聚吡咯/壳聚糖复合膜的制备及其对Cu(Ⅱ)和Cr(Ⅵ)吸附机制

狄婧; 刘海霞; 姜永强; 郭金鑫; 赵国虎

doi:10.13801/j.cnki.fhclxb.20200831.005

聚吡咯/壳聚糖复合膜的制备及其对Cu(Ⅱ)和Cr(Ⅵ)吸附机制

doi: 10.13801/j.cnki.fhclxb.20200831.005

狄婧^1,,
刘海霞^2,,
姜永强^2,,
郭金鑫^2,,
赵国虎^{1, 2, ,}

1.
兰州交通大学　化学与生物工程学院，兰州 730070
2.
兰州城市学院　化学化工学院　“城市环境污染控制”甘肃省高校省级重点实验室，兰州 730070

基金项目: “生态环境相关高分子材料教育部重点实验室”开放基金(KF-18-04)；甘肃省自然科学基金(18JR3RA220)

详细信息

通讯作者:
赵国虎，博士，教授，硕士生导师，研究方向为电分析化学与水污染处理技术　 E-mail：529401412@qq.com

中图分类号: TB332
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出版历程
- 收稿日期: 2020-03-18
- 录用日期: 2020-07-31
- 网络出版日期: 2020-09-01
- 刊出日期: 2021-01-15

Preparation of polypyrrole/chitosan composite membrane and its adsorption mechanism for Cu(Ⅱ) and Cr(Ⅵ)

DI Jing^1
,,
LIU Haixia^2
,,
JIANG Yongqiang^2
,,
GUO Jinxin^2
,,
ZHAO Guohu^{1, 2
, ,}

1.
School of Chemical and Biological Engineering, Lanzhou Jiaotong University, Lanzhou 730070, China
2.
School of Chemistry and Chemical Engineering, Provincial Key Laboratory of Gansu Higher Education for City Environmental Pollution Control, Lanzhou City University, Lanzhou 730070, China

摘要

摘要: 以聚吡咯(PPy)和壳聚糖(CS)为原料，制备PPy/CS复合膜，通过红外、孔径分析、热分析和SEM等手段对其结构进行表征，并研究了PPy/CS复合膜对Cu(Ⅱ)和Cr(Ⅵ)吸附性能的影响及吸附机制，考察了pH值、吸附时间、溶液起始浓度等因素对吸附率的影响。结果表明，初始浓度对吸附率影响最大；在pH=3.5、温度为333 K及速率为100 r·min⁻¹下震荡吸附50 min，20 mg的PPy/CS复合膜吸附6 mg·L⁻¹的Cu(Ⅱ)和Cr(Ⅵ)混合液时，PPy/CS复合膜对Cu(Ⅱ)表现出很好的选择性，吸附量达2.715 mg·g⁻¹；通过对PPy/CS复合膜和CS膜的吸附性能比较，PPy/CS复合膜对Cu(Ⅱ)的吸附率增加至94.14%；采用0.1 mol·L⁻¹的NaOH溶液对吸附Cu(Ⅱ)和Cr(Ⅵ)的PPy/CS复合膜进行脱附再生，循环15次后，其吸附量变化很小，可以多次使用。研究表明，PPy/CS复合膜对Cu(Ⅱ)和Cr(Ⅵ)的吸附符合准二级动力学模型和Langmuir吸附等温式。
- 聚吡咯 /
- 壳聚糖 /
- 复合膜 /
- 吸附 /
- Cu(Ⅱ) /
- Cr(Ⅵ)
Abstract: A polypyrrole/chitosan (PPy/CS) composite membrane was prepared using PPy and CS as raw materials, and the structure of the PPy/CS composite membrane was characterized by infrared, pore diameter analysis, thermal analysis and SEM. The effects of PPy/CS composite membrane on the adsorption performance and adsorption mechanism for Cu(Ⅱ) and Cr(Ⅵ) were discussed. The effects of pH value, adsorption time, and initial concentration of the solution on the adsorption efficiency were investigated. The results show that the adsorption efficiency of PPy/CS composite membrane for Cu(Ⅱ) and Cr(Ⅵ) are greater affected by the initial concentration of the solution. When pH=3.5, temperature is 333 K, the adsorption is shaken at 100 r·min⁻¹ for 50 min, 20 mg of PPy/CS composite membrane adsorbs 6 mg·L⁻¹ of Cu(Ⅱ) and Cr(Ⅵ), PPy/CS composite membrane for Cu(Ⅱ) shows good selectivity and adsorption amount reaches 2.715 mg·g⁻¹; Compared with PPy/CS composite membrane and CS membrane, the adsorption rate of PPy/CS composite membrane for Cu(Ⅱ) increases to 94.14%; The PPy/CS composite membrane adsorbing Cu(Ⅱ) and Cr(Ⅵ) is desorbed and regenerated with 0.1 mol·L⁻¹ NaOH solution. After circulation for 15 times, its adsorption amount changes very small, it can be used multiple times. The adsorption of Cu(Ⅱ) and Cr(Ⅵ) by PPy/CS composite membrane conforms to the pseudo-second-order kinetic model and Langmuir adsorption isotherm.
- polypyrroles /
- chitosan /
- composite membrane /
- adsorption /
- Cu(Ⅱ) /
- Cr(Ⅵ)

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图 1 聚吡咯/壳聚糖(PPy/CS)复合膜吸附Cu(Ⅱ)和Cr(Ⅵ)的机制

Figure 1. Mechanism of Cu(Ⅱ) and Cr(Ⅵ) adsorption by polypyrrole/chitosan (PPy/CS) composite membrane

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图 2 CS膜和PPy/CS复合膜的SEM图像

Figure 2. SEM images of CS membrane and PPy/CS composite membrane

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图 3 PPy/CS复合膜、CS膜和吸附Cu(Ⅱ)和Cr(Ⅵ)后的PPy/CS复合膜的FTIR图谱

Figure 3. FTIR spectra of PPy/CS composite membrane, CS membrane and PPy/CS composite membrane after adsorption of Cu(Ⅱ) and Cr(Ⅵ)

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图 4 PPy/CS复合膜的TG和DTA曲线

Figure 4. TG and DTA curves of PPy/CS composite membrane

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图 5 PPy/CS复合膜吸附Cu(Ⅱ)和Cr(Ⅵ)的XPS图谱

Figure 5. XPS spectra of PPy/CS composite membrane adsorption of Cu(Ⅱ) and Cr(Ⅵ)

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图 6 CS膜和PPy/CS复合膜的吸附率

Figure 6. Adsorption rate of CS membrane and PPy/CS composite membrane

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图 7 初始浓度(a)、投加量(b)、吸附时间(c)、pH值(d)、反应温度(e)和震荡速率(f)对PPy/CS复合膜吸附量和吸附率的影响

Figure 7. Effect of initial mass concentration (a), dosage (b), adsorption time (c), pH value (d), reaction temperature (e) and shock rate (f) on adsorption quantity and adsorption rate of PPy/CS composite membrane

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图 8 循环次数对PPy/CS复合膜吸附量的影响

Figure 8. Effects of cycling times on adsorption quantity of PPy/CS composite membrane

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表 1 CS膜和PPy/CS复合膜的比表面积和孔径

Table 1. Specific surface area and pore size of CS membrane and PPy/CS composite membrane

Sample	S_BET/(m²·g⁻¹)	D_BJH/nm
CS	27.32	3.507
PPy/CS	14.08	3.138
Notes: S_BET—Specific surface area measured by BET; D_BJH—Average pore measured by BJH.

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表 2 PPy/CS复合膜吸附Cr(Ⅵ)和Cu(Ⅱ)正交实验数据

Table 2. Orthogonal experimental data for adsorption of Cr(Ⅵ) and Cu(Ⅱ) on PPy/CS composite membrane

Experiment number (Cr/Cu)	A/(mg·L⁻¹)	B/mg	C	D/min	q_e/(mg·g⁻¹)
1	2	20	2.5	40	0.375/0.860
2	2	25	3.0	50	0.484/0.756
3	2	30	3.5	60	0.347/0.630
4	4	20	3.0	60	1.100/1.870
5	4	25	3.5	40	0.980/1.524
6	4	30	2.5	50	0.820/1.280
7	6	20	3.5	50	1.380/2.715
8	6	25	2.5	60	1.160/2.236
9	6	30	3.0	40	0.830/1.857
R	0.721/1.520	0.286/0.559	0.117/0.164	0.167/0.170
Notes: A—Initial mass concentration; B—Dosage of PPy/CS composite membrane; C—pH value; D—Adsorption time; q_e—Adsorption quantity.

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表 3 PPy/CS复合膜吸附Cr(Ⅵ)、Cu(Ⅱ)的准一级和准二级动力学模型参数

Table 3. Pseudo-first-order and pseudo-second-order kinetic model parameters for adsorption of Cr(Ⅵ) and Cu(Ⅱ) on PPy/CS composite membrane

Heavy metal ion	q_e,exp/(mg·g⁻¹)	Pseudo-first-order			Pseudo-second-order
Heavy metal ion	q_e,exp/(mg·g⁻¹)	k₁/min⁻¹	q_e,cal/(mg·g⁻¹)	R²	k₂/(g(mg·min)⁻¹)	q_e,cal/(mg·g⁻¹)	R²
Cu(Ⅱ)	1.5060	0.046800	1.9890	0.96560	0.01776	1.9710	0.9982
Cr(Ⅵ)	0.8897	0.009850	0.1131	0.07187	1.61400	0.8249	0.9923
Notes: q_e,cal, q_e,exp—Adsorption amount at time t and adsorption equilibrium, respectively; k₁—Pseudo-first-order adsorption rate constant; k₂—Pseudo-second-order adsorption rate constant.

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表 4 PPy/CS复合膜吸附Cr(Ⅵ)和Cu(Ⅱ)的吸附等温线参数

Table 4. Adsorption isotherm parameters of PPy/CS composite membrane for Cr(Ⅵ) and Cu(Ⅱ) adsorption

Heavy metal ion	Langmuir equation				Freundlich equation
Heavy metal ion	Q/(mg·g⁻¹)	K_L/(L·mg⁻¹)	R_L	R²	K_f/(mg·g⁻¹)	1/n	R²
Cr(Ⅵ)	3.190	0.3731	0.4012	0.9919	0.8349	0.6164	0.9804
Cu(Ⅱ)	1.789	0.2504	0.4996	0.9971	0.3725	0.5966	0.9879
Notes: K_L is a constant related to adsorption energy; Q is the saturated adsorption capacity of monolayer adsorption; K_f is a constant related to the adsorption capacity; 1/n is a measure of the adsorption strength.

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表 5 PPy/CS复合膜与文献报道的各种吸附剂对Cu(II)和Cr(VI)吸附能力比较

Table 5. Comparison on Cu(II) and Cr(VI) adsorption capacity of PPy/CS composite membrane and various adsorbents reported in literature

Sample		m/g	c₀/ (mg·L⁻¹)	q_e/(mg·g⁻¹)	v/mL	Reference
PPy/CS	Cu(Ⅱ)/Cr(Ⅵ)	0.02	6	2.715/1.308	10	This work
Sulfonate PAN ENM	Cr(Ⅵ)	0.005	50	220.4	100	[40]
RA-5CS/PMAA	Cr(Ⅵ)	0.02	6.5	4.980	30	[41]
Bagasse before dialdehyde cellulose	Cu(Ⅱ)/Cr(Ⅵ)	0.5	50	2.185/0.457	25	[42]
Modified pectin-Fe₃O₄	Cu(Ⅱ)	0.02	500	105.0	10	[43]
Bt/Bc/α-Fe₂O₃	Cr(Ⅵ)	0.04	50	81.70	150	[44]
HEBC	Cu(Ⅱ)	0.05	40	11.98	50	[45]
ZM-CSt-PVA	Cu(Ⅱ)	0.1	2 000	199.0	100	[46]
GP-CTAB	Cr(Ⅵ)	0.02	50	95.30	50	[47]
SBA-15-SH	Cr(Ⅵ)	0.02	0.8	6.850	100	[48]
NMA-LDHs	Cr(Ⅵ)	0.05	100	103.4	100	[49]
Cedrus atlantica Manetti	Cu(Ⅱ)	2.2	200	14.23	400	[50]

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