羧酸型接枝淀粉吸附树脂的制备和对染料的去除性能

doi:10.11901/1005.3093.2020.279

材料研究学报

2021, Vol. 35

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

研究论文

本期目录 | 过刊浏览

羧酸型接枝淀粉吸附树脂的制备和对染料的去除性能

张昊¹^,², 李帆¹^,², 常娜³(

), 王海涛⁴, 程博闻², 王攀磊¹

^1.天津工业大学纺织科学与工程学院天津 300387
^2.天津工业大学天津市先进纤维与储能技术重点实验室天津 300387
^3.天津工业大学化学工程与技术学院天津 300387
^4.天津工业大学环境科学与工程学院天津 300387

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

引用本文:

张昊, 李帆, 常娜, 王海涛, 程博闻, 王攀磊. 羧酸型接枝淀粉吸附树脂的制备和对染料的去除性能[J]. 材料研究学报, 2021, 35(6): 419-432.
Hao ZHANG, Fan LI, Na CHANG, Haitao WANG, Bowen CHENG, Panlei WANG. Preparation of Carboxylic Acid Grafted Starch Adsorption Resin and Its Dye Removal Performance[J]. Chinese Journal of Materials Research, 2021, 35(6): 419-432.

全文: PDF(8082 KB) HTML

摘要:

以天然淀粉(RS)为基体、以丙烯酸(AA)和乙酸乙烯酯(VAc)为原料在过硫酸铵(APS)和亚硫酸氢钠(SHS)的引发下用水相合成法制备羧酸型接枝淀粉吸附树脂(CSR)，使用SEM、IR、XRD、¹³C-NMR和GPC等手段表征树脂的结构，研究其对染料的去除性能。结果表明：当引发剂的浓度为0.03 mol/L、单体物质量比n(AA)：n(VAc)为3∶1、单体浓度为0.8 mol/L时CSR的羧酸基的含量为19.26%，对孔雀石绿的吸附量为17.35 mg/g。与天然淀粉相比，CSR树脂的耐水性和化学稳定性提高且对酸、碱及酶的耐受性增强，经碱处理后树脂的吸附性进一步提高。GPC分析结果表明，CSR树脂中的线型分子逐渐向分支型转化，使大分子形成复杂的网状结构。CSR的主链分子量随着单体添加量的增加和AA/VAc比例的增大呈下降趋势。CSR对碱性品红(BF)、亚甲基蓝(MB)和孔雀石绿(MG)的吸附量优于001×7强酸性离子交换树脂、D151弱酸性离子交换树脂以及羧甲基纤维素CMC与羧甲基淀粉CMS等合成及天然高分子吸附剂，与活性炭的性能接近，且具有广谱吸附性。CSR的零电荷点pH_PZC为3.83，远低于天然淀粉树脂(pH_PZC=7.38)，是其对阳离子染料吸附量提高的重要原因。CSR在较宽的pH值范围内具有良好的染料吸附性能，当pH值为8.5时吸附量最大值。CSR对混合染料废水的脱色率为87.42%，且具有较强的再生能力，8次再生循环后其脱色率不低于首次吸附的88.6%。

关键词 ：有机高分子材料, 淀粉, 羧酸型, 离子交换树脂, 染料吸附, 水处理技术

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

收稿日期: 2020-07-08

ZTFLH:

TQ321.2

基金资助:国家重点研发计划(2019YFC0408404);国家自然科学基金(51503147);天津市中外联合研究中心项目(19PTZWHZ00030);国家级大学生创新训练计划(201610058024)

作者简介: 张昊，男，1982年生，博士

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图1 单体比例对CSR羧酸基的含量和对孔雀石绿吸附量的影响

图2 单体添加量对CSR羧酸基的含量和对孔雀石绿吸附量的影响

表1 单体添加量对CSR反应体系粘度的影响

图3 RS和CSR的红外光谱图

图4 RS和CSR的13C-核磁共振谱

图5 RS和CSR的扫描电镜照片以及天然淀粉、RS树脂颗粒和CSR树脂颗粒的X-射线衍射谱

图6 RS在水、pH=2的HCl溶液、pH=12的NaOH溶液、用50 mg/L糖化酶溶液处理1 d后的形态和CSR经水、pH=2的HCl溶液、pH=12的NaOH溶液及50 mg/L糖化酶溶液处理1 d后的形态

图7 RS和CSR树脂颗粒经水、酸(pH=2)、碱(pH=12)及糖化酶(50 mg/L)处理1 d后的质量损失率

图8 CSR树脂经酸碱酶处理后的X-射线衍射谱

图9 单体比例对CSR分子量及其分布的影响

图10 单体添加量对CSR分子量及其分布的影响

图11 RS和GSR的氮气吸脱附曲线以及热力学拟合结果

表2 CSR对MG、FB和MB染料吸附的Langmuir、Freundlich等温方程参数

图12 RS、硅藻土、CMC、沸石、001×7树脂、D151树脂、 CMS、CSR和活性炭对MG、BF、MB的吸附量

图13 RS和CSR零电荷点的确定

图14 RS和CSR在pH值为4~10时对MG、BF和MB的吸附量

图15 CSR经酸、碱、酶处理后的吸附量

图16 不同吸附剂对由MG、BF、MB和MV组成的模拟混合染料废水的脱色率和CSR经不同再生循环次数后对混合染料废水的脱色率

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