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Preparation and Application of 2-Hydroxymethyl-12-crown Ether-4 Modified Hierarchical Porous Silicon Materials

A multi-level porous, silicon material technology, applied in the direction of silicon compound, polluted waterway/lake/pond/river treatment, other chemical processes, etc. Simple and easy to operate, improve adsorption capacity, high selectivity adsorption separation effect

Active Publication Date: 2019-04-02
江阴智产汇知识产权运营有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In particular, the coexistence of magnesium ions with similar chemical properties makes it difficult to extract and separate lithium from salt lake brine, which seriously restricts the development of my country's salt lake industry, especially the lithium salt industry.

Method used

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  • Preparation and Application of 2-Hydroxymethyl-12-crown Ether-4 Modified Hierarchical Porous Silicon Materials
  • Preparation and Application of 2-Hydroxymethyl-12-crown Ether-4 Modified Hierarchical Porous Silicon Materials
  • Preparation and Application of 2-Hydroxymethyl-12-crown Ether-4 Modified Hierarchical Porous Silicon Materials

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preparation example Construction

[0036] Preparation of Nanocrystalline Cellulose (NCC)

[0037] Weigh 5 g of absorbent cotton, place it in 75 mL of 1:1 sulfuric acid, control the temperature at 45 °C, and hydrolyze for 2 hours; add a large amount of water to terminate the hydrolysis reaction, and let it stand for 10 hours; then pour off the supernatant, take the lower layer, and Centrifuge to control the volume to less than 130mL; adjust the pH of the solution to 2.4 by dialysis, and set aside.

Embodiment 1

[0039] (1) Dissolve 30 mg of CTAB in a mixed solution of 40 mL of distilled water and 20 mL of ethanol, and stir vigorously at 30 °C for 2 h. Add 400 μL NH 3 ·H 2 O and 4mL of 0.5% NCC (pre-sonicated for 30min), stirred for 10min. Then add 100μL TEOS and stir for 2h. After the reaction, wash twice with distilled water and ethanol alternately, dry at 30°C to obtain a hierarchical porous silicon / NCC composite, and calcinate in a muffle furnace at 540°C for 6 hours to remove NCC and obtain a hierarchical porous silicon material.

[0040] (2) Take 1 g of the activated hierarchical porous silicon material, add it to 75 mL of dry toluene, add 0.2 mL of 2C12M4 under nitrogen protection for 30 min, and condense and reflux at 80 ° C for 24 h. After the reaction, filter, wash with ethanol three times, and dry at 60°C to obtain the lithium ion adsorption material.

[0041] (3) Add the prepared pure lithium chloride solution into a 10mL colorimetric tube, then add lithium ion adsorpti...

Embodiment 2

[0043] (1) Dissolve 30 mg of CTAB in a mixed solution of 40 mL of distilled water and 20 mL of ethanol, and stir vigorously at 30 °C for 1.5 h. Add 300 μL NH 3 ·H 2 O and 3mL of 0.5% NCC (pre-sonicated for 30min), stirred for 8min. Then add 80μLTEOS, continue to stir for 2h. After the reaction, wash twice with distilled water and ethanol alternately, dry at 30°C to obtain a hierarchical porous silicon / NCC composite, and calcinate in a muffle furnace at 540°C for 6 hours to remove NCC and obtain a hierarchical porous silicon material.

[0044] (2) Take 1 g of the activated hierarchical porous silicon material, add it to 75 mL of dry toluene, add 0.1 mL of 2C12M4 under nitrogen protection for 30 min, and reflux at 80 ° C for 24 h. After the reaction, filter, wash with ethanol three times, and dry at 60°C to obtain the lithium ion adsorption material.

[0045] (3) Add the prepared pure lithium chloride solution into a 10mL colorimetric tube, then add lithium ion adsorption mate...

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Abstract

The invention relates to preparation of a lithium ion adsorption material, especially to a preparation method for a 2-hydroxymethyl-12-crown 4-ether modified hierarchically-porous silicon material, belonging to the technical field of synthesis of composite materials. The preparation method comprises the following steps: preparing nanocrystal cellulose at first; then with nanocrystal cellulose as a hard template and cetyl trimethyl ammonium bromide as a soft template, preparing a hierarchically-porous silicon material by using a template process; and then modifying the hierarchically-porous silicon material with 2-hydroxymethyl-12-crown 4-ether. The invention also discloses application of the modified hierarchically-porous silicon material to adsorption of alkali metal ions, especially to adsorption of lithium ions in salt lake bittern. According to the invention, the hierarchically-porous material with a high specific surface is employed, so the adsorption capacity of the modified hierarchically-porous silicon material is greatly improved; and the preparation process is simple and easy to operate. The lithium ion adsorption material prepared in the invention can realize high-efficiency high-selectivity adsorption and separation of alkali metal ions, especially lithium ions, and provides a feasible solution to sustainable development of the industry of extraction of lithium from a salt lake.

Description

technical field [0001] The invention belongs to the technical field of composite material synthesis and relates to the preparation of lithium ion adsorption materials, in particular to the preparation and application of a 2-hydroxymethyl-12-crown-4 modified hierarchical porous silicon material. Background technique [0002] Lithium (lithium), as the "energy metal of the 21st century", has a wide range of applications in various industries, especially in the fields of lithium batteries and nuclear fusion, so it is known as an important element that drives the world forward. [0003] At present, 80% of the total global production of lithium comes from salt lake brine, and my country also has abundant brine lithium resources in the salt lake areas of Tibet and Qinghai. Among them, the lithium reserves in Qinghai Salt Lake rank first in the country, accounting for more than 90% of the country's proven lithium reserves, and have the characteristics of large reserves and high grad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/10B01J20/30C02F1/28
CPCB01J20/103B01J20/22C02F1/281C02F2103/007
Inventor 邱凤仙徐雪超杨冬亚郑旭东王媛媛张涛潘建明徐吉成
Owner 江阴智产汇知识产权运营有限公司
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