One-step method for preparing manganese ion sieve precursor lixmn3-xo4

Abstract

The invention discloses a one-step method for preparing manganese oxide ion sieve precursor Li x mn 3‑x o 4 The method is to mix the manganese salt, oxidant, and lithium-containing inorganic powders, and the slurry after one-step liquid-solid phase reaction in a closed environment is directly dried and then roasted and annealed to obtain the manganese oxide lithium ion sieve precursor. stamina x mn 3‑x o 4 . The lithium ion sieve precursor Li x mn 3‑x o 4 It can be used for selective adsorption and extraction of lithium from lithium-containing aqueous solutions such as brine and seawater. The preparation method of the invention has simple operation process, low sintering temperature, no waste water and waste material, abundant raw material sources, low price and low energy consumption. It is an energy-saving and environment-friendly green economic lithium ion sieve production method.

Description

technical field [0001] The invention belongs to the field of energy-saving production of inorganic compounds, in particular to one-step preparation of manganese ion sieve precursor Li x mn 3-x o 4 Methods. Background technique [0002] Li x mn 3-x o 4 It is a general term for manganese oxide ion sieve precursors. The most studied lithium manganese oxide ion sieve precursors are LiMn 2 o 4 , Li 1.33 mn 1.67 o 4 (Li 4 mn 5 o 12 ) and Li 1.6 mn 1.6 o 4 (LiMnO 2 ). Usually, the methods for preparing the above precursors include soft chemical methods, sol-gel methods, hydrothermal methods, etc. The existing synthesis methods generally use MnOOH as a manganese source to synthesize LiMnO 2 , and the synthesis of MnOOH itself is relatively complicated, requiring high operating conditions, and MnOOH is unstable in the air, which is not conducive to industrial production; in the preparation process of the hydrothermal method, other additives such as oxidants need to ...

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Problems solved by technology

The raw material used in this document is the trivalent manganese raw material Mn 2 o 3 , instead of manganese salt, the reaction process not only has high temperature and high energy consumption, but also has a complicated preparation process and a low degree of industrialization;

[0005] Also, "CN103121724A prepares lithium ion sieve MnO 2 0.5H 2 O and its precursor Li 1.6 mn 1.6 o 4 method", using inorganic manganese salts and lithium salts as raw materials, one-step hydrothermal synthesis of intermediates, and then low-temperature roasting to obtain the required precursor Li 1.6 mn 1.6 o 4 ; Then the precursor is acid-treated to extract the Li in it to become an H-type ion sieve, and then wash, filter, and dry to obtain the ion sieve adsorbent MnO which has a screening effect on lithium ions. 2 0.5H 2 O; obtained by hydrothermal synthesis first, and then roasted, the preparation process is complicated and the preparation time is long

[0006] In addition, "CN106311190A preparation method of porous manganese lithium ion sieve adsorbent" uses manganese salt and lithium salt as raw materials, uses chitosan solution as dispersant, undergoes hydrothermal reaction, and roasts at low temperature to obtain lithium ion sieve precursor Li 4 mn 5 o 12 ; Then the precursor is acid-treated, the Li therein is extracted, washed with acid leaching, filtered and dried to obtain lithium ion sieve H 4 mn 5 o 12 In this patent, it takes multi-step treatment to obtain the precursor, hydrothermal and roasting, the treatment process is complicated, and the reaction time is long. The prepared adsorbent takes more than 10 hours to reach the adsorption equilibrium, and the adsorption time is long

[0007] It can be seen that the preparation methods in the prior art do not really realize the simplification of the process and the good adsorption effect. The present invention is based on the simple preparation process (one-step method) and the good preparation method of the obtained adsorbent.

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