Preparation of Carboxylic Acid Grafted Starch Adsorption Resin and Its Dye Removal Performance

doi:10.11901/1005.3093.2020.279

Chinese Journal of Materials Research

2021, Vol. 35

Issue (6): 419-432 DOI: 10.11901/1005.3093.2020.279

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Preparation of Carboxylic Acid Grafted Starch Adsorption Resin and Its Dye Removal Performance

ZHANG Hao¹^,², LI Fan¹^,², CHANG Na³(

), WANG Haitao⁴, CHENG Bowen², WANG Panlei¹

^1.School of Textile Science and Engineering, TianGong University, Tianjin 300387, China
^2.Tianjin Municipal Key Laboratory of Advanced Fiber and Energy Storage, TianGong University, Tianjin 300387, China
^3.School of Chemical Engineering and Technology, TianGong University, Tianjin 300387, China
^4.School of Environmental Science and Engineering, TianGong University, Tianjin 300387, China

Cite this article:

ZHANG Hao, LI Fan, CHANG Na, WANG Haitao, CHENG Bowen, WANG Panlei. Preparation of Carboxylic Acid Grafted Starch Adsorption Resin and Its Dye Removal Performance. Chinese Journal of Materials Research, 2021, 35(6): 419-432.

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Abstract

Carboxylic acid grafted starch adsorption resin (CSR) was synthesized by using natural starch (RS) as matrix, acrylic acid (AA) and vinyl acetate (VAc) as raw materials in the presence of ammonium persulfate (APS) and sodium bisulfite (SHS). The resulted CSR product was characterized by SEM, IR, XRD, ¹³C-NMR and GPC. The results show that when the initiator concentration was 0.03 mol/L, the monomer mass ratio n (AA): n (VAc) was 3:1 and the monomer concentration was 0.8 mol/l, the prepared CSR product presents the carboxyl group content of 19.26% with adsorption capacity of 17.35mg/g for malachite green, in other words, the water resistance and chemical stability and the tolerance to acid, alkali and enzyme of CSR resin were enhanced in comparison to those of the natural starch. After alkali treatment the adsorption capacity of the resin can be further improved. Linear molecules in CSR resin gradually transformed into branched type, resulting in complex network structure of macromolecules. The molecular mass of the main chain of CSR decreased with the increase of monomer dosage and AA / VAc ratio. The adsorption capacity of CSR for basic fuchsin (BF), methylene blue (MB) and malachite green (MG) is better than that of 001×7 strong acid ion exchange resin, D151 weak acid ion exchange resin, carboxymethyl cellulose CMC and carboxymethyl starch CMS and other synthetic and natural polymer adsorbents. The CSR has broad-spectrum of adsorption closed to that of active carbon. The zerocharge point pH_pzc of CSR was 3.83, which was much lower than that of natural starch resin (pH_pzc=7.38), that may be an important reason for the increase of adsorption capacity of cationic dyes. The CSR has good dye adsorption performance in a wide range of pH values, and the adsorption capacity reaches the maximum value when pH=8.5. The decolorization rate of CSR for mixed dye waste water was 87.42%. Finally the CSR had strong regeneration ability. Even after eight regeneration cycles, its decolorization rate was not lower than 88.6% of the initial adsorption ability.

Key words: organic polymer materials starch carboxylic acid type ion-exchange resin dye adsorption water treatment technology

Received: 08 July 2020

ZTFLH:

TQ321.2

Fund: National Key R&D Program of China (Nos. 2019YFC0408404＆ 2019YFC0408405);National Natural Science Foundation of China(51503147);Tianjin Key Science and Technology Program Foundation(19PTZWHZ00030);National Innovation Training Program for College Students(201610058024)

About author: CHANG Na, Tel: 18920020088, E-mail: changna@tiangong.edu.cn

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	Hao ZHANG
	Fan LI
	Na CHANG
	Haitao WANG
	Bowen CHENG
	Panlei WANG

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https://www.cjmr.org/EN/10.11901/1005.3093.2020.279 OR https://www.cjmr.org/EN/Y2021/V35/I6/419

Fig.1 Effect of monomer proportion on the carboxylic acid group content and MG adsorption capacity of CSR

Fig.2 Effect of monomer addition on content of carboxylic acid group and MG adsorption capacity of CSR

Table 1 Effect of monomer addition on viscosity of CSR reaction system

Fig.3 IR spectrum of RS and CSR

Fig.4 ¹³C-NMR spectra of RS and CSR

Fig.5 Scanning electron microscopy of RS and CSR, respectively (a, b), X-ray diffraction patterns of natural starch, RS resin particles and CSR resin particles X-ray diffraction of RS and CSR (c)

Fig.6 Forms of RS in water (a), HCl solution with pH=2 (b), NaOH solution with pH=12 (c) and saccharifying enzyme solution with 50 mg/L for 1 d (d) and e, f, g, h were the forms of CSR in water (e), HCl solution with pH=2 (f), NaOH solution with pH=12 (g) and saccharifying enzyme solution with 50 mg/L for 1 day (h)

Fig.7 Mass loss rate of RS and CSR resin particles after 1d treatment with water, acid (pH=2), alkali (pH=12) and glucoamylase (50 mg/L)

Fig.8 X-ray diffraction pattern of CSR resin treated with acid base enzyme

Fig.9 Effect of monomer ratio on molecular weight and distribution of CSR

Fig.10 Effect of monomer addition on molecular weight and distribution of CSR and thermodynamic fitting result (b) of RS and GSR

Fig.11 Nitrogen adsorption desorption curve (a) and thermodynamic fitting results (b)

Table 2 Langmuir and Freundlich isothermal adsorption parameters of CSR to MG, FB and MB dyes

Fig.12 Adsorption capacity of RS different adsorbents to MG, BF and MB

Fig.13 Curves for the determination of the corresponding points of zero charge (pH_pzc)

Fig.14 Adsorption capacity of RS and CSR for MG, BF and MB at pH 4~10

Fig.15 Adsorption capacity of CSR treated with acid, alkali and enzyme

Fig.16 Decolorization rate of different adsorbents to simulated mixed dyestuff waste water composed of MG, BF, MB and MV (a) and the decolorization rate of CSR to mixed dye waste water after different regeneration cycles (b)

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