Solvent-free mechanochemical mild oxidation method to enhance adsorption properties of chitosan

doi:10.1007/s11783-021-1416-4

Front. Environ. Sci. Eng.

2021, Vol. 15

Issue (6) : 128 https://doi.org/10.1007/s11783-021-1416-4

RESEARCH ARTICLE

Solvent-free mechanochemical mild oxidation method to enhance adsorption properties of chitosan

Mohammadtaghi Vakili¹, Wen Qiu², Giovanni Cagnetta²(

), Jun Huang²(

), Gang Yu²

¹. Green Intelligence Environmental School, Yangtze Normal University, Chongqing 408100, China
². State Key Joint Laboratory of Environment Simulation and Pollution Control (SKJLESPC), Beijing Key Laboratory for Emerging Organic Contaminants Control (BKLEOC), School of Environment, Tsinghua University, Beijing 100084, China

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Abstract

• Solvent-free chitosan oxidation is obtained by rapid mechanochemical reaction.

• Different oxidants induce very diverse physicochemical changes on chitosan.

• Oxidized chitosan with persulfate or percarbonate has improved adsorption capacity.

• Uptake on oxidized chitosan with persulfate is 125-fold faster than on pristine one.

Oxidation has been profitably utilized to improve some properties of chitosan. However, only solvent-based oxidation procedures have been proposed so far, which are hardly feasible at industrial scale in an economic way because of product recovery cost. In this study, a solvent-free, rapid, and effective oxidation method is proposed. It is based on direct solid-state reaction between chitosan and oxidant powder in a mechanochemical reactor. Results prove that by short high energy ball milling (<3 h) it is possible to achieve diverse physicochemical modifications employing different reagents. Apart from polysaccharidic chain shortening, persulfate provokes high amorphization and induces formation of ketonic groups; percarbonate heightens deacetylation degree, preserving in part crystallinity; calcium peroxide merely deprotonates amino groups and increases amorphization degree. Adsorption tests with the azo-dye reactive red 2 show that adsorption capacity of chitosan co-milled with persulfate (974 mg/g milled product), which is the best performing adsorbent, is twice that of pristine chitosan, while adsorption rate is outstandingly boosted (125 times).

Keywords Chitosan High energy ball milling Mechanochemistry Oxidation

Corresponding Author(s): Giovanni Cagnetta,Jun Huang

Issue Date: 24 March 2021

Cite this article:

Mohammadtaghi Vakili,Wen Qiu,Giovanni Cagnetta, et al. Solvent-free mechanochemical mild oxidation method to enhance adsorption properties of chitosan[J]. Front. Environ. Sci. Eng., 2021, 15(6): 128.

URL:

https://academic.hep.com.cn/fese/EN/10.1007/s11783-021-1416-4
https://academic.hep.com.cn/fese/EN/Y2021/V15/I6/128

Fig.1 SEM images of (a) pristine chitosan, (b) chitosan milled for 1 h, and (c) chitosan co-milled with 30%_w/w potassium persulfate for 1 h.

Fig.2 X-ray diffractograms of chitosan (unmilled and milled) and its oxidized products.

Fig.3 ¹³C CP-MAS NMR of chitosan (unmilled and milled) and its oxidized products.

Fig.4 FTIR spectra of chitosan (unmilled and milled) and its oxidized products.

Fig.5 Thermograms of chitosan (unmilled and milled) and its oxidized products.

Fig.6 Proposed chemical modifications of chitosan caused by the investigated mechanochemical treatment.

Fig.7 Adsorption capacities of chitosan (unmilled and milled) and the products oxidized with (from top to bottom) potassium persulfate, calcium peroxide, and sodium percarbonate under different mechanochemical treatment conditions.

Tab.1 Best-fit parameters of isotherm models

Fig.8 (a) BET isotherm model and (b) pseudo-second order kinetic model for chitosan, 1 h-milled chitosan, and chitosan co-milled for 1 h with 30%_w/w potassium persulfate.

Tab.2 Best-fit parameters of kinetic models

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