Method for producing anhydrous lithium chloride special for electrolyzing by using lithium recovered from lithium-containing pharmaceutical waste water

A pharmaceutical wastewater and lithium chloride technology, applied in the direction of lithium halide, etc., can solve the problems of low product purity, no sodium removal, and poor product appearance, and achieve the effects of avoiding environmental pollution, avoiding waste of resources, and less investment in equipment

A pharmaceutical wastewater and lithium chloride technology, applied in the direction of lithium halide, etc., can solve the problems of low product purity, no sodium removal, and poor product appearance, and achieve the effects of avoiding environmental pollution, avoiding waste of resources, and less investment in equipment

CN102874849AActive Publication Date: 2013-01-16FENGXIN GANFENG LITHIUM
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  • Method for producing anhydrous lithium chloride special for electrolyzing by using lithium recovered from lithium-containing pharmaceutical waste water
  • Method for producing anhydrous lithium chloride special for electrolyzing by using lithium recovered from lithium-containing pharmaceutical waste water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] a. Ingredients removal: mix 7.6m 3 Lithium-containing pharmaceutical wastewater (contained Ca by analysis 2+ % is 0.02%, SO4 2- % is 0.07%, namely Ca 2+ The mass percentage content is 0.02%, SO4 2- The mass percentage content is 0.07%, at this time the solution density is 1070Kg / m 3 ) into the batching kettle, adjust the pH of the solution to 12 with lithium hydroxide solution, stir and react for 30 minutes, and precipitate the Mg in the waste liquid 2+ , Fe 3+ Plasma, then add 12.3Kg of BaCl 2 Stir and react with 5.0Kg ammonium oxalate for 30 minutes to remove Ca in the solution 2+ and SO 4 2- , remove the solid precipitate by pressure filtration;

[0039] b, initial organic removal: add hydrochloric acid to the filtrate obtained in step a, adjust the pH value of the solution to 8, add 8.1Kg powdered activated carbon, heat up and control it at 80°C, stir for 90 minutes, and obtain a clear solution after press filtration;

[0040] c, micro-electrolysis deep or...

Embodiment 2

[0047] a. Ingredients removal: mix 7.5m 3 Lithium-containing waste liquid (contains Ca after analysis 2+ % is 0.03%, SO4 2- % is 0.1%, then the density of the solution is 1090Kg / m 3 ) into the batching kettle, adjust the pH of the solution to 11 with lithium hydroxide solution, stir and react for 15 minutes, and precipitate the Mg in the waste liquid 2+ , Fe 3+ Plasma, then add 17.7Kg BaCl 2 Stir and react with 7.6Kg ammonium oxalate for 15 minutes to remove Ca in the solution 2+ and SO 4 2- , remove the solid precipitate by pressure filtration;

[0048] b. Initial organic removal: add hydrochloric acid to the filtrate obtained in step a, adjust the pH value of the solution to 7, add 8.2Kg powdered activated carbon, heat up and control it at 50°C, stir for 40 minutes, and obtain a clear solution after press filtration;

[0049] c, micro-electrolysis deep organic removal: pass through the solution of step b to remove organics through the micro-electrolysis organic devic...

Embodiment 3

[0056] a. Ingredients removal: mix 7.5m 3 Lithium-containing pharmaceutical wastewater (contained Ca by analysis 2+ % is 0.04%, SO42- % is 0.13%, and the density of the solution at this time is 1080Kg / m 3 ) into the batching kettle, adjust the pH of the solution to 10.5 with lithium hydroxide solution, react for 25 minutes, and precipitate the Mg in the wastewater 2+ , Fe 3+ Plasma, then add 22.8Kg BaCl 2 React with 10Kg ammonium oxalate for 25 minutes to remove Ca in wastewater 2+ and SO 4 2- , remove the solid precipitate by pressure filtration;

[0057] b, initial organic removal: add hydrochloric acid to the filtrate obtained in step a, adjust the pH value of the solution to 7.5, add 8.1Kg powdered activated carbon, heat up and control it at 65°C, stir for 65 minutes, and obtain a clear solution after press filtration;

[0058] c, micro-electrolysis deep organic removal: pass through the solution of step b to remove organics through the micro-electrolysis organic de...

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Abstract

The invention discloses a method for producing anhydrous lithium chloride special for electrolyzing lithium by using lithium recovered from lithium-containing pharmaceutical waste water. The method comprises the following steps of: (a) preparing materials and removing impurities; (b) initially removing organic matters; (c) performing microelectrolysis and deeply removing the organic matters; (d) concentrating to separate sodium out; (e) evaporating and crystallizing; (f) performing centrifugal separation; (g) drying; and (h) cooling and packaging. By the method, the anhydrous lithium chloride special for producing and electrolyzing the lithium can be directly obtained by using the lithium recovered from the lithium-containing pharmaceutical waste water, so that the product impurity is more than 99 percent, the content of the sodium is less than 0.25 percent, and the whiteness of the products is high.

Description

technical field [0001] The invention relates to a preparation method of special anhydrous lithium chloride for electrolysis, in particular to a method for producing special anhydrous lithium chloride for electrolysis by recovering lithium from lithium-containing pharmaceutical wastewater. Background technique [0002] At present, many manufacturers of pharmaceutical intermediates use metal lithium, butyllithium or other organic lithium compounds as catalysts for the reaction of pharmaceutical intermediates. After completion, the lithium-containing catalyst components that have not been fully recycled are discharged into the pharmaceutical wastewater treatment system. In addition to lithium chloride, the pharmaceutical wastewater also contains residual organic substances such as ethyl trichloroacetate, diisopropylamine, tetrahydrofuran, and sodium salts. , Calcium salt, sulfate and other impurities, if the pharmaceutical wastewater is directly discharged, it will cause seriou...

Claims

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Application Information

Patent Timeline
16 Jan 2013
Publication
CN102874849A
IPC
C01D15/04
Inventors
李良彬; 熊训满