IP Library › Granted Patent US 10,662,504
Granted Patent B2
US 10,662,504 · App. 16/261,156 · Granted May 26, 2020

Method for recovering lithium from low-context extraction tailwater and recycling extraction tailwater

Inventors: Xunbing Liu (Yiyang, CN); Jianjun Ouyang (Yiyang, CN); Xijuan Liu (Yiyang, CN)
C22B26/12C01D5/00C01D5/02C01D15/08C01F11/22C02F1/58C22B3/0005C22B3/22C22B3/44H01M10/052H01M10/54Y02P10/234
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Quick Facts
Patent No.
US 10,662,504
App. No.
16/261,156
Granted
May 26, 2020
Kind
B2
Abstract

A method for recovering lithium from low-content extraction tailwater and recycling extraction tailwater is provided. The disclosure is characterized that recovery of lithium from lithium-containing extraction tailwater is achieved by adding calcium to remove fluorine, carrying out evaporative crystallization and precipitating lithium salts. Recycle of extraction tailwater is achieved by adopting the following steps: in the lithium-containing extraction tailwater, adding calcium to remove fluorine, carrying out evaporative crystallization, recovering condensate water, precipitating a lithium salt and recycling mother liquor. According to the disclosure, lithium is recovered from low-content extraction tailwater via enrichment and sodium sulfate and distilled water therein are incidentally recovered, so that zero release of battery waste treatment wastewater is achieved.

Claims (30)

1. A method for recovering lithium from low-content extraction tailwater, comprising:

adding calcium into a first extraction tailwater which is lithium-containing to remove fluorine to obtain a second extraction tailwater;

carrying out evaporative crystallization on the second extraction tailwater to obtain a third extraction tailwater;

precipitating lithium salts from the third extraction tailwater to obtain a fourth extraction tailwater which is non-lithium containing; and

recycling the fourth extraction tailwater.

2. The method for recovering lithium from low-content extraction tailwater according to claim 1 , comprising the following steps:

adding calcium to remove fluorine in the first extraction tailwater which is lithium-containing to obtain the second extraction tailwater;

carrying out evaporative crystallization on the second extraction tailwater to obtain the third extraction tailwater;

recovering condensate water;

precipitating the lithium salts from the third extraction tailwater to obtain the fourth extraction tailwater; and

recycling the fourth extraction tailwater.

3. The method for recovering lithium from low-content extraction tailwater-according to claim 1 , wherein, after evaporative crystallization, removing impurities from the third extraction tailwater.

4. The method for recovering lithium from low-content extraction tailwater according to claim 1 , wherein, the step of adding calcium to remove fluorine comprises the following steps:

adding sodium hydroxide to the first extraction tailwater in which cobalt, nickel and manganese is extracted to regulate a pH value to 8-13;

adding a calcium-containing material so that a F/Ca ion mole is 1/(1-5);

reacting for 0.5-4 h;

filtering and washing, wherein filtrate is evaporation stock solution.

5. The method for recovering lithium from low-content extraction tailwater according to claim 1 , wherein, the evaporative crystallization is realized by the following steps:

concentrating the second extraction tailwater-to 1/(4-16) by evaporating the second extraction tailwater and crystallizing sodium sulfate in the second extraction tailwater so that a content of lithium in third extraction tailwater reaches 5-30 g/L, and

recovering the condensate water.

6. The method for recovering lithium from low-content extraction tailwater according to claim 3 , wherein, the step of removing impurities comprises the following steps:

regulating the pH value of the third extraction tailwater to 11-14 with alkali to remove impurities including calcium and magnesium.

7. The method for recovering lithium from low-content extraction tailwater according to claim 1 , wherein, the step of precipitating the lithium salts comprises the following steps:

preparing a saturated carbonate solution with the condensate water;

heating the third extraction tailwater;

adding the saturated carbonate solution to the third extraction tailwater which is heated so that a lithium ion is precipitated as lithium carbonate for recovery.

8. The method for recovering lithium from low-content extraction tailwater according to claim 2 , wherein, the step of recycling the fourth extraction tailwater comprises the following steps:

regulating the pH value of the fourth extraction tailwater to 2.5-6 to remove carbonate radicals therein, and

returning the fourth extraction tailwater back to an evaporation stock solution tank.

9. The method for recovering lithium from low-content extraction tailwater-according to claim 8 , wherein, the pH value of the fourth extraction tailwater is regulated to 3.0-5.5 with acid.

Priority Claims (1)
CN 2016 1 0928469 · Oct 31, 2016 · national
Continuity (2)
Continuation PCTCN2017103692 · Sep 27, 2017
Related Publication 20190153563A1 · May 23, 2019