Method for preparing high purity lithium fluoride

A high-purity lithium fluoride and lithium fluoride technology, applied in the direction of lithium halide, etc., can solve the problems of reducing LiF production cost, insufficient pretreatment, and high content of transition metal impurity elements

Inactive Publication Date: 2009-06-24
NORTHWEST RES INST OF MINING & METALLURGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The ion exchange preparation method makes full use of the by-product Na of the phosphate fertilizer plant 2 SiF 6 , which effectively reduces the production cost of LiF, its main disadvantage is that the content of silicon and some transition metal impurity elements in the prepared high-purity LiF is still high, the reason may be that the Na 2 SiF 6 Insufficient pretreatment, so that the high-purity LiF prepared by this method is not suitable for fields sensitive to these impurity ions

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  • Method for preparing high purity lithium fluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1, a kind of method for preparing high-purity lithium fluoride has the following steps:

[0029] (1) The preparation of lithium hexafluorophosphate by solvent method is usually based on excess LiF and PCl 5 As a raw material, lithium hexafluorophosphate is directly synthesized by metathesis reaction, and the reaction is as follows:

[0030]

[0031] In order to ensure the completeness of the reaction, an excess of 0.1-2 mol of lithium fluoride is usually required in the actual preparation. After the reaction is completed and the obtained lithium hexafluorophosphate is separated and purified, a large amount of mixed by-products of lithium fluoride and lithium chloride will be obtained at the same time.

[0032] (2) drop the mixture of lithium fluoride and lithium chloride into deionized water, stir the solution to fully dissolve the mixture,

[0033] And made into a slightly acidic aqueous solution with a pH value of 0.1 to 7;

[0034] (3) In the state of...

Embodiment 2

[0036] Embodiment 2, a kind of method for preparing high-purity lithium fluoride has the following steps:

[0037] (1) Lithium chloride is obtained after acidifying lithium hydroxide by hydrochloric acid.

[0038]

[0039] (2) drop lithium chloride into deionized water, stir the solution to fully dissolve the mixture, and make a slightly acidic aqueous solution with a pH value of 0.1 to 7;

[0040] (3) In the state of stirring, quickly drop the solution of saturated ammonium bifluoride (no ratio and no temperature requirement) in the aqueous solution described in the above steps to obtain lithium fluoride precipitation; continue to stir for 0.5-1h, and stand still for 1-2h;

[0041] (4) Step 4 is the same as step (4) of Embodiment 1.

Embodiment 3

[0042] Embodiment 3, a kind of method for preparing high-purity lithium fluoride has the following steps:

[0043](1) Lithium acetate is obtained after lithium carbonate is acidified by acetic acid:

[0044]

[0045] (2) Lithium acetate is dropped into deionized water, the solution is stirred to fully dissolve the mixture, and it is made into an acidic aqueous solution with a pH value of 0.1 to 7;

[0046] (3) In the state of stirring, quickly drop saturated ammonia and hydrogen fluoride two elemental solutions (no ratio and no temperature requirement) into the aqueous solution described in the above steps to obtain lithium fluoride precipitation; continue stirring for 0.5-1h, Stand still for 1-2h;

[0047] Step 4 is the same as step (4) of Embodiment 1.

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Abstract

The invention in particular relates to a method for preparing lithium fluoride. The method for preparing the high-purity lithium fluoride is mainly characterized by comprising the following steps: (1) putting a mixture of the lithium fluoride and lithium chloride or the lithium chloride or lithium acetate in deionized water and stirring the solution so as to make the mixture sufficiently dissolve and prepare a meta acid aqueous solution of which the pH value is between 0.1 and 7; (2) under a stirring state, quickly dropping a solution of two simple substances of saturated ammonium fluoride or ammonium hydrogen fluoride or ammonia and fluorine hydride in the aqueous solution of the step (1) so as to obtain lithium fluoride precipitates, and continuing to stir for 0.5 to 1 hour and standing for 1 to 2 hours; and (3) through the step (1) and the step (2), finishing forming the lithium fluoride into the precipitates which are not dissolved in the water, filtering and drying the lithium fluoride precipitates and washing the precipitates for 3 to 5 times, and drying the obtained lithium fluoride in vacuum for 1 to 2 hours at a temperature of between 100 and 200 DEG C. The method has the advantages that the purities of the prepared lithium fluoride meet the following requirements: the purity of lithium fluoride (LiF) is more than or equal to 99.99 percent; the purity of silicon dioxide (SiO2) is less than or equal to 4ppm; the purity of heavy metal is less than or equal to that of iron of which the purity is less than or equal to 1 ppm; and the purity of the total weight of other metals (metered by Ca, Mg and Al) is less than or equal to 1 ppm.

Description

Technical field: [0001] The present invention specifically relates to a method for preparing lithium fluoride. Background technique: [0002] With the increasing demand for high-purity lithium fluoride in traditional application fields and the continuous emergence of some new application fields (such as applying it to the raw materials for the synthesis of lithium hexafluorophosphate, long-distance communication optical fiber materials, etc.), the preparation of high-purity lithium fluoride is becoming more and more important. People have paid more and more attention to it. In the late 1980s, reports on the preparation technology of high-purity lithium fluoride began to appear internationally. The methods introduced successively include direct preparation, ion exchange preparation, and extraction preparation. [0003] The direct preparation method is the main method for the early preparation of high-purity LiF, and the raw material is generally solid Li 2 CO 3 with hydrofl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/04
Inventor 王永斌杨进忠雷思维周涛符嵩涛顾晓玲
Owner NORTHWEST RES INST OF MINING & METALLURGY INST
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