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Membrane electrode material, preparation method and application of membrane electrode material adsorption-electrochemical lithium method to extract lithium

A membrane electrode and lithium extraction technology, applied in chemical instruments and methods, carbon preparation/purification, nanotechnology for materials and surface science, etc., can solve the problems of power consumption and low lithium adsorption capacity, and achieve high-efficiency separation Effect

Active Publication Date: 2020-09-11
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

LiMn by Siekierka et al. 2 o 4 TiO 2 Doping modification, the adsorption capacity is significantly increased to 36.5mg / g, although it has reached the level of lithium extraction by adsorption, but additional electric energy is consumed in this process (Siekierka A. Lithium dedicated adsorbent for the preparation of electrodesuseful in the ion pumping method. Separation and Purification Technology, 2018, 194, 231-238.)
At present, lithium extraction from membrane capacitors improves the capacity of membrane electrodes through process modification and lattice doping, but there is still the problem of low lithium adsorption capacity.

Method used

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  • Membrane electrode material, preparation method and application of membrane electrode material adsorption-electrochemical lithium method to extract lithium
  • Membrane electrode material, preparation method and application of membrane electrode material adsorption-electrochemical lithium method to extract lithium
  • Membrane electrode material, preparation method and application of membrane electrode material adsorption-electrochemical lithium method to extract lithium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A. Weigh Li 2 CO 3 2.9556g, MnCO 3 18.392g, calcined at 500°C for 4h, heating rate 3°C / min, to obtain LiMn 2 o 4 . 2.7g LiMn 2 o 4 Disperse in 120mL of 0.5mol / L hydrochloric acid solution, stir for 24h; separate the solid product, dry to obtain λ-MnO 2 .

[0037] B. Measure 53mL of N,N-dimethylformamide, 3.5mL of ethanol, and 3.5mL of water to prepare a mixed solution, and weigh MnCl 2 4H 2 O2.198g and 0.6665g of 2,5-dihydroxyterephthalic acid were dissolved in the mixed solution to prepare the raw material solution of Mn-MOF-74.

[0038] C. The 1.5g λ-MnO obtained in step A 2 Add to the 60mL Mn-MOF-74 raw material solution prepared in step B, mix evenly, transfer to the reactor, and react at 80°C for 2h; cool to room temperature, discharge, and centrifuge filter the suspension, and wash three times with DMF solution ;Dried at 40°C for 12h to obtain λ-MnO coated with Mn-MOF-74 2 .

[0039] D. The powder obtained in step C was calcined in a tubular atmosph...

Embodiment 2

[0051] A. Weigh Li 2 CO 3 1.4778g, MnCO 3 9.196g, calcined at 550°C for 5h, with a heating rate of 4°C / min, to obtain LiMn 2 o 4 . 1.35g LiMn 2 o 4 Disperse in 60mL of 0.5mol / L hydrochloric acid solution, stir for 26h; separate the solid product and dry to obtain λ-MnO 2 .

[0052] B. Measure 26.5mL of N,N-dimethylformamide, 1.8mL of ethanol, and 1.8mL of water to prepare a mixed solution, and weigh MnCl 2 4H 2 1.099 g of O and 0.333 g of 2,5-dihydroxyterephthalic acid were dissolved in the mixed solution to prepare a raw material solution of Mn-MOF-74.

[0053] C. The 1.5g λ-MnO obtained in step A 2 Add to the 60mL Mn-MOF-74 raw material solution prepared in step B, mix evenly, transfer to the reactor, and react at 60°C for 4h; cool to room temperature, discharge, and centrifuge filter the suspension, and wash three times with DMF solution ;Dried at 50°C for 10h to obtain λ-MnO coated with Mn-MOF-74 2 .

[0054] D. The powder obtained in step C was calcined in ...

Embodiment 3

[0062] A. Weigh Li 2 CO 3 5.9112g, MnCO 3 36.784g, calcined at 600°C for 6h, with a heating rate of 8°C / min, to obtain LiMn 2 o 4 . 5.4g LiMn 2 o 4 Disperse in 240mL of 0.5mol / L hydrochloric acid solution, stir for 36h; separate the solid product and dry to obtain λ-MnO 2 .

[0063] B. Measure 106mL of N,N-dimethylformamide, 7mL of ethanol, and 7mL of water to prepare a mixed solution, and weigh MnCl 2 4H 2 O4.396g and 1.333g of 2,5-dihydroxyterephthalic acid were dissolved in the mixed solution to prepare a raw material solution of Mn-MOF-74.

[0064] C. The 1.5g λ-MnO obtained in step A 2 Add to the 60mL Mn-MOF-74 raw material solution prepared in step B, mix evenly, transfer to the reactor, and react at 40°C for 6h; cool to room temperature, discharge, and centrifuge filter the suspension, and wash three times with DMF solution ;Dried at 60°C for 8h to obtain λ-MnO coated with Mn-MOF-74 2 .

[0065] D. The powder obtained in step C was calcined in a tubular a...

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Abstract

The invention provides a membrane electrode material, a preparation method of the membrane electrode material and application of the membrane electrode material to an adsorption-electrochemical lithium method to extract lithium. The membrane electrode material is represented as MnO@C. The preparation method comprises the following steps that lithium carbonate and manganese carbonate are calcined,LiMn2O4 is obtained and is dispersed in a hydrochloric acid solution, a solid product is obtained through stirring and separating, drying is carried out, and lambda-MnO2 is obtained; the lambda-MnO2 is added to a formulated Mn-MOF-74 stock solution, a hydrothermal reaction is carried out, and the Mn-MOF-74-coated lambda-MnO2 is obtained; and the Mn-MOF-74-coated lambda-MnO2 is calcined under a nitrogen atmosphere, and the membrane capacitor electrode material MnO2@C is obtained. The material is made into an adsorption membrane electrode plate, and the adsorption membrane electrode plate is assembled into an adsorption-electrochemical coupling lithium extraction device. A pure lithium solution is obtained in a recovery liquid tank through a lithium extraction process and a lithium recoveryprocess. The thickness of the carbon coating layer of the electrode material is adjustable, the adsorption-electrochemical coupling technology combines the dual effects of adsorption and electrochemical lithium intercalation and can extract lithium resources with high capacity and recover the lithium resources; and efficient separation of lithium resources is realized, and a new way is opened forextraction of lithium resources.

Description

technical field [0001] The invention relates to the field of separation and extraction of lithium resources, in particular to a preparation method of a membrane electrode material, which is used in the technology of extracting lithium from a salt lake by an adsorption-electrochemical coupling method. Background technique [0002] Lithium is the first metal element in the periodic table of chemical elements and is widely used in various fields. With the application of secondary batteries in electronic equipment, especially lithium-ion batteries are used to power new energy electric vehicles, the consumption of lithium in batteries has increased, making batteries account for more than half of the market where lithium is used . The demand for lithium-ion batteries has increased significantly, and the market demand for lithium resources will increase sharply, expected to increase by 20% year-on-year. my country's lithium reserves are 4.5 million tons, and salt lake brine lithi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/42C22B3/02C22B26/12C01G45/02C01D15/08C01B32/05B82Y40/00B82Y30/00
CPCC22B3/42C22B3/02C22B26/12C01D15/08C01G45/02C01B32/05B82Y30/00B82Y40/00C01P2004/80C01P2004/64C01G45/1242C01P2002/72C01P2004/04B01D61/52B01D2313/345C22B3/24B01D61/428C01P2006/40C22B7/006
Inventor 项顼孙颖
Owner BEIJING UNIV OF CHEM TECH
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