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In situ oxidation-reduction preparation of hmn 2 o 4 Methods

An in-situ oxidation and lithium ion technology, applied in chemical instruments and methods, manganese compounds, inorganic chemistry, etc., can solve the problems of reduced adsorption rate and adsorption area, and achieve fast adsorption rate, large adsorption capacity, and easy cleaning The effect of stripping and recycling

Active Publication Date: 2019-10-29
NANJING TECH UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Precursor LiMn was prepared by a combination of sol-gel and calcination 2 o 4 (Functional Materials, 2013, 4(44): 498-506), and Mn(NO 3 ) 2 ,LiOH,H 2 o 2 As a raw material, the precursor LiMn with one-dimensional nanowire structure was synthesized by hydrothermal reaction 2 o 4 (Journal of Process Engineering, 2010, 10 (1): 185-189), the product synthesized by the above method has slight crystal agglomeration, which reduces the adsorption area and the adsorption rate

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  • In situ oxidation-reduction preparation of hmn <sub>2</sub> o <sub>4</sub> Methods
  • In situ oxidation-reduction preparation of hmn <sub>2</sub> o <sub>4</sub> Methods
  • In situ oxidation-reduction preparation of hmn <sub>2</sub> o <sub>4</sub> Methods

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Embodiment 1

[0026] In the hydrothermal reactor, add 10mol / L LiCl.H 2 150mL (1.5 mol) of O deionized aqueous solution, slowly add 4.94g (0.031mol) potassium permanganate, 10mol / L lithium concentration, 0.2mol / L manganese concentration, add 11.03mL (0.05mol) ethanol solution, seal and heat React at 160°C for 14 hours, filter, wash, and dry the product to obtain 5.1 g of a crude lithium ion sieve precursor. The sample was further eluted with hydrochloric acid to obtain a lithium ion sieve, which was characterized by XRD. The spectrum showed that the sample had a sharp peak shape and was a pure phase HMn 2 O 4 , See figure 1 , Continue to perform SEM characterization, it can be seen that the ion sieve is a new flake hexagonal structure, the specific results are shown in figure 2 , Carrying out the adsorption experiment, the ICP measurement results show that the adsorption capacity is 23.4mg / g.

Embodiment 2

[0028] In the hydrothermal reactor, add 10mol / L LiCl.H 2 150mL (1.5 mol) of O deionized water solution, slowly add 19.8g (0.125mol) of potassium permanganate, 10mol / L of lithium, 0.83mol / L of manganese, add 44.2mL (0.2mol) of ethanol solution, seal and heat After reacting at 160°C for 14 hours, the product was filtered, washed, and dried to obtain 17.6 g of a crude lithium ion sieve precursor. XRD characterization of the sample showed that the sample was accompanied by γ-MnOOH impurities. LiMn 2 O 4 Perform elution to obtain HMn 2 O 4 Lithium ion sieve, adsorption experiment, ICP measurement results show that the adsorption capacity is 14.8mg / g.

Embodiment 3

[0030] In the hydrothermal reactor, add 150mL (1.5mol) of 10mol / L LiBr deionized water solution, slowly add 4.94g (0.031mol) of potassium permanganate, lithium concentration 10mol / L, manganese concentration 0.2mol / L, Add 19.83mL (0.09mol) ethanol solution, seal and heat to 130°C for 14h, filter, wash, and dry the product to obtain 4.2g of crude lithium ion sieve precursor. XRD characterization of the sample showed that the sample was accompanied by γ-MnOOH impurities. Further use dilute sulfuric acid to LiMn 2 O 4 Perform elution to obtain HMn 2 O 4 Lithium ion sieve, adsorption experiment, ICP measurement results show that the adsorption capacity is 12.5mg / g.

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Abstract

The invention relates to a method for preparing an HMn2O4 ion sieve through in-situ oxidation-reduction. The method comprises the following concrete steps: sequentially adding a lithium salt solution (lithium source) and permanganate (manganese source) to a hydrothermal reaction kettle according to a certain proportion and stirring till completely dissolving; adding an alcoholic solution, hermetically heating till the hydrothermal reaction is complete to obtain a lithium ion sieve precursor LiMn2O4; and finally eluting by using acid to obtain the HMn2O4 type lithium ion sieve. The lithium ion sieve precursor LiMn2O4 synthesized by adopting an in-situ oxidation-reduction technique has a novel regular flaky hexagonal nanostructure morphology; the HMn2O4 ion sieve obtained after the elution is large in specific area, high in adsorptive selectivity on lithium, large in adsorption capacity, simple in operation and short in consuming time and can be used for adsorption, purification and extraction of lithium ions; and the precursor can also serve as an electrode material of a lithium ion battery.

Description

Technical field [0001] The invention relates to an in-situ oxidation-reduction preparation of HMn 2 O 4 The ion sieve method is a preparation method of an ion sieve adsorbent with excellent adsorption effect and fast adsorption rate. Background technique [0002] Lithium and its compounds are known as "industrial monosodium glutamate". It is widely used in emerging fields such as batteries, ceramics, glass, aluminum, lubricants, refrigerants, and the nuclear industry, and has become an important strategic resource for the national economy and national defense construction. [0003] The ion sieve adsorption method is recognized as the most promising green lithium extraction method due to its good selectivity and relatively low cost. Lithium ion sieve with spinel structure not only has good selectivity, but also has large adsorption capacity and high recycling rate. It is an ideal material with the most industrial application prospects. Among spinel lithium manganese oxide compounds...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/02B01J20/30C01G45/00
CPCB01J20/0222B01J2220/4806B01J2220/4812C01G45/00
Inventor 居沈贵史陈涛陈敏敏薛峰邢卫红
Owner NANJING TECH UNIV