the compound thereof are widely applied to industries and fields of glass, ceramic aluminum smelting, organic chemical industry, aerospace, nuclear fusion and the like as explosives of thermonuclear fusion (hydrogen bomb), high-performance propelling fuels of airplanes, rockets and missiles and shielding materials of nuclear reactors. The lithium battery has 4-30 times higher energy storage than a common battery, has good service performance, and can be used as the driving force of torpedoes, submarines and spacecraft for a long time. The lithium aluminum and lithium magnesium alloy has high strength and light weight, is a good material for aerospace and rocket, and is favored by military industry and aerospace industry.
The patent number CN108265176A discloses a method for extracting lithium from fly ash, which comprises the following steps: performing leaching pretreatment on the fly ash to obtain a leaching clear solution with the mass concentration of 5-10 mol/L, wherein the mass concentration of Li < + > is 0.1-8 g/L, Al3 < + >, and the mass concentration of 50-80 g/L, Cl < - >; acidifying the leached clear liquid to obtain acidified leaching liquid with the acidity of 0.01-0.1 mol/L as an extraction water phase; preparing an extraction system with tributyl phosphate as an extractant and FeCl3 as a co-extractant to form an extracted organic phase; an extraction step and a back extraction step. According to the method disclosed by the invention, the traditional method for extracting lithium from the fly ash is abandoned, and the lithium in the fly ash is extracted by a method of firstly leaching the fly ash and then extracting leaching solution.
However, the precipitates obtained in the above patents are not recycled, and are not in accordance with the concept of recycling, so that the waste of resources is caused, the production cost is increased, and the purity of the obtained lithium cannot be ensured finally.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for extracting lithium from fly ash, which has the advantages of avoiding resource waste, saving production cost, increasing enterprise benefits and the like, and solves the problems that the precipitate obtained by the existing lithium extraction method is not subjected to corresponding recycling measures, does not conform to the recycling concept, causes resource waste, increases production cost and finally cannot ensure the purity of the obtained lithium.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a method for extracting lithium from fly ash comprises the following specific steps:
the method comprises the following steps: taking fly ash, selecting a certain amount of coal blocks from a coal mine, crushing the coal blocks into small crushed blocks, then burning the small crushed blocks, collecting flue gas generated in the burning process, and finally collecting and catching the flue gas containing fine fly ash powder to obtain the fly ash;
step two: leaching, namely selecting a certain amount of fly ash in the step one, adding a certain amount of solution into the fly ash to fully mix the fly ash with water, and filtering a mixed solution of the fly ash and the water after mixing to obtain a fly ash leaching solution;
step three: acidifying the leachate, adding potassium carbonate and sodium carbonate into the leachate in the second step, wherein three addition processes are required to be ensured when the potassium carbonate and the sodium carbonate are added, namely the first process: adding twenty percent of the total volume of the leachate, and stirring by a stirring rod, wherein the second process comprises the following steps: adding fifty percent of the total volume of the leachate, and carrying out second stirring through a stirring rod, wherein the third process comprises the following steps: adding thirty percent of the total volume of the leachate, and stirring for the third time by using a stirring rod to finally obtain acidic leachate;
step four: filtering, namely filtering the liquid after the potassium carbonate and the sodium carbonate are completely added in the third step and completely react with the leachate, and separating solid substances from the liquid after the reaction;
step five: and (3) heating and crystallizing, namely placing the filtered liquid in the fourth step on a heating furnace for heating and crystallizing, wherein the heating temperature of the heating furnace is divided into three stages, namely a first stage: the temperature range of the heating furnace is 10-45 ℃, the heating time is 10-12 minutes, and the second stage is as follows: the temperature range of the heating furnace is 45-60 ℃, the heating time is 15-25 minutes, and the third stage is as follows: the temperature range of the heating furnace is 60-20 ℃, and the heating time is 8-10 minutes;
step six: drying, namely drying the crystal obtained in the step five, and quickly drying the crystal in a drying furnace;
step seven: carbon dioxide is added, and the crystal is dissolved in the aqueous solution vaporized by carbon dioxide, and the crystal and the aqueous solution vaporized by carbon dioxide are heated to dissolve the crystal and obtain lithium.
Preferably, a multi-stage crusher is used for crushing the coal blocks in the step one.
Preferably, the fly ash is collected in the first step by introducing the flue gas into a dust remover, so that the fly ash in the flue gas enters an ash hopper of the dust remover.
Preferably, in the second step, the fly ash and water are placed in a beaker, and then the beaker is placed on an oscillator, so that the fly ash and water in the beaker are fully mixed.
Preferably, the solid obtained in the fourth step is separated and then put into hot water to be heat-treated so that the solid is dissolved, and then potassium carbonate and sodium carbonate are added again to obtain a solid matter, which is repeated three to four times.
Preferably, the drying temperature range of the drying oven in the sixth step is as follows: 100 ℃ and 200 ℃, and the drying time is 2-4 hours.
Preferably, when the crystalline substance is dried in the sixth step, in order to ensure the drying effect and speed of the crystalline substance, a shaking mechanism is arranged in the drying furnace, so that the phenomenon that the crystalline substance shakes inside the drying furnace can be ensured, and the drying effect and drying speed of the crystalline substance can be improved.
Preferably, the heating temperature in the seventh step is 30 ℃.
(III) advantageous effects
Compared with the prior art, the invention provides a method for extracting lithium from fly ash, which has the following beneficial effects:
1. the method for extracting lithium from fly ash comprises the following steps: taking fly ash; step two: leaching treatment; step three: acidifying the leachate; step four: filtering; step five: heating and crystallizing; step six: drying treatment; step seven: the carbon dioxide is added, so that the precipitate can be treated for multiple times, the waste of resources is avoided, the production cost is saved, the benefit of enterprises is increased, and the purity of the obtained lithium is higher.
Detailed Description
The invention discloses a method for extracting lithium from fly ash, which can be realized by appropriately improving process parameters by taking the contents of the text as reference by a person skilled in the art. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the lithium extraction method of the present invention has been described in terms of preferred embodiments, it will be apparent to those skilled in the art that the techniques of the present invention may be implemented and applied by modifying or appropriately modifying or combining the lithium extraction methods described herein without departing from the spirit, scope, and spirit of the invention. 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 invention is further illustrated by the following examples.
A method for extracting lithium from fly ash comprises the following specific steps:
the method comprises the following steps: taking fly ash, selecting a certain amount of coal blocks from a coal mine, crushing the coal blocks into small crushed blocks, then burning the small crushed blocks, collecting flue gas generated in the burning process, and finally collecting and catching the flue gas containing fine fly ash powder to obtain the fly ash;
step two: leaching, namely selecting a certain amount of fly ash in the step one, adding a certain amount of solution into the fly ash to fully mix the fly ash with water, and filtering a mixed solution of the fly ash and the water after mixing to obtain a fly ash leaching solution;
step three: acidifying the leachate, adding potassium carbonate and sodium carbonate into the leachate in the second step, wherein three addition processes are required to be ensured when the potassium carbonate and the sodium carbonate are added, namely the first process: adding twenty percent of the total volume of the leachate, and stirring by a stirring rod, wherein the second process comprises the following steps: adding fifty percent of the total volume of the leachate, and carrying out second stirring through a stirring rod, wherein the third process comprises the following steps: adding thirty percent of the total volume of the leachate, and stirring for the third time by using a stirring rod to finally obtain acidic leachate;
step four: filtering, namely filtering the liquid after the potassium carbonate and the sodium carbonate are completely added in the third step and completely react with the leachate, and separating solid substances from the liquid after the reaction;
step five: and (3) heating and crystallizing, namely placing the filtered liquid in the fourth step on a heating furnace for heating and crystallizing, wherein the heating temperature of the heating furnace is divided into three stages, namely a first stage: the temperature range of the heating furnace is 10-45 ℃, the heating time is 10-12 minutes, and the second stage is as follows: the temperature range of the heating furnace is 45-60 ℃, the heating time is 15-25 minutes, and the third stage is as follows: the temperature range of the heating furnace is 60-20 ℃, and the heating time is 8-10 minutes;
step six: drying, namely drying the crystal obtained in the step five, and quickly drying the crystal in a drying furnace;
step seven: carbon dioxide is added, and the crystal is dissolved in the aqueous solution vaporized by carbon dioxide, and the crystal and the aqueous solution vaporized by carbon dioxide are heated to dissolve the crystal and obtain lithium.
And in the step one, a multi-stage crusher is adopted when the coal blocks are crushed.
The fly ash collecting mode in the first step is to introduce the flue gas into a dust remover, so that the fly ash in the flue gas enters an ash hopper of the dust remover.
And in the second step, the fly ash and water are placed into a beaker, and then the beaker is placed on an oscillator, so that the fly ash and the water in the beaker are fully mixed.
The solid obtained in the fourth step is separated and then put into hot water to be heat-treated so that the solid is dissolved, and then potassium carbonate and sodium carbonate are added again to obtain a solid matter, which is repeated three to four times.
The drying temperature range of the drying furnace in the step six is as follows: 100 ℃ and 200 ℃, and the drying time is 2-4 hours.
In the sixth step, when the crystalline substance is dried, in order to ensure the drying effect and speed of the crystalline substance, the shaking mechanism is arranged in the drying furnace, so that the phenomenon that the crystalline substance shakes in the drying furnace can be ensured, and the drying effect and the drying speed of the crystalline substance can be improved.
And the heating temperature in the seventh step is 30 ℃.
In summary, through the steps of: taking fly ash; step two: leaching treatment; step three: acidifying the leachate; step four: filtering; step five: heating and crystallizing; step six: drying treatment; step seven: the carbon dioxide is added, so that the precipitate can be treated for multiple times, the waste of resources is avoided, the production cost is saved, the benefit of enterprises is increased, and the purity of the obtained lithium is higher.
It is to be noted that the term "comprises," "comprising," or any other variation thereof is intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
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 (8)

1. The method for extracting lithium from fly ash is characterized by comprising the following specific steps:
the method comprises the following steps: taking fly ash, selecting a certain amount of coal blocks from a coal mine, crushing the coal blocks into small crushed blocks, then burning the small crushed blocks, collecting flue gas generated in the burning process, and finally collecting and catching the flue gas containing fine fly ash powder to obtain the fly ash;
step two: leaching, namely selecting a certain amount of fly ash in the step one, adding a certain amount of solution into the fly ash to fully mix the fly ash with water, and filtering a mixed solution of the fly ash and the water after mixing to obtain a fly ash leaching solution;
step three: acidifying the leachate, adding potassium carbonate and sodium carbonate into the leachate in the second step, wherein three addition processes are required to be ensured when the potassium carbonate and the sodium carbonate are added, namely the first process: adding twenty percent of the total volume of the leachate, and stirring by a stirring rod, wherein the second process comprises the following steps: adding fifty percent of the total volume of the leachate, and carrying out second stirring through a stirring rod, wherein the third process comprises the following steps: adding thirty percent of the total volume of the leachate, and stirring for the third time by using a stirring rod to finally obtain acidic leachate;
step four: filtering, namely filtering the liquid after the potassium carbonate and the sodium carbonate are completely added in the third step and completely react with the leachate, and separating solid substances from the liquid after the reaction;
step five: and (3) heating and crystallizing, namely placing the filtered liquid in the fourth step on a heating furnace for heating and crystallizing, wherein the heating temperature of the heating furnace is divided into three stages, namely a first stage: the temperature range of the heating furnace is 10-45 ℃, the heating time is 10-12 minutes, and the second stage is as follows: the temperature range of the heating furnace is 45-60 ℃, the heating time is 15-25 minutes, and the third stage is as follows: the temperature range of the heating furnace is 60-20 ℃, and the heating time is 8-10 minutes;
step six: drying, namely drying the crystal obtained in the step five, and quickly drying the crystal in a drying furnace;
step seven: carbon dioxide is added, and the crystal is dissolved in the aqueous solution vaporized by carbon dioxide, and the crystal and the aqueous solution vaporized by carbon dioxide are heated to dissolve the crystal and obtain lithium.
2. The method for extracting lithium from fly ash according to claim 1, wherein the method comprises the following steps: and in the first step, a multi-stage crusher is adopted when the coal blocks are crushed.
3. The method for extracting lithium from fly ash according to claim 1, wherein the method comprises the following steps: the fly ash collecting mode in the first step is to introduce the flue gas into a dust remover, so that the fly ash in the flue gas enters an ash hopper of the dust remover.
4. The method for extracting lithium from fly ash according to claim 1, wherein the method comprises the following steps: and in the second step, the fly ash and water are placed into a beaker, and the beaker is placed on an oscillator, so that the fly ash and the water in the beaker are fully mixed.
5. The method for extracting lithium from fly ash according to claim 1, wherein the method comprises the following steps: the solid obtained in the fourth step is separated and then put into hot water to be heated so that the solid is dissolved, and then potassium carbonate and sodium carbonate are added again to obtain a solid matter, which is repeated three to four times.
6. The method for extracting lithium from fly ash according to claim 1, wherein the method comprises the following steps: the drying temperature range of the drying furnace in the sixth step is as follows: 100 ℃ and 200 ℃, and the drying time is 2-4 hours.
7. The method for extracting lithium from fly ash according to claim 1, wherein the method comprises the following steps: and in the sixth step, when the crystal is dried, in order to ensure the drying effect and speed of the crystal, a shaking mechanism is arranged in the drying furnace, so that the phenomenon that the crystal shakes in the drying furnace can be ensured, and the drying effect and the drying speed of the crystal can be improved.
8. The method for extracting lithium from fly ash according to claim 1, wherein the method comprises the following steps: and the heating temperature in the seventh step is 30 ℃.
CN201911070888.5A 2019-11-05 2019-11-05 Method for extracting lithium from fly ash Pending CN110643832A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118130325A (en) * 2024-05-06 2024-06-04 中国煤炭地质总局勘查研究总院 Experimental device for survey different granularity fly ash lithium leaching rates

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CN102923743A (en) * 2012-11-19 2013-02-13 河北工程大学 Technical method for comprehensively extracting aluminum and lithium from coal ash through acid process
CN102923742A (en) * 2012-11-19 2013-02-13 河北工程大学 Method for comprehensively extracting aluminum and lithium from coal ash
CN103101935A (en) * 2012-12-28 2013-05-15 中国神华能源股份有限公司 Method for preparing lithium carbonate from coal ash
CN104477948A (en) * 2014-12-03 2015-04-01 宋英宏 Method for extracting lithium carbonate from coal ashes
CN105692659A (en) * 2016-01-26 2016-06-22 中国科学院过程工程研究所 Method for extracting lithium from fly ash
CN107619952A (en) * 2017-09-15 2018-01-23 山东大学 A kind of method that lithium is leached from flyash
CN108588445A (en) * 2018-04-18 2018-09-28 成都新柯力化工科技有限公司 A method of refining lithium using the continuously extruded Rapid Leaching from flyash of screw rod
CN109354046A (en) * 2018-11-08 2019-02-19 中国神华能源股份有限公司 A method of lithium carbonate is prepared using dirty mother liquor is steamed
CN109721081A (en) * 2019-02-25 2019-05-07 河北工程大学 A method of extracting lithium from rich lithium flyash alkaline process mother liquor

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102923743A (en) * 2012-11-19 2013-02-13 河北工程大学 Technical method for comprehensively extracting aluminum and lithium from coal ash through acid process
CN102923742A (en) * 2012-11-19 2013-02-13 河北工程大学 Method for comprehensively extracting aluminum and lithium from coal ash
CN103101935A (en) * 2012-12-28 2013-05-15 中国神华能源股份有限公司 Method for preparing lithium carbonate from coal ash
CN104477948A (en) * 2014-12-03 2015-04-01 宋英宏 Method for extracting lithium carbonate from coal ashes
CN105692659A (en) * 2016-01-26 2016-06-22 中国科学院过程工程研究所 Method for extracting lithium from fly ash
CN107619952A (en) * 2017-09-15 2018-01-23 山东大学 A kind of method that lithium is leached from flyash
CN108588445A (en) * 2018-04-18 2018-09-28 成都新柯力化工科技有限公司 A method of refining lithium using the continuously extruded Rapid Leaching from flyash of screw rod
CN109354046A (en) * 2018-11-08 2019-02-19 中国神华能源股份有限公司 A method of lithium carbonate is prepared using dirty mother liquor is steamed
CN109721081A (en) * 2019-02-25 2019-05-07 河北工程大学 A method of extracting lithium from rich lithium flyash alkaline process mother liquor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118130325A (en) * 2024-05-06 2024-06-04 中国煤炭地质总局勘查研究总院 Experimental device for survey different granularity fly ash lithium leaching rates

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Application publication date: 20200103