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Preparation method of manganese oxide ion sieve adsorbent and precursor thereof

An ion sieve and adsorbent technology, which is applied in the field of preparation of manganese-based ion sieve adsorbent and its precursor, can solve the problems of incomplete recovery of ion sieve, reduced cycle performance, attenuation of adsorption capacity, etc., so as to improve lithium adsorption performance, The effect of reducing dissolution loss and high selectivity

Inactive Publication Date: 2015-04-22
CHONGQING TECH & BUSINESS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these ion sieves all have the following problems: in the process of adsorption and elution, the released Li + A small number of vacancies cannot be relocated to Li + , so that the adsorbed ion sieve cannot completely return to the state of the precursor, resulting in attenuation of its adsorption capacity and reduced cycle performance

Method used

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  • Preparation method of manganese oxide ion sieve adsorbent and precursor thereof
  • Preparation method of manganese oxide ion sieve adsorbent and precursor thereof
  • Preparation method of manganese oxide ion sieve adsorbent and precursor thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] according to figure 1 The process shown is for the preparation of lithium ion sieve adsorbent and its precursor, the steps are as follows:

[0038] (1) Weigh lithium hydroxide (LiOH·H 2 O) 1.6886g, manganese acetate (Mn(CH 3 COO) 2 4H 2 (2) 12.2550g, dissolved in water respectively to obtain a lithium hydroxide solution and a manganese acetate solution; the lithium hydroxide solution was poured into the manganese acetate solution, and reacted in a constant temperature water bath at 80°C for 3h to generate a brown colloidal precipitate;

[0039] (2) Dry the colloidal precipitate in an oven at 120°C to obtain a light yellow solid; grind the solid into powder and put it in a muffle furnace at a rate of 5°C / min to 450°C for 12 hours to obtain intermediate Product 1 is Li 4 mn 5 o 12 powder;

[0040] (3) Will Li 4 mn 5 o 12 The powder is immersed in 500mL, 0.5mol / L hydrochloric acid solution, stirred for 5h to remove lithium ions, and filtered to obtain the interm...

Embodiment 2

[0046] according to figure 1 The process shown is for the preparation of lithium ion sieve adsorbent and its precursor, the steps are as follows:

[0047] (1) Weigh lithium hydroxide (LiOH·H 2 O) 1.2585g, manganese acetate (Mn(CH 3 COO) 2 4H 2 (2) 12.2550g, dissolved in water respectively to obtain lithium hydroxide solution and manganese acetate solution; the lithium hydroxide solution was poured into the manganese acetate solution, reacted in a constant temperature water bath at 90° C. for 2 hours, and produced a brown colloidal precipitate;

[0048] (2) Dry the colloidal precipitate in an oven at 120°C to obtain a light yellow solid; grind the solid into powder and put it in a muffle furnace at a rate of 5°C / min to 300°C for 18 hours to obtain intermediate Product 1 is Li 4 mn 5 o 12 powder;

[0049] (3) Will Li 4 mn 5 o 12 Add the powder into 500mL, 0.8mol / L hydrochloric acid solution, stir for 5h to remove lithium ions, and filter to obtain the intermediate pro...

Embodiment 3

[0054] according to figure 1 The process shown is for the preparation of lithium ion sieve adsorbent and its precursor, the steps are as follows:

[0055] (1) Weigh lithium hydroxide (LiOH·H 2 O) 1.8877g, manganese acetate (Mn(CH 3 COO) 2 4H 2 (2) 12.2550g, dissolved in water respectively to obtain lithium hydroxide solution and manganese acetate solution; Lithium hydroxide solution was poured into the manganese acetate solution, reacted in a constant temperature water bath at 70°C for 5h, and produced a brown colloidal precipitate;

[0056] (2) Dry the colloidal precipitate in an oven at 120°C to obtain a light yellow solid; grind the solid into powder and put it in a muffle furnace at a rate of 5°C / min to 500°C for 6 hours to obtain intermediate Product 1 is Li 4 mn 5 o 12 powder;

[0057] (3) Will Li 4 mn 5 o 12 Add the powder into 500mL, 0.8mol / L hydrochloric acid solution, stir for 5h to remove lithium ions, and filter to obtain the intermediate product 2, name...

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Abstract

The invention discloses a preparation method of manganese oxide ion sieve adsorbent and a precursor of the manganese oxide ion sieve adsorbent. The method comprises the specific steps that lithium hydroxide solutions are firstly added into manganous salt solutions for a co-precipitation reaction, generated gelatinous precipitate is dried and calcinated, obtained powder is soaked in acid for lithium removal, solutions with lithium are added for a hydrothermal reaction, cooling, filtering, washing and drying are carried out, and the ion sieve precursor Li<4>Mn<5>O<12> is obtained; the precursor is soaked in the acid for lithium removal again, and the ion sieve adsorbent MnO<2>.0.31H<2>O is obtained. The synthetic lithium ion sieve precursor material Li<4>Mn<5>O<12> has a spinel structure, the synthetic ion sieve MnO<2>.0.31H<2>O can be used for extracting lithium of salt lake brine, seawater and other lithium solutions, and the advantages of being large in adsorption capacity, high in selectivity and good in circulating performance are achieved.

Description

technical field [0001] The invention belongs to the field of materials, and in particular relates to a preparation method of a manganese ion sieve adsorbent and its precursor. Background technique [0002] Lithium and its compounds are of great significance to the national economy and national defense, and are widely used in glass and ceramic industries, nonferrous metallurgy industries, air conditioners, medicine, and organic synthesis. In recent years, due to the rapid development of information technology and electric vehicles, lithium-ion batteries have become one of the fastest-growing fields of new energy. As the key raw materials of lithium-ion batteries-lithium compounds (lithium carbonate and lithium hydroxide), the demand is strong. However, solid lithium ore resources are decreasing day by day, and the cost of extracting lithium remains high, which limits the rapid development of related industries. At present, lithium extraction from liquid lithium-containing br...

Claims

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Application Information

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IPC IPC(8): B01J20/06B01J20/30
CPCB01J20/06B01J20/30B01J2220/4806
Inventor 许惠熊晓莉
Owner CHONGQING TECH & BUSINESS UNIV
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