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Method for directly preparing battery-grade lithium hydroxide from lithium phosphate

A lithium hydroxide, battery-level technology, applied in the direction of lithium oxide;/hydroxide, etc., can solve the problems of low lithium conversion rate and low yield, and achieve the effect of improving yield

Active Publication Date: 2019-07-09
SHANGHAI CHINA LITHIUM INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the production of battery-grade lithium hydroxide usually adopts the process of industrial-grade lithium hydroxide or industrial-grade lithium hydroxide purification. This process is a traditional production method of battery-grade lithium hydroxide, but after many cycles of lithium hydroxide mother liquor, the mother liquor The calcium, magnesium, and sulfate ions in the solution are highly enriched and cannot continue to produce lithium hydroxide. It is necessary to precipitate the lithium ions in the solution with phosphoric acid, resulting in low conversion rate and low yield of lithium.

Method used

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  • Method for directly preparing battery-grade lithium hydroxide from lithium phosphate
  • Method for directly preparing battery-grade lithium hydroxide from lithium phosphate
  • Method for directly preparing battery-grade lithium hydroxide from lithium phosphate

Examples

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Effect test

Embodiment 1

[0021] Lithium phosphate used in this example is a dry material, and the content of main impurities such as sodium, potassium, calcium, magnesium, and sulfate radicals is 1-20ppm; sulfuric acid is 98%; barium hydroxide content is 99%.

[0022] (1) Weigh 1000g of lithium phosphate wet material into a 2L beaker, add 1L of pure water, then add 740g of 98% concentrated sulfuric acid until the lithium phosphate wet material is completely dissolved, then add a theoretical amount of 120% of lithium oxalate to precipitate Calcium ions, filtered for later use;

[0023] (2), the filtered solution was evaporated to 155°C in a beaker, and when cooled to 30°C, a large amount of lithium sulfate crystals were precipitated; 1810g of solids were obtained after suction filtration;

[0024] (3), put the lithium sulfate solid of 1810g in poly 3L beaker, add again 1800g pure water, the pH of solution is 3-4, add industrial grade lithium hydroxide 12g to adjust the pH of solution to 7.5, there is ...

Embodiment 2

[0036] The lithium phosphate wet material content used in this example is 85%, and the content of main impurity such as sodium, potassium, calcium, magnesium, sulfate radical is 1-20ppm; Sulfuric acid is 98%; Barium hydroxide content is 99%.

[0037] (1) Weigh 5000g of lithium phosphate wet material into a 5L PTFE beaker, add 4L of pure water, then add 3550g of 98% concentrated sulfuric acid until the lithium phosphate wet material is completely dissolved, then add a theoretical amount of 120% oxalic acid Lithium precipitated calcium ions, filtered for later use;

[0038] (2), the filtered solution is evaporated to 155°C in a beaker, and when cooled to 30°C, a large amount of lithium sulfate crystals are separated out, and 5220g of solid is obtained after separation with a small centrifuge;

[0039] (3), put the lithium sulfate solid of 5220g in poly 2L beaker, add again 5000g pure water, the pH of solution is 3-4, add industrial grade lithium hydroxide 32g to adjust the pH of...

Embodiment 3

[0051] The raw material that this example adopts is identical with example 1, but enlarges input amount

[0052] The lithium phosphate wet material content used in this example is 85%, and the content of main impurity such as sodium, potassium, calcium, magnesium is 1-20ppm; Sulfuric acid is 98%; Barium hydroxide content is 99%.

[0053] (1), weigh 2000kg of lithium phosphate wet material in 3M 3 Add 3000L of pure water and 1620kg of 98% concentrated sulfuric acid until the lithium phosphate is completely dissolved, then add a theoretical amount of 120% of lithium oxalate to precipitate calcium ions, filter until clarified and set aside;

[0054] (2), the filtered solution is evaporated to 155°C in a beaker, and when cooled to 30°C, a large amount of lithium sulfate crystals are separated out; 2713kg of solid is obtained after separation with a centrifuge;

[0055] (3), put 2713kg of lithium sulfate wet material in 3M 3 Add 2000kg of pure water to the enamel reaction kettle an...

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Abstract

The invention discloses a method for directly preparing battery-grade lithium hydroxide from lithium phosphate. The method comprises the following steps: dissolving lithium phosphate by sulfuric acid,removing impurities, then transferring the dissolved lithium salt into a stirring enamel reaction kettle for evaporation and concentration, and carrying out cooling to obtain a lithium sulfate crudeproduct; adding pure water into the enamel reaction kettle to dissolve the lithium sulfate crude product, carrying out heating to 85-95 DEG C for later use, then adding lithium hydroxide or metal lithium, adjusting the pH value of the solution to 7.5, and then carrying out evaporating, concentrating and cooling to obtain lithium sulfate monohydrate; precipitating the lithium sulfate monohydrate byusing a barium hydroxide solution to form lithium hydroxide, and then carrying out washing to obtain a battery-grade lithium hydroxide wet material; and carrying out drying and crushing to obtain thebattery-grade lithium hydroxide. According to the method disclosed by the invention, the current situation that after a lithium hydroxide mother liquor is circulated for multiple times, ions such ascalcium, magnesium, sulfate and the like in the mother liquor is highly enriched and production of lithium hydroxide cannot be continued can be avoided, and the yield of the product (battery-grade lithium hydroxide) can be effectively improved.

Description

technical field [0001] The invention belongs to the field of lithium hydroxide preparation, in particular to a method for directly preparing battery-grade lithium hydroxide from lithium phosphate. Background technique [0002] At present, the production of battery-grade lithium hydroxide usually adopts the process of industrial-grade lithium hydroxide or industrial-grade lithium hydroxide purification. This process is a traditional production method of battery-grade lithium hydroxide, but after many cycles of lithium hydroxide mother liquor, the mother liquor The calcium, magnesium, sulfate radicals and other ions in the solution are highly enriched, and lithium hydroxide cannot be continued to be produced. It is necessary to precipitate the lithium ions in the solution with phosphoric acid, resulting in low conversion rate and low yield of lithium. Contents of the invention [0003] In order to overcome the above-mentioned defects of the prior art, the present invention p...

Claims

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Application Information

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IPC IPC(8): C01D15/02
CPCC01D15/02C01P2006/80
Inventor 魏述彬程涛顾金峰员江平贾硕高清华
Owner SHANGHAI CHINA LITHIUM INDAL
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