Preparation method of granular titanium-based lithium ion sieve adsorbent with high adsorption capacity

A titanium-based lithium, high-adsorption technology, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the problems of separation and washing difficulties, reduction of specific surface area, difficulty in filtration and separation, etc. Achieve the effect of high lithium adsorption capacity, small specific gravity and simple molding process

Active Publication Date: 2022-04-15
CHENGDU CHEMPHYS CHEM IND +1
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Problems solved by technology

[0005] Lithium ion sieve in powder state has the advantages of large adsorption capacity and high adsorption efficiency due to its fine particle size, large specific surface area, and sufficient solid-liquid contact; however, there are engineering problems such as separation and washing difficulties in industrial use. , high dissolution loss and other issues, it is necessary to shape and granulate the powder lithium ion sieve. After granulation, the filterability and washing efficiency are greatly improved, and the dissolution loss of the adsorbent is also greatly reduced. The adsorption capacity has been greatly attenuated, even only 20%-30% of the original lithium-ion sieve powder. In order to improve the particle size and specific surface area of ​​the formed adsorbent, researchers at home and abroad have actively developed adsorbent forming methods in recent years. Cost, efficient, scalable process and device

Method used

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  • Preparation method of granular titanium-based lithium ion sieve adsorbent with high adsorption capacity
  • Preparation method of granular titanium-based lithium ion sieve adsorbent with high adsorption capacity
  • Preparation method of granular titanium-based lithium ion sieve adsorbent with high adsorption capacity

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preparation example Construction

[0041] A method for preparing high adsorbing capacity granulated titanium-based lithium ion sieve adsorbents, including steps:

[0042] Step 1, preparing titanium-based lithium ion sieve precursor powder;

[0043] a) mix the lithium source, titanium dioxide, and dispersant mechanical ball milling, control the purification Li / Ti molar ratio 2: (1-1.2), then add a high temperature mixing agent mix, and the spray is dry to granulate powder, will The grain powder was transferred to a microwave high temperature sintering furnace, and the calcination of 2-3 h, cooled, and the titanium-based lithium ion sieve precursor powder was carried out at 350-650 ° C.

[0044] Or b) mix the titanium source, lithium hydroxide, and appropriate amount of water, control the feed Li / Ti molar ratio 2: (1-1.2), and add 0.5 to 1.5 wt% hydrogen oxygen, stirred under ultrasound 60-90 ° C. 3-6h, sequentially filtered, washed, added high-temperature mixing agent mixing, spray drying to granulated powder, t...

Embodiment 1

[0068] A method for preparing high adsorbing capacity granulated titanium-based lithium ion sieve adsorbents, including steps:

[0069] (1) Preparation of lithium titanate powder;

[0070] 19.7 kg of titanium dioxide, 17.4 kg of battery-grade carbonate, 0.1 kg of 1.5 wt% PEG6000 aqueous solution high-speed dispersion, mechanical ball milling control particle size D50 = 550 ~ 850 nm, then add polyether sulfone powder mixing to spray precomive grain, spray The pre-storage temperature is set 200 ° C, and finally calcined the lithium ion screen before the microwave oven 600 ° C. 2 TiO 3 ;

[0071] (2) PES-H 2 TiO 3 Rod-shaped adsorbent

[0072] S1 Preprocessing: After the precursor of the lithium-bias ion sieve precursor was ground, it was 250 mesh, and the lithium-sized ion-sieve precursor was obtained.

[0073] S2 15% PES sol formulation: Take 2.7 kg of PES (polyether sulfone) to add 15 l of dimethylacetamide, continuously stirred in a 50 ° C water bath to completely dissolve, 15% P...

Embodiment 2

[0086] (1) Preparation of lithium titanate powder;

[0087] 40 kg of titanium dioxide was mixed with 10 kg of water into a hierarrier, 10.5 kg of solid lithium hydroxide and mixed stirring uniform; the ultrasonic frequency was 10 ° C under conditions, and the reaction was stirred at normal pressure for 6 h, and the reaction process was added dropwise (total) 30% hydrogen oxide water is about 100 mL), filtered, washed, washed, obtained by tidal lithium ion sieve powder, filtrate returning generic cycle; wet material is pulped, add 0.1 kg of polymer pore agent polyethersulfone mixed, mixed, spray Pre-enrichment to 450 ° C under air atmosphere, calcined for 3 h, cool to room temperature to obtain a lithium-ion sieve Li 2 TiO 3 .

[0088] (2) PES-H 2 TiO 3 Rod-shaped adsorbent

[0089] PES-H 2 TiO 3 The preparation process of the rod-shaped adsorbent is in Example 1, and the granulation is used for centrifugal devices, and the slurry is over 80 mesh sieve, the drum diameter is 60 mm, ...

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Abstract

The invention relates to a preparation method of a high-adsorption-capacity granular titanium-based lithium ion sieve adsorbent. The method comprises the following steps: step 1, preparing titanium-based lithium ion sieve precursor powder; step 2, preparation of the high-adsorption-capacity granular titanium-based lithium ion sieve adsorbent: 1) pretreatment of precursor powder; 2) preparing a composite adhesive; (3) doping, blending and homogenizing; (4) molding and granulating; and 5) eluting and replacing. The prepared granular adsorbent has relatively high porosity, shows good suspension property when being used for extracting lithium from salt lake brine or simulated brine, and is high in adsorption and desorption rate and high in lithium extraction activity, and the lithium ion selectivity and the elution rate can reach 95% or above; the granular adsorbent is stable in structure, low in solution loss and long in cycle service life; the forming and granulating process of the granular adsorbent is simple and easy to control, and industrialization is easy to realize.

Description

Technical field [0001] The present invention relates to the preparation of new chemical materials, and is specifically a method for preparing a high adsorption capacity granular titanium-based lithium ion sieve adaptive. Background technique [0002] In the 21st century, computer, digital cameras, mobile phones, mobile power tools and other electronic products, the continuous development of new energy vehicles, and lithium-ion batteries have become the largest consumption in the world. [0003] Lithium resources in nature are mainly stored in granite-type deposits and salt lakes, seawater and geothermal water, indicating that lithium resources mainly based on lithium, and the lithium-lithium resource accounts for 61% of the total resources of lithium, and ore lithium 34%, the remaining 5% of lithium resources exist in oilfield and geothermal water. [0004] Adsorption Lithium Technology is a new type of salt lake lithium solution in recent years. This process uses a particular li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/06B01J20/28B01J20/30B01J20/32C22B26/12C22B3/24
CPCB01J20/06B01J20/28B01J20/30B01J20/32C22B3/24C22B26/12Y02P10/20
Inventor 杨进锋孟强班文俊蔡荣富戴毅華
Owner CHENGDU CHEMPHYS CHEM IND
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