Apparatus and method for preparing high-purity lithium fluoride

A high-purity lithium fluoride and grinding device technology, applied in chemical instruments and methods, lithium halides, feeding devices, etc., can solve problems such as not considering the corrosion requirements of hydrofluoric acid, and achieve the effect of avoiding corrosion and high purity

Pending Publication Date: 2019-09-03
GUIZHOU INST OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the patent "A Synthetic Reactor for Granular Lithium Fluoride", although a three-stage stirring method is adopted, the lithium carbonate wrapped on the surface by lithium fluoride cannot be completely exposed, which is a major difficulty in the industry; In addition, in the above-mentioned patents, hydrofluoric acid does not take into account the high corrosion requirements of equipment, and does not describe the problems caused by the large amount of mixed gas of hydrogen fluoride and carbon dioxide released during the reaction process.

Method used

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  • Apparatus and method for preparing high-purity lithium fluoride
  • Apparatus and method for preparing high-purity lithium fluoride

Examples

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Comparison scheme
Effect test

Embodiment 1

[0023] figure 1 and figure 2 A device for preparing high-purity lithium fluoride according to an embodiment of the present invention is schematically shown.

[0024] refer to figure 1 and figure 2 , a device for preparing high-purity lithium fluoride Reactor 1, condensation reflux device 2, grinding device 3, tail gas absorption device 4, first corrosion-resistant pump 5, second corrosion-resistant pump 6, first return pipe 7, the second Two return pipes 8, motors 9 and stirring paddles 10.

[0025] The reaction kettle 1 is made of stainless steel, and the reaction kettle 1 is lined with polytetrafluoroethylene, which can effectively prevent hydrofluoric acid corrosion. The reaction kettle 1 is provided with a solid feed port 11, a liquid feed port 16, a discharge port 12, a condensation return port 13 and a mixed slurry return port 14, and the feed port includes a solid feed port 11 and a liquid feed port 16, The solid feed port 11 , the liquid feed port 16 , the conde...

Embodiment 2

[0033] The present invention also provides a method for preparing high-purity lithium fluoride, comprising the steps of:

[0034] 1) Lithium carbonate solid particles and hydrofluoric acid liquid are mixed in reactor 1, violent reaction takes place under the stirring of paddle 10 and has generated lithium fluoride-hydrofluoric acid-lithium carbonate mixed slurry and carbon dioxide gas;

[0035] The chemical reaction equation of this reaction is: Li 2 CO 3 +2HF=2LiF↓+CO 2 ↑+H 2 O.

[0036]Due to the violent reaction, hydrogen fluoride gas will be volatilized in the hydrofluoric acid liquid raw material, and the hydrogen fluoride gas will mix with the carbon dioxide gas generated by the reaction and overflow together.

[0037] The lithium fluoride produced by the reaction will be wrapped on the surface of lithium carbonate crystal, hindering the further reaction of lithium carbonate and hydrofluoric acid. Therefore, in the prior art, this reaction process usually cannot mak...

Embodiment 3

[0046] Weigh 100g of lithium carbonate dried to constant weight for later use, connect the pipeline of the device, open the condensation reflux device 2 (condensation medium is absolute ethanol, temperature -30°C), weigh 56.87g of anhydrous hydrogen fluoride (5% excess) and place in In the reaction kettle 1, the sodium carbonate weighed was slowly added into the reaction kettle, and the first corrosion-resistant pump 5, the second corrosion-resistant pump 6 and the grinding device 3 were started after stirring and reacting for 10 minutes, and the reaction was further carried out for 30 minutes to obtain lithium fluoride- The hydrofluoric acid mixed slurry was filtered, the filter residue was washed to PH~7, and 68.12g of lithium fluoride product was obtained after drying. The conversion rate of lithium carbonate was 97.0%, while the conversion rate of lithium carbonate by conventional stirring reaction was only 70%. %about. According to HG / T 4507-2013 "High Purity Industrial L...

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Abstract

The invention discloses an apparatus for preparing high-purity lithium fluoride, wherein the apparatus comprises a reaction kettle, a condensation reflux device, a grinding device and a tail gas absorption device. The invention further provides a method for preparing high-purity lithium fluoride, wherein the method comprises: 1) carrying out a mixing reaction on lithium carbonate solid particles and a hydrofluoric acid liquid in a reaction kettle to form a lithium fluoride-hydrofluoric acid-lithium carbonate mixed slurry, hydrogen fluoride and carbon dioxide gas; 2) conveying the lithium fluoride-hydrofluoric acid-lithium carbonate mixed slurry to a grinding device, and grinding; and 3) conveying the grinded mixed slurry to the reaction kettle, continuously carrying out a reaction, makingthe hydrogen fluoride and the carbon dioxide gas generated by the reaction enter a condensation reflux device, and carrying out condensation reflux on the hydrogen fluoride. According to the present invention, with the apparatus and the method, the reaction process can be completely carried out, the problem of separation of carbon dioxide from hydrogen fluoride in the tail gas of the lithium fluoride synthesis process is solved, no other elemental impurities are introduced during the reaction, and the obtained lithium fluoride has high purity.

Description

technical field [0001] The invention relates to the field of inorganic fine chemicals, in particular to a device and method for preparing high-purity lithium fluoride. Background technique [0002] Lithium fluoride is an important inorganic fluoride, which is widely used in enamel, glass, ceramics, communication optical fiber, lithium battery and other fields. At present, there are four main types of preparation technologies for high-purity lithium fluoride reported at home and abroad, namely direct synthesis, metathesis preparation, extraction and ion exchange. The direct synthesis method directly reacts lithium carbonate and hydrofluoric acid to obtain lithium fluoride. Although the principle of this method is simple and no other impurity elements are introduced, during the reaction process, the corrosion resistance of the equipment is required to be high, the reaction is violent, and the hydrogen fluoride and carbon dioxide produced overflow together and cannot be separa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/18B01J4/00B01J19/00C01D15/04
CPCB01J4/008B01J19/0006B01J19/0013B01J19/0053B01J19/1862B01J2204/007C01D15/04C01P2006/80
Inventor 张建刚陈学航肖超王晓雄苏向东
Owner GUIZHOU INST OF TECH
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