Preparation method of powder type high-capacity titanium-based lithium ion exchanger

A technology of lithium ions and exchangers, which is applied in the field of preparation of inorganic non-metallic materials, can solve the problems of unfavorable industrialization, high cost, and difficulty in mass production, so as to avoid the loss of lithium sources, reduce sanding treatment, and reduce raw material costs Effect

Inactive Publication Date: 2019-09-10
JIANGSU TOP FINE NEW RAW MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first two methods have problems such as complex process, expensive raw materials, and difficult process control, which are not conducive to industrialization
High-temperature solid-phase method, the synthesis method is simple, and it is easy to achieve mass production. Usually, the titanium source is mixed with anatase or rutile titanium dioxide and lithium source, and then calcined at high temperature. However, due to the diffusion rate of lithium source in TiO2 crystal, it takes a long time. Sintering, resulting in an excess of more than 20% of the expensive lithium source to make up for the loss of lithium during the sintering process, there are problems of high lithium source consumption and easy sintering of particles
The precursor lithium ion elution process is often eluted with flowing acid. In order to reduce the dissolution loss of titanium, the acid concentration is usually less than 0.2mol / L, resulting in too low concentration of the dissolved lithium solution, which requires high energy consumption for concentration, and contains A large amount of acid, neutralization requires a large amount of base and introduces too many cationic impurities, increasing the cost of lithium source recovery
The above problems lead to the difficulty in quality control of titanium-based lithium ion exchangers, difficulty in mass production and high cost, making it difficult to popularize and apply

Method used

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  • Preparation method of powder type high-capacity titanium-based lithium ion exchanger
  • Preparation method of powder type high-capacity titanium-based lithium ion exchanger
  • Preparation method of powder type high-capacity titanium-based lithium ion exchanger

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A preparation method of a powder type high-capacity titanium series lithium ion exchanger, comprising the following steps:

[0037] Step 1. Take the sulfuric acid method titanium dioxide production process and take the second washing qualified metatitanic acid and beat it with deionized water to TiO 2 The concentration was 300g / L to obtain slurry A; the slurry A was heated to 70°C, and 100g / L sodium hydroxide solution was added dropwise under stirring to control the pH range of 9.5, and the slurry B was obtained after aging for 2 hours;

[0038] Step 2. Slowly add 10% hydrochloric acid solution to the slurry B under stirring to control the pH range to 5.0, and mature for 2 hours to obtain slurry C;

[0039] Step 3, slurry C is filtered, washed with water until the conductivity of the filtrate is less than 50 μS / cm, and the filter cake is made of TiO by adding saturated lithium carbonate solution 2 Slurry D with a concentration of 400g / L;

[0040] Step 4, beating Lithi...

Embodiment 2

[0048] A preparation method of a powder type high-capacity titanium series lithium ion exchanger, comprising the following steps:

[0049] Step 1. Take the sulfuric acid method titanium dioxide production process and take the second washing qualified metatitanic acid and beat it with deionized water to TiO 2 The concentration was 200g / L to obtain slurry A; the slurry A was heated to 65°C, and 100g / L potassium hydroxide solution was added dropwise under stirring to control the pH range of 8.5, and the slurry B was obtained after aging for 3 hours;

[0050] Step 2. Slowly add 10% sulfuric acid solution to the slurry B under stirring to control the pH range to 6.0, and mature for 3 hours to obtain slurry C;

[0051] Step 3, slurry C is filtered, washed with water until the conductivity of the filtrate is less than 50 μS / cm, and the filter cake is made of TiO by adding saturated lithium carbonate solution 2 Slurry D with a concentration of 350g / L;

[0052] Step 4, beating Lithiu...

Embodiment 3

[0060] A preparation method of a powder type high-capacity titanium series lithium ion exchanger, comprising the following steps:

[0061] Step 1. Take the sulfuric acid method titanium dioxide production process and take the second washing qualified metatitanic acid and beat it with deionized water to TiO 2 The concentration was 300g / L to obtain slurry A; the slurry A was heated to 70°C, and 100g / L ammonia solution was added dropwise under stirring to control the pH range of 8.0, and the slurry B was obtained after aging for 2 hours;

[0062] Step 2. Slowly add 10% oxalic acid solution to the slurry B under stirring to control the pH range to 7.0, and mature for 2 hours to obtain slurry C;

[0063] Step 3, slurry C is filtered, washed with water until the conductivity of the filtrate is less than 50 μS / cm, and the filter cake is made of TiO by adding saturated lithium carbonate solution 2 Slurry D with a concentration of 400g / L;

[0064] Step 4, beating Lithium Carbonate wi...

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PUM

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Abstract

The invention provides a preparation method of a powder type high-capacity titanium-based lithium ion exchanger, wherein the titanium source is metatitanic acid on a sulfuric acid process production line, and the precursor can be prepared at low lithium source consumption and short calcination time. The lithium ion elution process of a precursor comprises stirring and adding acid to remove lithiumin a tank, that concentration of slurry H+ in the tank is controlled to prevent the dissolution of titanium, the dissolved lithium is concentrated in a solution, the solid and liquid are separated toobtain a lithium solution with high concentration and low acidity, the concentration energy consumption is reduced and alkali for neutralizing waste acid is reduced, thereby greatly reducing production cost.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic non-metallic materials, in particular to a preparation method of a titanium series lithium ion exchanger. Background technique [0002] Lithium and its compounds are important strategic materials for national economy and national defense construction, and are widely used in many fields such as glass, ceramics, aviation, nuclear energy and new energy. According to the annual report published by the United States Geological Survey (USGS) in January 2016, the world's proven reserves of onshore lithium resources in terms of metal lithium are about 14 million tons, of which reserves in salt lake brine Accounting for 70% to 80%; and the amount stored in seawater is about 260 billion tons. Therefore, in order to meet the needs of sustainable development, scholars from various countries are actively looking for new technologies for extracting lithium from salt lake brine and (concentrated) seawate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J39/09B01J41/10C02F1/28C02F1/42C02F101/10C02F101/20
CPCB01J39/09B01J41/10C02F1/42C02F1/28C02F2101/10C02F2101/20
Inventor 蒋磊朱贤荣杨伟伟
Owner JIANGSU TOP FINE NEW RAW MATERIAL CO LTD
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