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Method for preparing industrial sodium fluoride and industrial ammonium chloride by using mixed acid as lithium salt byproduct

A technology of industrial ammonium chloride and industrial sodium fluoride, which is applied in the direction of ammonium chloride, ammonium halide, alkali metal fluoride, etc., can solve the problems of environmental pollution, waste of resources, and environmental hidden dangers, and achieve non-polluting, environmental protection resource effect

Inactive Publication Date: 2017-06-20
刘放放
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) A large amount of calcium fluoride sludge is produced as a by-product, which cannot be effectively treated and has environmental hazards;
[0007] (2) By-product high-chlorine waste liquid is directly discharged to pollute the environment. If the evaporation process is used, the cost of treatment is high;
[0008] (3) Wastewater treatment costs are high and resources are wasted

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A method for preparing industrial sodium fluoride and industrial ammonium chloride by using lithium salt by-product mixed acid, comprising:

[0036] 1. Take 575g of lithium salt by-product mixed acid, control the temperature at 23°C; then start stirring at a speed of 85r / min, and slowly add 1000g of ammonia water with a mass concentration of 23% during the stirring process to control the reaction speed and prevent leakage; adjust the final State pH value is 6~6.5, obtains ammonium salt solution 1560g.

[0037] 2. Raise the temperature at the end of the reaction to 65°C, and continue to stir the reaction for 10 minutes; then slowly add 500g of saturated sodium chloride solution at a stirring speed of 80r / min, slow down the stirring speed to 65r / min, and continue adding Saturated brine 2000g.

[0038] 3. After the addition, continue stirring for 15 minutes and then filter to obtain 510g of sodium fluoride filter cake and 3420g of filtrate. At this time, the fluorine cont...

Embodiment 2

[0042] A method for preparing industrial sodium fluoride and industrial ammonium chloride by using lithium salt by-product mixed acid, comprising:

[0043] 1. Take 575g of lithium salt by-product mixed acid, control the temperature at 23°C; then start stirring at a speed of 85r / min, and slowly add 1010g of ammonia water with a mass concentration of 23% during the stirring process to control the reaction speed and prevent leakage; adjust the final State pH value is 6~6.5, obtains ammonium salt solution 1565g.

[0044] 2. Raise the temperature at the end of the reaction to 65°C, continue stirring for 10 minutes; then slowly add 500 g of saturated sodium chloride solution at a stirring speed of 80 r / min, slow down the stirring speed to 65 r / min and continue adding saturated brine 2000g.

[0045] 3. After the addition, continue to stir for 15 minutes and filter to obtain 518g of sodium fluoride filter cake and 3431g of filtrate. At this time, the fluorine content in the filtrate ...

Embodiment 3

[0049] A method for preparing industrial sodium fluoride and industrial ammonium chloride by using lithium salt by-product mixed acid, comprising:

[0050] 1. Take 575g of lithium salt by-product mixed acid, control the temperature at 23°C; then start stirring, and slowly add 1000g of ammonia water with a mass concentration of 23% at a speed of 85r / min to control the reaction speed and prevent leakage; adjust The final pH value was 6-6.5, and 1565 g of the ammonium salt solution was obtained.

[0051] 2. The temperature at the end of the reaction rises to 65°C, continue to stir for 10 minutes, then slowly add 500g of saturated sodium chloride solution at a stirring speed of 80r / min, slow down the stirring speed to 65r / min, and continue to add saturated Salt water 2000g.

[0052] 3. After the addition, continue stirring for 15 minutes and filter to obtain 513g of sodium fluoride filter cake and 3480g of filtrate. At this time, the fluorine content in the filtrate is 1.4%; then...

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Abstract

The invention belongs to the field of mixed acid treatment, and specifically relates to a method for preparing industrial sodium fluoride and industrial ammonium chloride by using mixed acid as a lithium salt byproduct. The method comprises the following steps: allowing a mixed acid to be dephosphorized and settled, reacting a supernatant with ammonia water at atmospheric pressure under mixing to obtain an ammonium fluoride and ammonium chloride mixed solution; adding a saturated sodium chloride solution to react under stirring to obtain sodium fluoride solid particles; filtering by a centrifuge after the reaction is finished, subjecting a filtrate to a precipitation reaction by adding calcium chloride to deeply remove fluoride to obtain an ammonium chloride and calcium chloride mixed solution, removing calcium by adding a sodium sulfate solution to obtain an ammonium chloride solution; and finally, subjecting the solution to evaporative crystallization to obtain an industrial ammonium chloride product. Through the method, the resource utilization of the waste acid as the lithium salt byproduct can be realized, the waste can be turned into treasure, no secondary waste is produced, and the environment cannot be polluted.

Description

technical field [0001] The invention belongs to the field of processing mixed acid, a by-product during the preparation of lithium hexafluorophosphate, and specifically relates to a method for preparing industrial sodium fluoride and industrial ammonium chloride by utilizing mixed acid produced by lithium salt. Background technique [0002] Lithium battery is a new type of clean energy, which has been widely used in mobile phones, laptop computers, and various working tools for human work. With the expansion of lithium battery application fields, as a main raw material in lithium battery production—— The output of lithium hexafluorophosphate is gradually increasing. According to statistics, the output of lithium hexafluorophosphate in 2015 was 13,500 tons. [0003] However, during the production of lithium hexafluorophosphate, a mixed acid (waste acid) will be produced by-product. The main components of the mixed acid are hydrofluoric acid (HF, mass concentration 15-35%) and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D3/02C01C1/16
CPCC01C1/164C01D3/02C01P2006/80
Inventor 刘松刘放放
Owner 刘放放