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

doi:10.11949/0438-1157.20240492

摘要/Abstract

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。

关键词: 自由基, 响应面模型, 染料废水, 动力学, 降解

Abstract:

Dye wastewater has the characteristics of high chromaticity, complex composition, strong biological toxicity and difficult degradation. The Fe⁰/H₂O₂ system can efficiently remove refractory contaminants from dye wastewater because of its great oxidation capability, quick efficiency and low cost. In this study, the Fe⁰/H₂O₂ process was utilized to treat simulated dye wastewater and the response surface method was employed to optimize process conditions. Reactive free radicals were detected using electron paramagnetic resonance (EPR), and the degradation mechanism of dye wastewater was analyzed by comparing the changes in organic components before and after treatment using Fourier transform infrared spectroscopy (FT-IR) and ultraviolet visible light (UV-Vis). The changes of removal efficiencies of crystal violet, saffron T, TOC, COD and chroma in the dye wastewater were investigated. The degradation kinetics and degradation mechanisms of dye wastewater were explored. The results showed that the predicted removal efficiency of crystal violet using response surface method was 97.94%, which was only 0.36% (<2%) lower than the measured value, and the predicted removal efficiency of saffron T was 77.31%, which was only 1.3% (<2%) lower than the measured value, under the initial pH of 3, iron powder concentration of 0.3 g/L and H₂O₂ dosage of 20 mL/L. According to the kinetic study, the degradation processes of crystal violet, saffron T, COD and chroma were consistent with the BMG kinetic model. The correlation coefficient was higher than 0.98 and the initial degradation rate of crystal violet was the fastest. According to EPR analysis, ·OH was the main active substance for degradation of dye wastewater. According to FT-IR and UV-Vis spectroscopy, removal efficiencies of crystal violet and saffron T was the highest using the Fe⁰/H₂O₂ process, and the dye molecules were oxidized into small intermediates or small molecules; According to gas chromatography-mass spectrometry (GC-MS), the molecular structure of crystal violet and saffron T was destroyed by ·OH. The intermediate products were gradually degraded with the reaction, and finally decomposed into CO₂ and H₂O.

Key words: radical, response surface model, dye wastewater, kinetics, degradation

中图分类号:

X 523

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.

图/表 17

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编码	因素	单位	水平
编码	因素	单位	-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

编码	因素	单位	水平
编码	因素	单位	-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（%）
序号	A	B	C	结晶紫去除率（%）	藏红T去除率（%）
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

序号	变量取值			结晶紫去除率（%）	藏红T去除率（%）
序号	A	B	C	结晶紫去除率（%）	藏红T去除率（%）
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

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

Process conditions optimization of Fe⁰/H₂O₂ system using response surface method and study on the degradation mechanism of dye wastewater

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参考文献 45

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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

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）	R₁²	（mg·L^-1·min^-1）	R₂²	（min^-1）	1/b	R₃²
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
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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