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A kind of preparation method of high-purity lithium fluoride

A lithium fluoride, high-purity technology, applied in the field of preparation of high-purity lithium fluoride, can solve the problems of lack of lithium fluoride and inaccurate recovery process of harmful gases, so as to reduce the emission of harmful gases, improve the accuracy, and improve the process flow. The effect of green environmental protection

Active Publication Date: 2019-02-01
四川沃耐稀新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method and device for high-purity lithium fluoride, to solve the problems of lack of harmful gas recovery and imprecise process in the current preparation process of lithium fluoride

Method used

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  • A kind of preparation method of high-purity lithium fluoride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A preparation method for high-purity lithium fluoride, comprising the following steps:

[0031] S1: Dissolve elemental lithium metal at a ratio of 1:100 in deionized water at a temperature of 2°C. During the dissolving process after placing lithium metal in deionized water, seal the gas collection hood of the gas collection device to the container. On the deionized water container, turn on the vacuum pump on the gas collection device, and pump the generated hydrogen into the gas collection bag connected to the vacuum pump;

[0032] S2: After the metal lithium is completely dissolved, slowly add a hydrofluoric acid solution with a concentration of 99% to the solution and stir to make the lithium fluoride precipitate slowly, and place a pH value detection device in the solution;

[0033] S3: When the pH of the solution is less than 7 and lithium fluoride is no longer precipitated in the solution, stop adding the hydrofluoric acid solution and let stand for 0.5h;

[0034]...

Embodiment 2

[0038] A preparation method for high-purity lithium fluoride, comprising the following steps:

[0039] S1: Dissolve elemental lithium metal in deionized water at a temperature of 5°C at a ratio of 1:100. During the dissolution process after placing lithium metal in deionized water, seal the gas collection hood of the gas collection device to the container. On the deionized water container, turn on the vacuum pump on the gas collection device, and pump the generated hydrogen into the gas collection bag connected to the vacuum pump;

[0040] S2: After the metal lithium is completely dissolved, slowly add a hydrofluoric acid solution with a concentration of 99% to the solution and stir to make the lithium fluoride precipitate slowly, and place a pH value detection device in the solution;

[0041] S3: When the pH of the solution is less than 7 and lithium fluoride is no longer precipitated in the solution, stop adding the hydrofluoric acid solution and let stand for 0.5h;

[0042...

Embodiment 3

[0046] The purity verification experiment of lithium fluoride:

[0047] Experimental method: number the lithium fluoride prepared in Example 1 and Example 2 as A and B; C is a high-purity lithium fluoride sample produced by a traditional lithium fluoride production process. Use the electrode method to detect and analyze the composition of lithium fluoride in A, B and C.

[0048] The experimental results are shown in Table 1:

[0049] Table 1 Lithium fluoride sample composition

[0050] Test sample

[0051] Analysis of experimental results: the purity of lithium fluoride prepared by the preparation method of the present invention is 99.41% and 99.58%, respectively. While the purity of lithium fluoride produced by the traditional lithium fluoride production process is 99.12%, it can be seen that the purity of lithium fluoride produced by the preparation method of the present invention is higher.

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Abstract

The invention belongs to the field of preparation of chemical industrial products, and particularly relates to a preparation method of high-purity lithium fluoride. The preparation method of high-purity lithium fluoride includes steps of S1, dissolving simple lithium metal in deionized water, and collecting the generated hydrogen by a gas collecting device; S2, slowly adding hydrofluoric acid solution with concentration of 99% in solution and stirring the solution; S3, when the pH value of solution is less than 7, and no lithium fluoride sediment is separated out from the solution, stopping adding hydrofluoric acid solution and statically keeping for 0.5 hour; S4, centrifuging the static solution in a freeze centrifugal machine, taking the sediment and washing the obtained sediment by the deionized water; S5, repeating the step S4 for 2-3 times; S6, settling the separated and washed lithium fluoride in a desulfuration tower to heat and dry for 1-3 hours; cooling the lithium fluoride after heating and drying so as to obtain the high-purity lithium fluoride. The preparation method has the functions of desulfuration and waste gas recycling; the method enhances the technical preparation precision while reduces the emission of harmful gas during the preparation process; besides, the technical flow is more green and environment-friendly.

Description

technical field [0001] The invention relates to the field of chemical product preparation, in particular to a method for preparing high-purity lithium fluoride. Background technique [0002] Lithium fluoride (LiF) is an inorganic reagent with the appearance of white powder or cubic crystal. As an important lithium-based basic material, lithium fluoride has been widely used in many fields. With the increasing demand for high-purity lithium fluoride traditional application fields and the continuous emergence of some new application fields such as optical fiber communication, high-energy chemical power supply, aerospace, etc., the research and preparation of high-purity lithium fluoride is becoming more and more attractive . [0003] The reported preparation methods of high-purity lithium fluoride mainly include direct preparation method, ion exchange preparation method, extraction preparation method and so on. Most of these disclosed methods need to prepare high-purity lithi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D15/04C01B3/08
CPCY02E60/36
Inventor 杨青
Owner 四川沃耐稀新材料科技有限公司
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