Preparation method of metal cation doped modified lithium ion sieve

A technology of metal cations and lithium ions, applied in chemical instruments and methods, inorganic chemistry, manganese compounds, etc., can solve the problems of long cycle time and cumbersome preparation process steps, and achieve the advantages of reduced dissolution loss, simple preparation process and mild preparation conditions Effect

Pending Publication Date: 2020-05-29
NANJING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, its preparation process steps are cumbersome and the cycle is long

Method used

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  • Preparation method of metal cation doped modified lithium ion sieve
  • Preparation method of metal cation doped modified lithium ion sieve
  • Preparation method of metal cation doped modified lithium ion sieve

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Embodiment 1

[0020] Embodiment 1: (gallium dosage x=0.2, gallium-manganese mixed solution ion concentration is 0.5mol / L, molar ratio Li + / (Mn 2+ + Ga 3+ )=4:1)

[0021] Weigh 0.0225mol of manganese chloride tetrahydrate and 0.0025mol of gallium nitrate hydrate, add 50mL of deionized water, stir until completely dissolved, and obtain a mixed solution of gallium and manganese. Weigh 0.1mol hydrated lithium hydroxide and add it to 50mL deionized water, after stirring for a period of time, add 4mL of 30% hydrogen peroxide solution and continue stirring until fully dissolved, then add the lithium solution dropwise to the above mixed solution at a rate of 5mL / min . After continuing to stir for a period of time, the black precipitate was transferred to a 200 mL polytetrafluoroethylene-lined reactor, and hydrothermally reacted at a temperature of 120° C. for 8 hours in an electric constant temperature blast drying oven. The product is filtered and ground to obtain the doped precursor LiGa 0....

Embodiment 2

[0022] Embodiment 2: (gallium dosage x=0.3, gallium-manganese mixed solution ion concentration is 1mol / L, molar ratio Li + / (Mn 2+ + Ga 3+ ) is 5:1),

[0023] Weigh 0.0425mol of manganese carbonate and 0.0075mol of anhydrous gallium chloride, add 50mL of deionized water, stir until completely dissolved, and obtain a mixed solution of gallium and manganese. Weigh 0.25mol hydrated lithium hydroxide and add it to 50mL deionized water. After stirring for a period of time, add 5mL of 30% hydrogen peroxide solution and continue to stir until fully dissolved. Then add the lithium solution dropwise to the above mixed solution at a rate of 4mL / min. . After continuing to stir for a period of time, the black precipitate was transferred to a 200 mL polytetrafluoroethylene-lined reactor, and hydrothermally reacted at a temperature of 160° C. for 14 hours in an electric constant temperature blast drying oven. The product is filtered and ground to obtain the doped precursor LiGa 0.3 mn ...

Embodiment 3

[0024]Embodiment 3: (gallium dosage x=0.05, gallium-manganese mixed solution ion concentration is 3mol / L, molar ratio Li + / (Mn 2+ + Ga 3+ ) is 1:1)

[0025] Weigh 0.14625mol of manganese bromide and 0.00375mol of anhydrous gallium chloride, add 50mL of deionized water, stir until completely dissolved, and obtain a mixed solution of gallium and manganese. Weigh 0.15mol hydrated lithium hydroxide and add it to 50mL deionized water. After stirring for a period of time, add 8mL of 30% hydrogen peroxide solution and continue stirring until fully dissolved, then add the lithium solution dropwise to the above mixed solution at a rate of 1mL / min. . After continuing to stir for a period of time, the black precipitate was transferred to a 200 mL polytetrafluoroethylene-lined reaction kettle, and hydrothermally reacted at a temperature of 140°C for 10 h in an electric constant temperature blast drying oven. The product is filtered and ground to obtain the doped precursor LiGa 0.05 ...

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Abstract

The invention provides a preparation method of a metal cation doped modified lithium ion sieve. The molecular formula of the metal cation doped modified lithium ion sieve is HGaxMn2-xO4, and x is equal to 0.05-1. The preparation method comprises the following specific steps: preparing a mixed salt solution from a gallium source and a manganese source according to a molar ratio of n(Ga<3+>: Mn<2+>)of x:(2-x) at normal temperature; mixing a lithium source and a hydrogen peroxide solution according to a certain proportion to prepare a lithium solution; slowly dropwise adding the lithium solutioninto the mixed solution, and carrying out a hydrothermal reaction at a certain temperature to obtain an ion sieve precursor doped with metal gallium ions; and finally, carrying out acid pickling treatment on the precursor powder material to obtain the metal gallium ion doped ion sieve adsorbent HGaxMn2-xO4. The adsorbent prepared in the invention is stable in crystal structure, the problem of solution loss of a traditional ion sieve is effectively reduced, and the reusability is improved.

Description

technical field [0001] The invention relates to a preparation method of doped metal cation modified lithium ion sieve, which is used to solve the problem of dissolution loss of traditional lithium ion sieve in the process of adsorption and desorption, and further improve its recyclability. Background technique [0002] Lithium and its compound resources have always been an important energy source for economic development in my country and the world, and are widely used in batteries, aerospace, chemical and other fields. At present, mature lithium extraction technologies include precipitation method, evaporation crystallization method and adsorption method. As one of the most promising adsorption methods, the ion sieve adsorption lithium extraction method has the advantages of high adsorption efficiency, green economy, and simple preparation process. Because the ion sieve has a unique spinel structure, it has the ability to screen and remember lithium ions, so that it can st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/12B01J20/06B01J20/30
CPCC01G45/1242B01J20/06B01J2220/4806C01P2002/72C01P2004/03
Inventor 居沈贵汪博洋薛峰邢卫红
Owner NANJING UNIV OF TECH
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