• •
贾艳萍(), 马艳菊, 管文昕, 杨彬, 张健, 张兰河(
)
收稿日期:
2024-05-06
修回日期:
2024-07-04
出版日期:
2024-07-10
通讯作者:
张兰河
作者简介:
贾艳萍(1973-),女,博士,教授,jiayanping1111@sina.com
基金资助:
Yanping JIA(), Yanju MA, Wenxin GUAN, Bin YANG, Jian ZHANG, Lanhe ZHANG(
)
Received:
2024-05-06
Revised:
2024-07-04
Online:
2024-07-10
Contact:
Lanhe ZHANG
摘要:
染料废水具有色度大、成分复杂、生物毒性强和难降解的特点。Fe0/H2O2体系氧化能力强、快速高效、成本低廉,可有效去除染料废水中的难降解污染物。本研究采用Fe0/H2O2工艺处理染料废水,利用响应面法优化工艺运行条件,通过电子顺磁共振波谱仪(EPR)检测活性自由基,采用傅里叶红外光谱(FT-IR)和紫外-可见光谱(UV-Vis)分析染料废水处理前后有机物成分的变化,考察染料废水中结晶紫、藏红T、TOC、COD和色度的去除率变化,探究染料废水的降解动力学和降解机理。结果表明:在初始pH为3、Fe0浓度为0.3 g/L、H2O2投加量为20 mL/L的条件下,利用响应面法预测结晶紫去除率为97.94%,与实测值仅相差0.36%(<2%);藏红T去除率为77.31%,与实测值仅相差1.3%(<2%)。由动力学分析可知:结晶紫、藏红T、COD和色度的降解过程符合BMG动力学模型,相关系数大于0.98,结晶紫的初始降解速率最快。由EPR分析可知:·OH为Fe0/H2O2降解染料废水的主要活性物种;通过FTIR和UV-Vis检测分析可知:Fe0/H2O2工艺对结晶紫和藏红T的去除效果最好,染料分子被氧化成分子量小的中间体或小分子物质;由气相色谱-质谱(GC-MS)分析可知:结晶紫与藏红T分子结构被·OH破坏,随着反应的进行,产生的中间产物逐渐被降解,最终分解为CO2和H2O。
中图分类号:
贾艳萍, 马艳菊, 管文昕, 杨彬, 张健, 张兰河. 响应面法优化Fe0/H2O2体系降解染料废水的工艺条件及机理研究[J]. 化工学报, DOI: 10.11949/0438-1157.20240492.
Yanping JIA, Yanju MA, Wenxin GUAN, Bin YANG, Jian ZHANG, Lanhe ZHANG. Process conditions optimization of Fe0/H2O2 system using response surface method and study on the degradation mechanism of dye wastewater[J]. CIESC Journal, DOI: 10.11949/0438-1157.20240492.
编码 | 因素 | 单位 | 水平 | ||
---|---|---|---|---|---|
-1 | 0 | 1 | |||
A | 初始pH值 | - | 2 | 3 | 4 |
B | Fe0浓度 | mg/L | 0.2 | 0.3 | 0.4 |
C | H2O2投加量 | ml/L | 15 | 20 | 25 |
表1 响应面实验因素和水平设计表
Table 1 The experimental factors and level design table for response surface
编码 | 因素 | 单位 | 水平 | ||
---|---|---|---|---|---|
-1 | 0 | 1 | |||
A | 初始pH值 | - | 2 | 3 | 4 |
B | Fe0浓度 | mg/L | 0.2 | 0.3 | 0.4 |
C | H2O2投加量 | ml/L | 15 | 20 | 25 |
序号 | 变量取值 | 结晶紫去除率(%) | 藏红T去除率(%) | ||
---|---|---|---|---|---|
A | B | C | |||
1 | -1 | -1 | 0 | 94.96 | 57.45 |
2 | 1 | -1 | 0 | 95.83 | 66.28 |
3 | -1 | 1 | 0 | 96.95 | 48.35 |
4 | 1 | 1 | 0 | 91.03 | 67.84 |
5 | -1 | 0 | -1 | 96.85 | 52.83 |
6 | 1 | 0 | -1 | 94.75 | 59.75 |
7 | -1 | 0 | 1 | 96.56 | 51.63 |
8 | 1 | 0 | 1 | 94.19 | 67.68 |
9 | 0 | -1 | -1 | 92.05 | 62.84 |
10 | 0 | 1 | -1 | 95.10 | 60.18 |
11 | 0 | -1 | 1 | 96.31 | 72.11 |
12 | 0 | 1 | 1 | 91.95 | 64.81 |
13 | 0 | 0 | 0 | 98.07 | 78.14 |
14 | 0 | 0 | 0 | 98.34 | 78.57 |
15 | 0 | 0 | 0 | 97.92 | 77.85 |
16 | 0 | 0 | 0 | 97.86 | 76.85 |
17 | 0 | 0 | 0 | 97.50 | 75.15 |
表2 响应面实验组设计及实验结果
Table 2 Experiment design and experimental results of response surface test group
序号 | 变量取值 | 结晶紫去除率(%) | 藏红T去除率(%) | ||
---|---|---|---|---|---|
A | B | C | |||
1 | -1 | -1 | 0 | 94.96 | 57.45 |
2 | 1 | -1 | 0 | 95.83 | 66.28 |
3 | -1 | 1 | 0 | 96.95 | 48.35 |
4 | 1 | 1 | 0 | 91.03 | 67.84 |
5 | -1 | 0 | -1 | 96.85 | 52.83 |
6 | 1 | 0 | -1 | 94.75 | 59.75 |
7 | -1 | 0 | 1 | 96.56 | 51.63 |
8 | 1 | 0 | 1 | 94.19 | 67.68 |
9 | 0 | -1 | -1 | 92.05 | 62.84 |
10 | 0 | 1 | -1 | 95.10 | 60.18 |
11 | 0 | -1 | 1 | 96.31 | 72.11 |
12 | 0 | 1 | 1 | 91.95 | 64.81 |
13 | 0 | 0 | 0 | 98.07 | 78.14 |
14 | 0 | 0 | 0 | 98.34 | 78.57 |
15 | 0 | 0 | 0 | 97.92 | 77.85 |
16 | 0 | 0 | 0 | 97.86 | 76.85 |
17 | 0 | 0 | 0 | 97.50 | 75.15 |
变差来源 | 平方和 | 自由度 | 均方和 | F值 | P值 | 显著性 |
---|---|---|---|---|---|---|
模型 | 81.51 | 9 | 9.06 | 53.69 | <0.0001 | 极显著 |
A | 11.33 | 1 | 11.33 | 67.16 | <0.0001 | 极显著 |
B | 2.12 | 1 | 2.12 | 12.58 | 0.0094 | 显著 |
C | 0.0085 | 1 | 0.0085 | 0.0501 | 0.8293 | 不显著 |
AB | 11.53 | 1 | 11.53 | 68.33 | <0.0001 | 极显著 |
AC | 0.0182 | 1 | 0.0182 | 0.1080 | 0.7520 | 不显著 |
BC | 13.73 | 1 | 13.73 | 81.38 | <0.0001 | 显著 |
A2 | 2.40 | 1 | 2.40 | 14.24 | 0.0070 | 显著 |
B2 | 26.11 | 1 | 26.11 | 154.79 | <0.0001 | 极显著 |
C2 | 10.72 | 1 | 10.72 | 63.52 | <0.0001 | 极显著 |
残差 | 1.18 | 7 | 0.1687 | |||
失拟项 | 0.8035 | 3 | 0.2678 | 2.84 | 0.1696 | 不显著 |
误差 | 0.3773 | 4 | 0.0943 | |||
合计 | 82.69 | 16 | ||||
标准偏差 | 0.4107 | 相关系数 | 0.9857 | |||
平均值 | 95.66 | 校正决定系数 | 0.9674 | |||
变异系数 | 0.4293 | 预测相关系数 | 0.8374 | |||
信噪比 | 21.1047 |
表3 结晶紫去除率模型方差分析
Table 3 Variance analysis of crystal violet removal efficiency model
变差来源 | 平方和 | 自由度 | 均方和 | F值 | P值 | 显著性 |
---|---|---|---|---|---|---|
模型 | 81.51 | 9 | 9.06 | 53.69 | <0.0001 | 极显著 |
A | 11.33 | 1 | 11.33 | 67.16 | <0.0001 | 极显著 |
B | 2.12 | 1 | 2.12 | 12.58 | 0.0094 | 显著 |
C | 0.0085 | 1 | 0.0085 | 0.0501 | 0.8293 | 不显著 |
AB | 11.53 | 1 | 11.53 | 68.33 | <0.0001 | 极显著 |
AC | 0.0182 | 1 | 0.0182 | 0.1080 | 0.7520 | 不显著 |
BC | 13.73 | 1 | 13.73 | 81.38 | <0.0001 | 显著 |
A2 | 2.40 | 1 | 2.40 | 14.24 | 0.0070 | 显著 |
B2 | 26.11 | 1 | 26.11 | 154.79 | <0.0001 | 极显著 |
C2 | 10.72 | 1 | 10.72 | 63.52 | <0.0001 | 极显著 |
残差 | 1.18 | 7 | 0.1687 | |||
失拟项 | 0.8035 | 3 | 0.2678 | 2.84 | 0.1696 | 不显著 |
误差 | 0.3773 | 4 | 0.0943 | |||
合计 | 82.69 | 16 | ||||
标准偏差 | 0.4107 | 相关系数 | 0.9857 | |||
平均值 | 95.66 | 校正决定系数 | 0.9674 | |||
变异系数 | 0.4293 | 预测相关系数 | 0.8374 | |||
信噪比 | 21.1047 |
变差来源 | 平方和 | 自由度 | 均方和 | F值 | P值 | 显著性 |
---|---|---|---|---|---|---|
模型 | 1520.80 | 9 | 168.98 | 65.06 | <0.0001 | 极显著 |
A | 328.83 | 1 | 328.83 | 126.60 | <0.0001 | 极显著 |
B | 38.28 | 1 | 38.28 | 14.74 | 0.0064 | 显著 |
C | 53.20 | 1 | 53.20 | 20.48 | 0.0027 | 显著 |
AB | 28.41 | 1 | 28.41 | 10.94 | 0.0130 | 显著 |
AC | 20.84 | 1 | 20.84 | 8.02 | 0.0253 | 显著 |
BC | 5.38 | 1 | 5.38 | 2.07 | 0.1932 | 不显著 |
A2 | 623.85 | 1 | 623.85 | 240.19 | <0.0001 | 极显著 |
B2 | 112.10 | 1 | 112.10 | 43.16 | 0.0003 | 显著 |
C2 | 216.29 | 1 | 216.29 | 83.28 | <0.0001 | 极显著 |
残差 | 18.18 | 7 | 2.60 | |||
失拟项 | 10.74 | 3 | 3.58 | 1.92 | 0.2675 | 不显著 |
误差 | 7.45 | 4 | 1.86 | |||
合计 | 1538.98 | 16 | ||||
标准偏差 | 1.61 | 相关系数 | 0.9882 | |||
平均值 | 65.78 | 校正决定系数 | 0.9730 | |||
变异系数 | 2.45 | 预测相关系数 | 0.8808 | |||
信噪比 | 23.1347 |
表4 藏红T去除率模型方差分析
Table 4 Variance analysis of saffron T removal efficiency model
变差来源 | 平方和 | 自由度 | 均方和 | F值 | P值 | 显著性 |
---|---|---|---|---|---|---|
模型 | 1520.80 | 9 | 168.98 | 65.06 | <0.0001 | 极显著 |
A | 328.83 | 1 | 328.83 | 126.60 | <0.0001 | 极显著 |
B | 38.28 | 1 | 38.28 | 14.74 | 0.0064 | 显著 |
C | 53.20 | 1 | 53.20 | 20.48 | 0.0027 | 显著 |
AB | 28.41 | 1 | 28.41 | 10.94 | 0.0130 | 显著 |
AC | 20.84 | 1 | 20.84 | 8.02 | 0.0253 | 显著 |
BC | 5.38 | 1 | 5.38 | 2.07 | 0.1932 | 不显著 |
A2 | 623.85 | 1 | 623.85 | 240.19 | <0.0001 | 极显著 |
B2 | 112.10 | 1 | 112.10 | 43.16 | 0.0003 | 显著 |
C2 | 216.29 | 1 | 216.29 | 83.28 | <0.0001 | 极显著 |
残差 | 18.18 | 7 | 2.60 | |||
失拟项 | 10.74 | 3 | 3.58 | 1.92 | 0.2675 | 不显著 |
误差 | 7.45 | 4 | 1.86 | |||
合计 | 1538.98 | 16 | ||||
标准偏差 | 1.61 | 相关系数 | 0.9882 | |||
平均值 | 65.78 | 校正决定系数 | 0.9730 | |||
变异系数 | 2.45 | 预测相关系数 | 0.8808 | |||
信噪比 | 23.1347 |
图6 不同因素对结晶紫与藏红T去除率影响的响应面三维图和等高线图
Fig. 6 Three-dimensional graph and contour map of the response surface affected by different factors on the removal efficiency of crystal violet and saffron T
污染物 | 一级动力学方程 | 二级动力学方程 | BMG动力学方程 | ||||
---|---|---|---|---|---|---|---|
k1 | R12 | k2 | R22 | 1/m | 1/b | R32 | |
(min-1) | (mg·L-1·min-1) | (min-1) | |||||
结晶紫 | 0.00754 | 0.98256 | 0.00303 | 0.93845 | 0.27635 | 0.9851 | 0.99977 |
藏红T | 0.00318 | 0.96553 | 4.62E-05 | 0.98636 | 0.00638 | 0.7637 | 0.99290 |
表5 不同污染物降解动力学的拟合结果
Table 5 The fitting results of degradation kinetic of different pollutants
污染物 | 一级动力学方程 | 二级动力学方程 | BMG动力学方程 | ||||
---|---|---|---|---|---|---|---|
k1 | R12 | k2 | R22 | 1/m | 1/b | R32 | |
(min-1) | (mg·L-1·min-1) | (min-1) | |||||
结晶紫 | 0.00754 | 0.98256 | 0.00303 | 0.93845 | 0.27635 | 0.9851 | 0.99977 |
藏红T | 0.00318 | 0.96553 | 4.62E-05 | 0.98636 | 0.00638 | 0.7637 | 0.99290 |
产物 | 保留时间/min | m/z | 分子式 | 分子结构 |
---|---|---|---|---|
1 | 3.815 | 94 | C6H6O | ![]() |
2 | 4.330 | 93 | C6H7N | ![]() |
3 | 5.771 | 287 | C18H15N4 | ![]() |
4 | 6.033 | 166 | C6H14O5 | ![]() |
5 | 7.360 | 142.5 | C6H7ClN2 | ![]() |
6 | 9.615 | 165 | C9H11O2N | ![]() |
7 | 11.350 | 184 | C12H12N2 | ![]() |
8 | 13.540 | 137 | C8H11ON | ![]() |
9 | 14.556 | 134.5 | C6H11OCl | ![]() |
10 | 15.627 | 112.5 | C6H5Cl | ![]() |
11 | 16.055 | 137 | C7H7O2N | ![]() |
12 | 17.645 | 109 | C6H7ON | ![]() |
13 | 21.830 | 121 | C8H11N | ![]() |
14 | 22.048 | 268 | C17H20ON2 | ![]() |
15 | 27.895 | 72 | C3H4O2 | ![]() |
表6 结晶紫与藏红T降解过程的中间产物
Table 6 Intermediate products in the degradation process of crystal violet and saffron T
产物 | 保留时间/min | m/z | 分子式 | 分子结构 |
---|---|---|---|---|
1 | 3.815 | 94 | C6H6O | ![]() |
2 | 4.330 | 93 | C6H7N | ![]() |
3 | 5.771 | 287 | C18H15N4 | ![]() |
4 | 6.033 | 166 | C6H14O5 | ![]() |
5 | 7.360 | 142.5 | C6H7ClN2 | ![]() |
6 | 9.615 | 165 | C9H11O2N | ![]() |
7 | 11.350 | 184 | C12H12N2 | ![]() |
8 | 13.540 | 137 | C8H11ON | ![]() |
9 | 14.556 | 134.5 | C6H11OCl | ![]() |
10 | 15.627 | 112.5 | C6H5Cl | ![]() |
11 | 16.055 | 137 | C7H7O2N | ![]() |
12 | 17.645 | 109 | C6H7ON | ![]() |
13 | 21.830 | 121 | C8H11N | ![]() |
14 | 22.048 | 268 | C17H20ON2 | ![]() |
15 | 27.895 | 72 | C3H4O2 | ![]() |
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