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Preparation method and application of modified mesoporous hollow silica sphere adsorbent

A technology of hollow silicon and adsorbent, applied in chemical instruments and methods, adsorption water/sewage treatment, other chemical processes, etc., can solve problems such as separation, purification and deep processing of products, increase the complexity of purification process, etc., and achieve unique physical Chemical properties, good monodispersity, high selectivity adsorption separation effect

Inactive Publication Date: 2019-06-28
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Because rubidium is a dispersed element, it often coexists with other alkali metal elements potassium, sodium, lithium, and cesium, and their physical and chemical properties are very similar, which brings great difficulties to the separation, purification and deep processing of rubidium products. Complexity of extraction and purification process

Method used

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  • Preparation method and application of modified mesoporous hollow silica sphere adsorbent
  • Preparation method and application of modified mesoporous hollow silica sphere adsorbent
  • Preparation method and application of modified mesoporous hollow silica sphere adsorbent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Weigh 0.317g CTAB, dissolve it in a mixed solution of 33mL ethanol and 95mL deionized water, stir mechanically for 3 minutes, quickly add 1.92mL ammonia water, continue stirring for 50 minutes, and add 1.92mL TEOS dropwise. After stirring at 35 °C for 22 h, it was centrifuged and washed 3 times with ethanol. Then add 600mL of water and stir at 50°C for 10h. Filter with suction, wash, and place in a muffle furnace for calcination at 500°C for 4 hours to obtain mesoporous hollow silica spheres (HS).

[0044] (2) Weigh LiCl·H according to the ratio of Li:Mn:Si=1:1:10, 1:1:25, 1:1:50 2 O and MnCl 2 4H 2 O, dissolved in 80mL ethanol, made into lithium / manganese ethanol solutions with different concentrations. Take 0.502g of mesoporous hollow silicon spheres and place them in the above lithium / manganese ethanol solutions with different concentrations, shake in a water bath for 20 hours, dry at 70°C, and place them in a muffle furnace at 520°C for calcination for 4 hou...

Embodiment 2

[0048] (1) Weigh 0.320g CTAB, dissolve it in a mixed solution of 35mL ethanol and 98mL deionized water, stir mechanically for 7min, quickly add 2mL ammonia water, continue stirring for 60min, and add 2mL TEOS dropwise. After stirring at 35 °C for 24 h, it was centrifuged and washed 3 times with ethanol. Then add 700mL of water and stir at 80°C for 15h. Suction filtration, washing, and calcination in a muffle furnace at 530° C. for 5 hours to obtain mesoporous hollow silica spheres (HS).

[0049] (2) Weigh LiCl·H according to the ratio of Li:Mn:Si=1:1:10, 1:1:25, 1:1:50 2 O and MnCl 2 4H 2 O, dissolved in 90mL ethanol, made into lithium / manganese ethanol solutions with different concentrations. Take 0.514g of mesoporous hollow silicon spheres and place them in the above lithium / manganese ethanol solutions with different concentrations, shake in a water bath for 22 hours, dry at 75°C, and place them in a muffle furnace at 540°C for calcination for 5 hours. After the reactio...

Embodiment 3

[0053] (1) Weigh 0.324g CTAB, dissolve it in a mixed solution of 37mL ethanol and 102mL deionized water, stir mechanically for 8min, then quickly add 2.05mL ammonia water, continue stirring for 70min, and add 2.07mL TEOS dropwise. After stirring at 35 °C for 26 h, it was centrifuged and washed 3 times with ethanol. Then add 800mL of water and stir at 65°C for 14h. Suction filtration, washing, and calcination in a muffle furnace at 550° C. for 5 h to obtain mesoporous hollow silica spheres (HS).

[0054] (2) Weigh LiCl·H according to the ratio of Li:Mn:Si=1:1:10, 1:1:25, 1:1:50 2 O and MnCl 2 4H 2 O, dissolved in 120mL ethanol, made into lithium / manganese ethanol solutions with different concentrations. Take 0.520g of mesoporous hollow silicon spheres and place them in the above-mentioned lithium / manganese ethanol solutions with different concentrations, shake in a water bath for 24 hours, dry at 75°C, and place them in a muffle furnace at 550°C for calcination for 5 hours....

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Abstract

The invention belongs to the technical field of material preparation and separation, and relates to preparation of lithium / rubidium ion adsorbing materials, in particular to a preparation method and application of a modified hollow mesoporous silicon sphere adsorbent. Hollow mesoporous silicon spheres (HSs) are synthesized, a manganese-based lithium ion sieve (HMO) is supported on the surface of the hollow mesoporous silicon spheres (HS), and finally, 3-aminopropyltriethoxysilane (APTES) is modified to form the modified hollow mesoporous silicon sphere adsorbent. Synthetic process steps are simple, the prepared micro-nano hollow mesoporous silicon spheres have the advantages of large specific surface area, modifiable surface hydroxyl, good mono-dispersity, good particle size and duct size adjustability and the like, the surface of the micro-nano hollow mesoporous silicon spheres with a high specific surface is modified, and the adsorbing capacity of the materials is greatly improved. The manganese-based lithium ion sieve and the APTES are compounded with the micro-nano hollow mesoporous silicon spheres to obtain the modified hollow mesoporous silicon sphere adsorbent with unique physical and chemical properties, and lithium / rubidium ions can be efficiently adsorbed and separated in a high-selectivity manner.

Description

technical field [0001] The invention belongs to the technical field of material preparation and separation, and relates to the preparation of lithium / rubidium ion adsorption materials, in particular to a preparation method and application of a modified mesoporous hollow silicon sphere adsorbent. Background technique [0002] China's salt lakes are mainly distributed in the Qinghai-Tibet Plateau, and the lake water contains more than 59 elements, among which B has a close symbiotic relationship with Li, Cs, K, and Rb, and its content is roughly positively correlated with the increase in the salinity of the lake water. The carbonate-type salt lakes in Tibet are distributed in a belt shape, and are divided into two salt lake sub-zones, Gangnan and Gangbei, with the Gangdise Mountains-Nyainqentanglha Mountains as the boundary. The salt lakes in the Gangnan subbelt are small in scale and low in lithium content; the salt lakes in the west part of the Gangbei subbelt are characteri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/28B01J20/22B01J20/30C02F1/28C22B3/24C22B26/10C22B26/12C02F101/10
CPCB01J20/02B01J20/0262B01J20/22B01J20/28021B01J20/28057B01J20/28083C02F1/28C02F1/281C02F1/285C02F2101/10C22B3/24C22B26/10C22B26/12
Inventor 邱凤仙王媛媛徐雪超郑旭东张涛徐吉成
Owner JIANGSU UNIV
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