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A two-dimensional transition metal carbide (nitride) compound airgel and its preparation method and application

A technology of transition metals and nitrides, applied in the direction of alkali metal compounds, nitrogen and non-metal compounds, alkali metal oxides/hydroxides, etc., can solve the problem of underdeveloped three-dimensional pore structure of airgel and the specific surface area of ​​single-layer MXene Large, high specific surface area and other issues, to achieve good application prospects, good adsorption effect, the effect of large specific surface area

Active Publication Date: 2022-04-26
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still many problems in the application of MXene in the field of adsorption, such as the small specific surface area of ​​multilayer MXene, which limits its adsorption capacity; the large specific surface area of ​​monolayer MXene makes it easy to disperse in water and contact with adsorbates, but it is difficult to recover. It is easy to cause secondary pollution, etc.
MXene airgel is a macroscopic body with three-dimensional porous structure formed by overlapping MXene nanosheets. As an adsorption material, it not only has the advantages of high specific surface area and high porosity, but also is easy to recycle, which can avoid secondary pollution to the environment. It has great application potential in the field of adsorption, but there is still little research on the preparation and application of MXene airgel
Li et al. successfully prepared MXene aerogels using ethylenediamine as a cross-linking agent, but the three-dimensional pore structure of the prepared aerogels is not developed, which is not conducive to full contact with the adsorbed substances.
[Li L, Zhang M, Zhang X, et al. New Ti 3C 2, aerogel as promising negative electrode materials for asymmetric supercapacitors [J]. Journal of PowerSources, 2017, 364:234-241.] Liu et al. combined polyacrylic acid and MXene Mix well, prepare MXene / polyacrylic acid airgel by freeze-drying, and then anneal at 300 °C for 2 h in an argon atmosphere to convert it into MXene / polyimide airgel. The airgel has good mechanical properties, but its The process is complicated, high temperature treatment is required, the cost is high, and polyimide will wrap MXene nanosheets, which is not conducive to making full use of the excellent adsorption performance of MXene

Method used

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  • A two-dimensional transition metal carbide (nitride) compound airgel and its preparation method and application
  • A two-dimensional transition metal carbide (nitride) compound airgel and its preparation method and application
  • A two-dimensional transition metal carbide (nitride) compound airgel and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Weigh 1g of lithium fluoride and add it to 20mL of 9M hydrochloric acid solution, stir for 20min to form a uniform solution, then slowly add 1g of ternary layered carbide Ti which has passed through a 200 mesh sieve3 AlC 2 Powder, heated in a water bath at 35°C, and stirred magnetically at 400r.p.m for 24h. Then use absolute ethanol and deionized water to alternately centrifuge and wash 6 times (rotating speed is 4000r.p.m, centrifuge 10min each time), until the supernatant pH=6.2, obtain multilayer Ti 3 C 2 T x . The resulting multilayer Ti 3 C 2 T x Disperse in 50mL deionized water, vortex for 20min, and centrifuge at 1500r.p.m for 1h to remove uncorroded Ti 3 AlC 2 and multilayer Ti 3 C 2 T x , take the above suspension and centrifuge it at 4500r.p.m for 1h to get monolayer or few layers of Ti 3 C 2 T x Nanosheet precipitation.

[0026] (2) Ti obtained in the above steps 3 C 2 T x The nanosheet precipitate was redispersed in water, and its concen...

Embodiment 2

[0030] (1) Weigh 0.5g lithium fluoride and add it into 10mL 9M hydrochloric acid solution, stir for 20min to form a uniform solution, then put 0.5g of Ti 3 AlC 2 The powder was slowly added into the lithium fluoride hydrochloride solution, heated in a water bath at 40°C, and stirred by magnetic force at 400r.p.m for 20h. Then use absolute ethanol and deionized water to alternately centrifuge and wash 6 times (rotating speed is 4000r.p.m, centrifuge 10min each time), until the supernatant pH=6.5, obtain multilayer Ti 3 C 2 T x . The resulting multilayer Ti 3 C 2 T x Disperse in 25mL deionized water, vortex for 10min, and centrifuge at 1500r.p.m for 2h to remove uncorroded Ti 3 AlC 2 and multilayer Ti 3 C 2 T x , take the above suspension and centrifuge at 3500r.p.m for 2h to obtain single or few layers of Ti 3 C 2 T x Nanosheet precipitation.

[0031] (2) Ti obtained in the above steps 3 C 2 T x The nanosheet precipitate was redispersed in water, and its conce...

Embodiment 3

[0035] (1) Weigh 1g of lithium fluoride and add it to 20mL of 9M hydrochloric acid solution, stir for 20min to form a uniform solution, then slowly add 1g of ternary layered carbide Ti which has passed through a 200 mesh sieve 3 AlC 2 Powder, heated in a water bath at 30°C, and stirred with magnetic force at 300r.p.m for 48h. Then use absolute ethanol and deionized water to alternately centrifuge and wash 6 times (rotating speed is 5000r.p.m, centrifuge 5min each time), until the supernatant pH=6.4, obtain multilayer Ti 3 C 2 T x . Disperse the obtained multilayer in 100mL deionized water, shake it by hand for 60min, and centrifuge at 1500r.p.m for 1h to remove uncorroded Ti 3 AlC 2 and multilayer Ti 3 C 2 T x , take the above suspension and centrifuge at 3500r.p.m for 1h to obtain a single layer or few layers of Ti 3 C 2 T x Nanosheet precipitation.

[0036] (2) Ti obtained in the above steps 3 C 2 T x The nanosheet precipitate was redispersed in water, and its...

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Abstract

The invention discloses a two-dimensional transition metal carbon (nitride) compound aerogel, a preparation method and application thereof. The ternary layered carbon (nitride) oxide MAX powder was corroded by HCl+LiF solution, and a stable colloidal suspension of two-dimensional transition metal carbon (nitride) oxide nanosheets was obtained by washing and exfoliation. Adding hydrochloric acid solution to it destroys the electrostatic balance between the two-dimensional transition metal carbon (nitride) nanosheets, guides them to self-assemble to form a hydrogel, and finally obtains a two-dimensional transition metal carbon (nitride) compound gas by vacuum freeze-drying. gel. The prepared airgel has high specific surface area and well-developed pores, the adsorption capacity of lead ion reaches 246mg / g, and the adsorption capacity of toluene reaches 17g / g, which is an ideal adsorption material. The preparation method of the invention is simple, safe, easy to control and suitable for large-scale industrial production, and the prepared two-dimensional transition metal carbide (nitride) compound aerogel has good application prospects in the field of adsorption.

Description

technical field [0001] The invention belongs to the field of nanometer materials and adsorption, and in particular relates to a two-dimensional transition metal carbon (nitride) compound airgel and its preparation method and application. Background technique [0002] In recent years, with the rapid development of industry, we are facing increasingly serious environmental problems, especially heavy metal ions and organic pollution of water resources caused by industries such as metallurgy, electroplating, and textiles, which have had a great impact on the natural environment and human health. harm. Therefore, controlling the pollution of water resources has become an urgent need. Adsorption is a commonly used method for water treatment. It uses the high specific surface area, porous structure and abundant active sites of the adsorbent to absorb heavy metal ions or organic substances in water into its pore structure through physical and chemical actions. Simple and safe, wil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/921C01B32/907C01B32/914C01B32/949C01B21/082B01J20/02B01J20/28B01J20/30C02F1/28B82Y40/00C02F101/20C02F101/30
CPCB01J20/0259B82Y40/00C01B21/0828C01B32/907C01B32/914C01B32/921C01B32/949C02F1/281B01J20/28047B01J20/28054C02F2101/30C02F2101/20
Inventor 潘丽梅王贺贺李文龙任斌张祥刘超杨建丘泰
Owner NANJING TECH UNIV
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