RU2006107861A - METHOD FOR PRODUCING HIGH PURE LITHIUM FLUORIDE - Google Patents

METHOD FOR PRODUCING HIGH PURE LITHIUM FLUORIDE Download PDF

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RU2006107861A
RU2006107861A RU2006107861/15A RU2006107861A RU2006107861A RU 2006107861 A RU2006107861 A RU 2006107861A RU 2006107861/15 A RU2006107861/15 A RU 2006107861/15A RU 2006107861 A RU2006107861 A RU 2006107861A RU 2006107861 A RU2006107861 A RU 2006107861A
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RU
Russia
Prior art keywords
lithium
solution
technical
fluoride
carbonate
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RU2006107861/15A
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Russian (ru)
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RU2330811C2 (en
Inventor
Ирина Владимировна Шемякина (RU)
Ирина Владимировна Шемякина
Сергей Владимирович Шемякин (RU)
Сергей Владимирович Шемякин
Виктор Васильевич Мухин (RU)
Виктор Васильевич Мухин
Евгений Павлович Муратов (RU)
Евгений Павлович Муратов
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Открытое акционерное общество "Новосибирский завод химконцентратов" (RU)
Открытое акционерное общество "Новосибирский завод химконцентратов"
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Priority to RU2006107861/15A priority Critical patent/RU2330811C2/en
Publication of RU2006107861A publication Critical patent/RU2006107861A/en
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Publication of RU2330811C2 publication Critical patent/RU2330811C2/en

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Abstract

Способ получения высокочистого фторида лития из технических солей лития, включающий перевод технических солей лития в раствор гидрокарбоната лития путем обработки водных растворов технических солей лития углекислым газом, сорбционную очистку их на катионообменной смоле, получение очищенного карбоната лития, промывку его, приготовление водной пульпы очищенного карбоната лития, повторный процесс бикарбонизации водной пульпы карбоната лития углекислым газом и получение из него раствора гидрокарбоната лития, последующее фторирование, промывку и сушку полученного фторида лития, отличающийся тем, что в качестве технических солей лития используют технический карбонат лития или гидроксид лития, фторирование проводят медленным добавлением с постоянным перемешиванием раствора гидрокарбоната лития в реактор, заполненный раствором фтороводорода с 10-30% избытком от стехиометрии, промывку фторида лития проводят дистиллированной водой без COили 1% раствором фтороводорода, а сушку его осуществляют в две стадии в вакуумной печи, при этом температура сушки 1-ой стадии составляет не выше 100°С, а температура сушки 2-ой стадии - не выше 150°С.A method for producing high-purity lithium fluoride from technical lithium salts, including the conversion of technical lithium salts to a solution of lithium hydrogen carbonate by treating aqueous solutions of technical lithium salts with carbon dioxide, sorption cleaning them on a cation exchange resin, obtaining purified lithium carbonate, washing it, preparing an aqueous pulp of purified lithium carbonate the repeated process of bicarbonization of an aqueous pulp of lithium carbonate with carbon dioxide and obtaining a solution of lithium hydrogen carbonate from it, followed by fluorination, washing and drying the obtained lithium fluoride, characterized in that technical lithium carbonates or lithium hydroxide are used as technical lithium salts, fluorination is carried out by slow addition with constant stirring of a solution of lithium hydrogen carbonate in a reactor filled with a solution of hydrogen fluoride with 10-30% excess from stoichiometry, washing lithium fluoride is carried out with distilled water without CO or 1% hydrogen fluoride solution, and it is dried in two stages in a vacuum oven, while the drying temperature of the first stage is ie above 100 ° C, and the drying temperature 2nd step - not higher than 150 ° C.

Claims (1)

Способ получения высокочистого фторида лития из технических солей лития, включающий перевод технических солей лития в раствор гидрокарбоната лития путем обработки водных растворов технических солей лития углекислым газом, сорбционную очистку их на катионообменной смоле, получение очищенного карбоната лития, промывку его, приготовление водной пульпы очищенного карбоната лития, повторный процесс бикарбонизации водной пульпы карбоната лития углекислым газом и получение из него раствора гидрокарбоната лития, последующее фторирование, промывку и сушку полученного фторида лития, отличающийся тем, что в качестве технических солей лития используют технический карбонат лития или гидроксид лития, фторирование проводят медленным добавлением с постоянным перемешиванием раствора гидрокарбоната лития в реактор, заполненный раствором фтороводорода с 10-30% избытком от стехиометрии, промывку фторида лития проводят дистиллированной водой без CO2 или 1% раствором фтороводорода, а сушку его осуществляют в две стадии в вакуумной печи, при этом температура сушки 1-ой стадии составляет не выше 100°С, а температура сушки 2-ой стадии - не выше 150°С.A method for producing high-purity lithium fluoride from technical lithium salts, including the conversion of technical lithium salts to a solution of lithium hydrogen carbonate by treating aqueous solutions of technical lithium salts with carbon dioxide, sorption cleaning them on a cation exchange resin, obtaining purified lithium carbonate, washing it, preparing an aqueous pulp of purified lithium carbonate the repeated process of bicarbonization of an aqueous pulp of lithium carbonate with carbon dioxide and obtaining a solution of lithium hydrogen carbonate from it, followed by fluorination, washing and drying the obtained lithium fluoride, characterized in that technical lithium carbonates or lithium hydroxide are used as technical lithium salts, fluorination is carried out by slow addition with constant stirring of a solution of lithium hydrogen carbonate in a reactor filled with a solution of hydrogen fluoride with 10-30% excess from stoichiometry, washing lithium fluoride is carried out with distilled water without CO 2 or 1% solution of hydrogen fluoride, and its drying is carried out in two stages in a vacuum oven, wherein the drying temperature of the first stage is not higher than 100 ° C, and the drying temperature 2nd step - not higher than 150 ° C.
RU2006107861/15A 2006-03-13 2006-03-13 Method of obtaining high-purity lithium fluoride RU2330811C2 (en)

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RU2006107861A true RU2006107861A (en) 2007-09-20
RU2330811C2 RU2330811C2 (en) 2008-08-10

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105645437A (en) * 2016-01-08 2016-06-08 中国科学院上海应用物理研究所 Lithium fluoride recovery device and recovery method
CN111994924A (en) * 2020-09-09 2020-11-27 江西云锂材料股份有限公司 Novel method for producing high-purity lithium fluoride by taking industrial-grade lithium carbonate as raw material
CN117160314A (en) * 2023-08-01 2023-12-05 多氟多阳福新材料有限公司 High-purity lithium fluoride purification system of battery level

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104364198B (en) 2012-05-25 2016-07-06 朗盛德国有限责任公司 The preparation of high-purity lithium fluoride
CN103553086B (en) * 2013-11-18 2015-07-29 上海晶纯生化科技股份有限公司 A kind of method preparing high purity lithium fluoride
CN105197966B (en) * 2015-10-29 2017-05-31 湖北省宏源药业科技股份有限公司 A kind of purification process of super-active lithium fluoride
RU2627427C1 (en) * 2016-11-18 2017-08-08 Акционерное общество "Ведущий научно-исследовательский институт химической технологии" Method for inactivation of impurity in lithium fluoride sorbent

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105645437A (en) * 2016-01-08 2016-06-08 中国科学院上海应用物理研究所 Lithium fluoride recovery device and recovery method
CN105645437B (en) * 2016-01-08 2017-04-05 中国科学院上海应用物理研究所 A kind of retracting device and its recovery method of lithium fluoride
CN111994924A (en) * 2020-09-09 2020-11-27 江西云锂材料股份有限公司 Novel method for producing high-purity lithium fluoride by taking industrial-grade lithium carbonate as raw material
CN117160314A (en) * 2023-08-01 2023-12-05 多氟多阳福新材料有限公司 High-purity lithium fluoride purification system of battery level

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Effective date: 20071122