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Lithium tetrafluoroborate preparation method

A technology of lithium tetrafluoroborate and lithium metaborate, which is applied in the direction of tetrafluoroboric acid, borates, boron oxides, etc., can solve the problems of high equipment requirements, long production cycle, and easy corrosion of equipment, so as to achieve easy availability of raw materials, The effect of high product quality and non-toxic raw materials

Active Publication Date: 2015-02-04
SHANGHAI CHINA LITHIUM INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the first method, hydrofluoric acid and boric acid are used to neutralize first to generate fluoboric acid, and then neutralized with lithium hydroxide, the production cycle is long, the requirements for equipment are high, and the equipment is easy to corrode
Method 2 has a short reaction period, but boron trifluoride diethyl ether is a flammable and explosive substance with a low production safety factor. It needs to be produced under high vacuum conditions, and the remaining waste liquid of the reaction contains diethyl ether, unreacted raw materials and dissolved Lithium tetrafluoroborate is not easy to recycle and causes great environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Lithium carbonate raw material in the example is battery grade, and content is 99.9%, and impurity is mainly as sodium, potassium, calcium, magnesium, sulfate radical, and content is 1~10ppm, and boric acid, ammonium fluoride are analytically pure, and impurity is mainly such as Sodium, potassium, calcium, magnesium, and sulfate, the content is 5-20ppm.

[0023] (1) Weigh 650g of analytically pure boric acid into a PTFE beaker, then add 422g of battery-grade lithium carbonate with a purity of 99.9%, and mix thoroughly;

[0024] (2) Transfer the PTFE beaker to a muffle furnace at 200°C and burn for 12 hours to obtain a white foamy solid;

[0025] (3) After the white foamy solid was cooled to room temperature, it was pulverized to obtain a white powder lithium metaborate with a weight of 495.2 g and a yield of 99.04%. The quality analysis results were as follows:

[0026] (4) Put 495.2g of lithium metaborate powder in (3) into a 2L tetrafluorobeaker, add 1500g of analyti...

Embodiment 2

[0030] Lithium hydroxide monohydrate in the example is battery grade, with a content of 56.5%. The impurities are mainly sodium, potassium, calcium, magnesium, and sulfate, with a content of 1-10ppm. Boron oxide and ammonium hydrogen fluoride are analytically pure, and the impurities are mainly It is sodium, potassium, calcium, magnesium, and sulfate, with a content of 5-20ppm.

[0031] (1) Weigh 1000g of battery-grade lithium hydroxide monohydrate into a PTFE beaker, add 850g of analytically pure boron oxide, and fully stir and mix the two raw materials;

[0032] (2) Transfer the uniformly mixed raw materials to a muffle furnace at 200°C and burn for 12 hours to obtain a white foamy solid. Pulverize the white foamy solid to obtain lithium metaborate powder, weighing 590.1g, yield 99.54%;

[0033] (3) Add 590g of lithium metaborate powder from (2) into a 2L PTFE beaker, add 1360g of analytically pure ammonium bifluoride, fully stir the two raw materials, and mix them evenly; ...

Embodiment 3

[0037] The purity of lithium carbonate used in the examples is battery grade, with a content of 99.95%. The impurities are mainly sodium, potassium, calcium, magnesium, and sulfate radicals, with a content of 1 to 10 ppm. Both boron oxide and ammonium fluoride are analytically pure, and the impurities are mainly It is sodium, potassium, calcium, magnesium, and sulfate, with a content of 10-50ppm.

[0038] (1) Weigh 370g of analytically pure boron oxide into a beaker, then add 362g of battery-grade lithium carbonate with a purity of 99.95%, mix well and transfer to a PTFE beaker;

[0039] (2) Transfer the PTFE beaker to a muffle furnace, control the temperature at 200°C, react for 12 hours, and press at normal pressure. After the reaction, a white foamy solid is obtained. After crushing, a white powdery solid is obtained. Weight is 465.4g;

[0040] (3) Transfer 465g of lithium metaborate obtained in (2) to a 2L PTFE beaker, add 1400g of analytically pure ammonium fluoride, and...

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PUM

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Abstract

The invention discloses a lithium tetrafluoroborate preparation method comprising the following steps: mixing lithium carbonate, lithium hydroxide monohydrate or anhydrous lithium hydroxide and boric acid and boric oxide to obtain lithium metaborate, crushing the lithium metaborate to obtain lithium metaborate powder, and mixing the lithium metaborate powder and ammonium fluoride or ammonium bifluoride for vacuum negative pressure burning reaction to obtain the lithium tetrafluoroborate product. The lithium tetrafluoroborate preparation method uses a solid lithium source and a solid boron source as raw materials for preparation of the lithium tetrafluoroborate, the process has the advantages that raw materials are easily obtained, non-toxic and non-corrosive, product quality is high, no side reaction is produced, and the method is environmentally friendly and high in efficiency, and the like.

Description

technical field [0001] The patent of the present invention relates to a new process for preparing lithium tetrafluoroborate. Background technique [0002] Lithium tetrafluoroborate is mainly used in lithium battery electrolyte and pharmaceutical chemical industry. The preparation of lithium tetrafluoroborate has the following methods. The first method is to neutralize with hydrofluoric acid, lithium hydroxide, boric acid, concentrate, crystallize, and dry to obtain lithium tetrafluoroborate dihydrate, and then dihydrate tetrafluoroborate dihydrate Lithium borate is dehydrated under vacuum to obtain lithium tetrafluoroborate. The second method is to use boron trifluoride ether and lithium fluoride to carry out complexation reaction in an organic medium, and then undergo steps such as vacuum drying to obtain lithium tetrafluoroborate. In the first method, hydrofluoric acid and boric acid are used to neutralize to generate fluoroboric acid, and then neutralized with lithium h...

Claims

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Application Information

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IPC IPC(8): C01B35/12
CPCC01B35/066
Inventor 米泽华
Owner SHANGHAI CHINA LITHIUM INDAL
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