CN1962445A - Preparation method of high-purity nano aluminium fluoride - Google Patents
Preparation method of high-purity nano aluminium fluoride Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 title claims 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 67
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Inorganic materials [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims abstract description 62
- 238000000034 method Methods 0.000 claims abstract description 22
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011347 resin Substances 0.000 claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 238000000605 extraction Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910052744 lithium Inorganic materials 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 239000012159 carrier gas Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 2
- 238000005507 spraying Methods 0.000 claims 2
- 238000004090 dissolution Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 claims 1
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 abstract description 9
- 238000000746 purification Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 239000002159 nanocrystal Substances 0.000 abstract description 5
- -1 chlorine Lithium fluoride Chemical compound 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 abstract description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 abstract description 2
- 150000002642 lithium compounds Chemical class 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 10
- 239000007921 spray Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 229910000990 Ni alloy Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
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Abstract
高纯纳米氟化锂的制备方法，以工业氯化锂和氟化氢铵为原料，氯化锂经水溶解、萃淋树脂色层法纯化、浓缩、喷雾干燥得到高纯无水氯化锂；氯化锂经氟化氢铵干法合成氟化锂。本发明相对于提纯碳酸锂、氢氧化锂等锂化合物而言，工艺简单、操作方便；采用干法合成氟化锂，引入杂质少，含水量低；合成与分离纯化在同一设备中分步完成，缩短了工艺流程，操作方便。采用本发明获得的高纯氟化锂产品为具有纳米介孔结构的类球形纳米晶聚结体，活性高。The preparation method of high-purity nano-lithium fluoride, using industrial lithium chloride and ammonium bifluoride as raw materials, lithium chloride is dissolved in water, purified by extraction resin chromatography, concentrated, and spray-dried to obtain high-purity anhydrous lithium chloride; chlorine Lithium fluoride is synthesized by dry method of ammonium bifluoride to lithium fluoride. Compared with the purification of lithium compounds such as lithium carbonate and lithium hydroxide, the present invention has simple process and convenient operation; the dry method is adopted to synthesize lithium fluoride, which has less impurities and low water content; the synthesis and separation and purification are completed step by step in the same equipment , Shorten the process flow, easy to operate. The high-purity lithium fluoride product obtained by the invention is a spherical nano-crystal aggregate with a nano-mesoporous structure, and has high activity.
Description
技术领域 本发明涉及一种高纯纳米氟化锂的制备方法。Technical Field The present invention relates to a method for preparing high-purity nano-lithium fluoride.
背景技术 锂及锂产品是二十一世纪的新型能源物资，在许多领域、尤其是新能源领域的应用越来越广泛；高纯锂产品在核聚变、航天航空、高能化学电源的应用日益增加。Background Art Lithium and lithium products are new energy materials in the 21st century, and they are widely used in many fields, especially new energy fields; high-purity lithium products are increasingly used in nuclear fusion, aerospace, and high-energy chemical power sources .
氟化锂是一种重要的锂基基础材料；高纯氟化锂主要用于高技术功能陶瓷、通讯光纤、锂离子电池等领域中。李世友等的《高纯氟化锂的制备方法与分析方法评述》(《IM & P化工矿物与加工》，2006，3：34)中综合评述了高纯氟化锂的制备方法，但实用化技术较少；至目前为止，高纯氟化锂的制备主要在液相中完成，高纯度的获得是通过对氟化锂生产原料的纯化，原料纯化过程主要为离子交换法与萃取法；通过对锂化合物氯化锂、氢氧化锂、硝酸锂等在水溶液中用离子交换、液剂萃取的方法去除杂质金属元素；再进行氟化沉淀制备高纯氟化锂。Lithium fluoride is an important lithium-based basic material; high-purity lithium fluoride is mainly used in high-tech functional ceramics, communication optical fibers, lithium-ion batteries and other fields. "Review of Preparation and Analysis Methods of High-Purity Lithium Fluoride" by Li Shiyou et al. ("IM & P Chemical Minerals and Processing", 2006, 3:34) comprehensively reviewed the preparation methods of high-purity lithium fluoride, but the practical There are few technologies; so far, the preparation of high-purity lithium fluoride is mainly completed in the liquid phase, and high purity is obtained through the purification of raw materials for lithium fluoride production. For lithium compounds lithium chloride, lithium hydroxide, lithium nitrate, etc., use ion exchange and liquid extraction methods to remove impurity metal elements in aqueous solution; then perform fluorination precipitation to prepare high-purity lithium fluoride.
由于湿法流程的特点，制备高纯氟化锂活性较低、粒度分布不均匀，难于满足作为新材料制备对原材料在活性、形貌及粒度等方面的要求。湿法制备高纯氟化锂流程长、工序转换繁以及使用原料多，过程中引入杂质较多；同时生产对设备要求高；使得产品生成成本高。Due to the characteristics of the wet process, the preparation of high-purity lithium fluoride has low activity and uneven particle size distribution, making it difficult to meet the requirements of raw materials in terms of activity, morphology and particle size for the preparation of new materials. The preparation of high-purity lithium fluoride by the wet method has a long process, complicated process conversion, and many raw materials are used, and more impurities are introduced in the process; at the same time, the production requires high equipment, which makes the production cost of the product high.
发明内容 本发明的目的是提供一种采用原料的湿法纯化和氟化锂的干法合成相结合，制备高活性纳米氟化锂的方法。SUMMARY OF THE INVENTION The purpose of the present invention is to provide a method for preparing highly active nano-lithium fluoride by combining wet purification of raw materials and dry synthesis of lithium fluoride.
高纯纳米氟化锂的制备方法，以工业氯化锂和氟化氢铵为原料，氯化锂经水溶解、萃淋树脂色层法纯化、浓缩、喷雾干燥得到高纯无水氯化锂；氯化锂经氟化氢铵干法合成氟化锂，具体过程为：The preparation method of high-purity nano-lithium fluoride, using industrial lithium chloride and ammonium bifluoride as raw materials, lithium chloride is dissolved in water, purified by extraction resin chromatography, concentrated, and spray-dried to obtain high-purity anhydrous lithium chloride; chlorine Lithium fluoride is synthesized by dry method of ammonium bifluoride to lithium fluoride, and the specific process is as follows:
(1)将工业氯化锂溶于水，配制成重量百分浓度为含锂10％～20％的水溶液；溶液经固体萃淋树脂萃取杂质金属离子，得纯化的氯化锂溶液；所用固体萃淋树脂是能有效吸附杂质金属离子的固态萃取树脂，包括P507(PC88A)萃淋树脂、P204萃淋树脂。(1) Dissolve industrial lithium chloride in water, and prepare an aqueous solution containing 10% to 20% lithium at a concentration of 10% to 20% by weight; the solution extracts impurity metal ions through a solid extraction resin to obtain a purified lithium chloride solution; the solid used Extraction resin is a solid-state extraction resin that can effectively adsorb impurity metal ions, including P507 (PC88A) extraction resin and P204 extraction resin.
(2)纯化的氯化锂溶液经加热浓缩到含氯化锂30％～40％；在喷雾干燥器内进行喷雾干燥，制得类球形、结构松散的无水高纯氯化锂。(2) The purified lithium chloride solution is heated and concentrated to contain 30% to 40% lithium chloride; it is spray-dried in a spray dryer to obtain anhydrous high-purity lithium chloride with spherical shape and loose structure.
(3)高纯氟化锂与氟化氢铵以固态形式充分混合；按氟化氢铵与氟化锂反应的化学计量，氟化氢铵过量10％～100％；使用气相法生产的氟化氢铵。(3) High-purity lithium fluoride and ammonium bifluoride are fully mixed in solid form; according to the stoichiometric reaction between ammonium bifluoride and lithium fluoride, the excess ammonium bifluoride is 10% to 100%; the ammonium bifluoride produced by gas phase method is used.
(4)将上述混合物置于一密闭的炉子中，在高纯氩气保护下于150～250℃下进行合成反应；反应时间为2～10小时。(4) The above mixture is placed in a closed furnace, and the synthesis reaction is carried out at 150-250° C. under the protection of high-purity argon; the reaction time is 2-10 hours.
(5)反应结束后，将炉温升至400～650℃，以高纯氩气作载气，驱除反应生成的氯化铵、氟化铵及过量的氟化氢铵；保温时间3～8小时。(5) After the reaction, raise the furnace temperature to 400-650°C, use high-purity argon as the carrier gas, and drive off the ammonium chloride, ammonium fluoride and excess ammonium bifluoride generated by the reaction; the holding time is 3-8 hours.
制得的产品用激光粒度仪测定其表观粒度及其分布；用SEM表征粉末形貌、TEM表征纳米晶及其晶粒大小。用原子吸收光谱法分析产品杂质金属含量，其中过渡金属元素杂质用石墨炉原子吸收法、碱金属和碱土金属元素杂质用火焰原子吸收法测定。The apparent particle size and distribution of the prepared product were measured by a laser particle size analyzer; the powder morphology was characterized by SEM, and the nanocrystal and its grain size were characterized by TEM. The impurity metal content of the product is analyzed by atomic absorption spectrometry, wherein transition metal element impurities are determined by graphite furnace atomic absorption method, and alkali metal and alkaline earth metal element impurities are determined by flame atomic absorption method.
本发明所指的高纯纳米氟化锂主要指用于锂离子电池材料、新型功能陶瓷和远程通讯光纤制造的高纯、高活性氟化锂；其特征为：材料表观为固体粉末，粒径0.5～5μm；其结构为具有纳米介孔结构的纳米氟化锂聚结体。产品LiF含量大于99.5％；总杂质金属含量少于100ppm。The high-purity nano-lithium fluoride referred to in the present invention mainly refers to high-purity and high-activity lithium fluoride used in the manufacture of lithium-ion battery materials, new functional ceramics and telecommunication optical fibers; The diameter is 0.5-5 μm; its structure is a nano-lithium fluoride aggregate with a nano-mesoporous structure. The LiF content of the product is greater than 99.5%; the total impurity metal content is less than 100ppm.
本发明采用氯化锂为原料，用固态萃淋树脂色层法进行纯化，并用喷雾干燥法制得类球形、结构松散的高纯无水氯化锂粉体；相对于提纯碳酸锂、氢氧化锂等锂化合物而言，工艺简单、操作方便；采用干法合成氟化锂，引入杂质少，含水量低；合成与分离纯化在同一设备中分步完成，缩短了工艺流程，操作方便。采用本发明获得的高纯氟化锂产品为具有纳米介孔结构的类球形纳米晶聚结体，活性高。The present invention adopts lithium chloride as a raw material, purifies by solid-state extraction resin chromatography, and uses a spray drying method to obtain a spherical, loosely structured high-purity anhydrous lithium chloride powder; compared to the purification of lithium carbonate and lithium hydroxide For lithium compounds such as lithium, the process is simple and the operation is convenient; the dry method is used to synthesize lithium fluoride, which has less impurities and low water content; the synthesis and separation and purification are completed step by step in the same equipment, which shortens the process flow and is easy to operate. The high-purity lithium fluoride product obtained by the invention is a spherical nano-crystal aggregate with a nano-mesoporous structure, and has high activity.
具体实施方式Detailed ways
以下为本发明的部分具体实施例。这些实施例的给出决不是限制本发明。The following are some specific embodiments of the present invention. These examples are given in no way to limit the invention.
实施例1Example 1
将工业氯化锂溶解于水，配制成含氯化锂15％的水溶液；用P507萃淋树脂吸附脱除杂质金属离子后，浓缩至含氯化锂40％；在适当喷雾条件下进行喷雾干燥，制成高纯无水氯化锂，产品为类球形、松散结构，中心粒径3.7微米；Dissolve industrial lithium chloride in water to prepare an aqueous solution containing 15% lithium chloride; use P507 extraction resin to adsorb and remove impurity metal ions, then concentrate to contain 40% lithium chloride; spray dry under appropriate spray conditions , made of high-purity anhydrous lithium chloride, the product is spherical, loose structure, and the central particle diameter is 3.7 microns;
按质量比2∶1将氟化氢铵与高纯无水氯化锂充分混合，装于衬钼不锈钢容器内，置于密封炉管为镍合金的加热炉内；在氩气保护下、160℃反应4小时；而后升温至500℃，用氩气作载气驱赶杂质气体，处理5小时；完成氟化锂的制备过程。Fully mix ammonium bifluoride and high-purity anhydrous lithium chloride according to the mass ratio of 2:1, put it in a molybdenum-lined stainless steel container, and place it in a heating furnace with a sealed furnace tube made of nickel alloy; under the protection of argon, react at 160 °C 4 hours; then raise the temperature to 500° C., use argon as carrier gas to drive away impurity gases, and treat for 5 hours; complete the preparation process of lithium fluoride.
高纯氟化锂产品表观中心粒径3.4微米，微观为平均粒径约43纳米、具有纳米介孔的氟化锂纳米晶聚结体。The apparent central particle size of the high-purity lithium fluoride product is 3.4 microns, and the microcosm is a lithium fluoride nanocrystal aggregate with an average particle size of about 43 nanometers and nano-mesoporous pores.
实施例2Example 2
将工业氯化锂溶解于水，配制成含氯化锂15％的水溶液；用P507萃淋树脂吸附脱除杂质金属离子后，浓缩至含氯化锂35％；在适当喷雾条件下进行喷雾干燥，制成高纯无水氯化锂，产品为类球形、松散结构，中心粒径3.1微米；Dissolve industrial lithium chloride in water to prepare an aqueous solution containing 15% lithium chloride; use P507 extraction resin to absorb and remove impurity metal ions, then concentrate to contain 35% lithium chloride; spray dry under appropriate spray conditions , made of high-purity anhydrous lithium chloride, the product is spherical, loose structure, and the central particle diameter is 3.1 microns;
按质量比1.6∶1将氟化氢铵与高纯无水氯化锂充分混合，装于衬钼不锈钢容器内，置于密封炉管为镍合金的加热炉内；在氩气保护下、200℃反应3小时；而后升温至550℃，用氩气作载气驱赶杂质气体，处理4小时；完成氟化锂的制备过程。Fully mix ammonium bifluoride and high-purity anhydrous lithium chloride according to the mass ratio of 1.6:1, put it in a molybdenum-lined stainless steel container, and place it in a heating furnace with a sealed furnace tube made of nickel alloy; under the protection of argon, react at 200 °C 3 hours; then raise the temperature to 550° C., use argon as a carrier gas to drive away impurity gases, and treat for 4 hours; complete the preparation process of lithium fluoride.
高纯氟化锂产品表观中心粒径2.6微米，微观为平均粒径约62纳米、具有纳米介孔的氟化锂纳米晶聚结体。The apparent central particle size of the high-purity lithium fluoride product is 2.6 microns, and the microcosm is a lithium fluoride nanocrystal aggregate with an average particle size of about 62 nanometers and nanometer mesopores.
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| CN103626208A (en) * | 2012-08-27 | 2014-03-12 | 枣庄海帝新能源锂电科技有限公司 | Preparation method for high-purity lithium fluoride by taking lithium hexafluorophosphate as raw material |
| 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 |
| CN106430251A (en) * | 2016-09-05 | 2017-02-22 | 中南大学 | Preparation method of micron superfine spherical sodium chloride |
| CN106430257A (en) * | 2016-10-09 | 2017-02-22 | 多氟多化工股份有限公司 | Preparation method of porous high-activity LiF and preparation method of LiFSI |
| CN119240752A (en) * | 2024-08-21 | 2025-01-03 | 江西云威新材料股份有限公司 | A method for preparing high-purity nano-scale lithium fluoride from industrial-grade lithium carbonate |
| CN119637911A (en) * | 2024-12-12 | 2025-03-18 | 湖北中誉新材料有限公司 | Method for preparing battery-grade lithium fluoride by solid-phase method |
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|---|---|---|---|---|
| JPH061264B2 (en) * | 1988-09-29 | 1994-01-05 | セントラル硝子株式会社 | Method for analysis of transition metals in fluoride |
| JP2772302B2 (en) * | 1991-06-24 | 1998-07-02 | 日本電信電話株式会社 | Method for producing high-purity metal fluoride |
| RU2277068C2 (en) * | 2004-02-26 | 2006-05-27 | Закрытое акционерное общество ЗАО "Экостар-Наутех" | Method of production of lithium fluorides for electrolytic production of aluminum (versions) |
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2006
- 2006-11-28 CN CNB2006101367511A patent/CN100447086C/en not_active Expired - Fee Related
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| CN103626208A (en) * | 2012-08-27 | 2014-03-12 | 枣庄海帝新能源锂电科技有限公司 | Preparation method for high-purity lithium fluoride by taking lithium hexafluorophosphate as raw material |
| CN103626208B (en) * | 2012-08-27 | 2016-08-24 | 枣庄海帝新能源锂电科技有限公司 | A kind of high purity lithium fluoride preparation method of lithium hexafluoro phosphate raw material |
| 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 |
| CN106430251A (en) * | 2016-09-05 | 2017-02-22 | 中南大学 | Preparation method of micron superfine spherical sodium chloride |
| CN106430257A (en) * | 2016-10-09 | 2017-02-22 | 多氟多化工股份有限公司 | Preparation method of porous high-activity LiF and preparation method of LiFSI |
| CN119240752A (en) * | 2024-08-21 | 2025-01-03 | 江西云威新材料股份有限公司 | A method for preparing high-purity nano-scale lithium fluoride from industrial-grade lithium carbonate |
| CN119637911A (en) * | 2024-12-12 | 2025-03-18 | 湖北中誉新材料有限公司 | Method for preparing battery-grade lithium fluoride by solid-phase method |
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