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Preparation method of pickling indissolvable lithium ion sieve suitable for industrialized production

A lithium ion and insoluble technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of short service life of lithium ion sieve, increased load of subsequent separation, high dissolution rate of manganese ion, etc., to ensure long-term use and Efficiency, reduced dissolution loss rate, low niobium dissolution rate effect

Inactive Publication Date: 2014-10-15
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
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AI Technical Summary

Problems solved by technology

The above-mentioned manganese-containing lithium ion sieve has a too high dissolution rate of manganese ions during the pickling process, usually 3%-20%, which not only increases the load for subsequent separation, but also leads to a short service life of the lithium ion sieve, which cannot be used repeatedly. Frequent replacement, resulting in increased production costs, especially not suitable for use when extracting lithium in industrial production

Method used

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Examples

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preparation example Construction

[0020] A preparation method suitable for industrialized production and insoluble in pickling lithium ion sieve, comprising the following steps:

[0021] ⑴. Preparation of precursor:

[0022] The powdered Li 2 CO 3 and Nb 2 o 5 Mix (the finer the two polycrystalline powders are, the better), the molar ratio of lithium ions and niobium ions in the two raw materials is 1-1.8:1, the mixture is placed in a mortar and ground for 2 hours to mix it evenly, and the ground The final mixture is placed in a crucible and put into a muffle furnace for calcination. The calcination temperature is 800-1200°C, and the calcination time is 2-12 hours. The reaction releases CO 2 , generating LiNbO 3 crystal;

[0023] ⑵. Preparation of lithium ion sieve:

[0024] The LiNbO prepared by step (1) 3 The crystal is placed in an acid solution to elute lithium ions in the crystal. The acid solution is hydrochloric acid (HCl) or nitric acid (HNO 3 ) or sulfuric acid (H 2 SO 4 ), the concentratio...

Embodiment 1

[0026] A preparation method suitable for industrialized production and insoluble in pickling lithium ion sieve, comprising the following steps:

[0027] ⑴. Preparation of precursor:

[0028] The powdered Li 2 CO 3 and Nb 2 o 5 Mixing, the molar ratio of lithium ions and niobium ions in the two raw materials is 1:1, the mixture is placed in a mortar and ground for 2 hours to make it evenly mixed, the ground mixture is placed in a crucible and put into a muffle Calcination is carried out in the furnace, the calcination temperature is 800°C, the calcination time is 12 hours, and the reaction releases CO 2 , generating LiNbO 3 crystal;

[0029] ⑵. Preparation of lithium ion sieve:

[0030] The LiNbO prepared by step (1) 3 The crystal is placed in an acid solution to elute lithium ions in the crystal. The acid solution is hydrochloric acid HCl. The elution rate of ions and the dissolution rate of niobium ions were analyzed, and the solid sample was washed three times with ...

Embodiment 2

[0032] A kind of preparation method suitable for industrialized production and insoluble lithium ion sieve to pickling, comprises the following steps:

[0033] ⑴. Preparation of precursor:

[0034] The powdered Li 2 CO 3 and Nb 2 o 5 Mixing, the molar ratio of lithium ions and niobium ions in the two raw materials is 1.6:1, the mixture is placed in a mortar and ground for 2 hours to make it evenly mixed, the ground mixture is placed in a crucible and put into a muffle Calcination is carried out in the furnace, the calcination temperature is 850°C, the calcination time is 6 hours, and the reaction releases CO 2 , generating LiNbO 3 crystal;

[0035] ⑵. Preparation of lithium ion sieve:

[0036] The LiNbO prepared by step (1) 3 The crystal is placed in an acid solution to elute lithium ions in the crystal, the acid solution is nitric acid HNO 3 , the concentration of the nitric acid solution is 10mol / L, the shaking washing time is 3 days, then filter, and collect the pi...

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Abstract

The invention relates to a preparation method of a pickling indissolvable lithium ion sieve suitable for industrialized production. The method comprises the steps of: (1) production of a precursor: mixing powdered Li2CO3 with Nb2O5 and conducting calcinations to generate a LiNbO3 crystal; and (2) preparation of a lithium ion sieve: placing the LiNbO3 crystal in an acid solution to elute lithium ions, thus obtaining the lithium ion sieve. The preparation method for the lithium ion sieve provided by the invention has the characteristics of reasonable design and simple operation. The method utilizes the characteristic of insolubility of the lithium ion sieve in acid to prepare the lithium ion sieve with the unique advantages of high lithium elution rate, low niobium solution loss rate and large adsorption capacity. The prepared lithium ion sieve can be used repeatedly, can withstand the adsorption and acid elution process, still can ensure integrity after continuous use for a long time, and is especially suitable for use in industrialized production. Lithium is extracted from salt lake brine and seawater, thus providing strong support for the industrialization development of lithium extraction from salt lake brine and seawater.

Description

technical field [0001] The invention relates to the field of ion sieve preparation, in particular to a preparation method of a lithium ion sieve suitable for industrial production and insoluble in pickling. Background technique [0002] Lithium is an important light metal. Lithium and its compounds are widely used in traditional industrial fields such as glass ceramics, electrolytic aluminum, grease, air conditioning and refrigeration, metallurgy, medicine, reagents, and organic synthesis, and are also used in emerging high-energy batteries, aerospace technology, and functional materials. Applications in high-tech fields such as nuclear fusion power generation are also developing rapidly. my country is a country with a large amount of lithium resources. More than 80% of the terrestrial lithium resources exist in salt lake brine. The technology of extracting lithium from salt lake brine and seawater has become a research hotspot. How to realize industrialized lithium extracti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/06B01J20/30
Inventor 王昶林鹏
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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