新型除磷填料的制备及除磷吸附床运行参数的优化

doi:10.11949/j.issn.0438-1157.20181054

化工学报 ›› 2019, Vol. 70 ›› Issue (3): 1099-1110.DOI: 10.11949/j.issn.0438-1157.20181054

新型除磷填料的制备及除磷吸附床运行参数的优化

张千¹(),刘向阳¹,陈旺¹,吴恒¹,肖芃颖¹,吉芳英²,李宸³,念海明³

1. 重庆理工大学化学化工学院，重庆 400054
2. 重庆大学三峡库区生态环境教育部重点实验室，重庆 400045
3. 重庆川仪环境科技有限公司，重庆 401121

收稿日期:2018-09-19 修回日期:2018-11-07 出版日期:2019-03-05 发布日期:2019-03-05
通讯作者: 张千
作者简介:及第一作者：张千（1986—），男，博士研究生，讲师，<email>zhangqianswu2005@163.com</email>
基金资助:
国家自然科学基金项目(51708077);重庆市社会事业与民生保障科技创新专项(cstc2018jscx-msybX0134)

Preparation of a novel phosphorus removal filler and optimization of phosphate removal adsorption bed process

Qian ZHANG¹(),Xiangyang LIU¹,Wang CHEN¹,Heng WU¹,Pengying XIAO¹,Fangying JI²,Chen LI³,Haiming NIAN³

1. School of Chemical Engineering, Chongqing University of Technology, Chongqing 400054, China
2. Key Laboratory of Three Gorges Reservoir Region’s Eco-Environment, Ministry of Education, Chongqing University, Chongqing 400045, China
3. Chongqing Chuanyi Environmental Technology Co., Ltd., Chongqing 401121, China

Received:2018-09-19 Revised:2018-11-07 Online:2019-03-05 Published:2019-03-05
Contact: Qian ZHANG

摘要/Abstract

摘要：

为解决现有除磷吸附剂粒径小造成的材料易流失和系统压降过大等问题，以实现吸附除磷工艺在实际工程中的应用，以聚氨酯填料为载体，水溶性聚氨酯为介质，将水化硅酸钙负载到聚氨酯填料上制成负载型除磷填料。研究了制备条件对除磷填料除磷效果的影响，采用扫描电子显微镜（SEM）和傅里叶变换红外光谱仪（FTIR）观察分析了负载前后水化硅酸钙微观结构及化学基团的变化；利用除磷填料作为除磷吸附床的滤料，研究了运行条件对吸附床除磷效果的影响。在此基础上，利用响应曲面法研究了除磷吸附床磷酸盐去除率和各变量之间的关系，并对工艺参数进行了优化。结果表明，水性聚氨酯溶液的浓度和用量分别为100 g/L和50 ml，水化硅酸钙的质量为12 g的条件下所制备的除磷填料除磷效果最好；SEM和FTIR分析结果显示，水化硅酸钙负载前后其孔隙结构和化学基团没有明显的变化；预测模型的方差分析结果表明，HRT(X ₁)、进水ρ(PO₄ ^3--P)(X ₂)、温度(X ₃)、初始pH(X ₄)以及X ₁ X ₂，X ₁ X ₄，X ₂ X ₃，X ₂ X ₄的交互作用均对磷酸盐的去除具有显著影响 (P＜0.05)，但X ₁ X ₃的交互作用对磷酸盐的去除影响不显著。通过预测模型获得的最佳运行条件为：HRT为79.77 min，进水ρ(PO₄ ^3--P)为1.70 mg/L, 温度为34.04℃，pH为9.68。在该条件下，反应器对磷酸盐的去除率可以达到93.46%。

关键词: 新型除磷填料, 除磷吸附床, 响应曲面法, 运行参数优化

Abstract:

To solve the problems of easy loss of materials and excessive system pressure drop caused by the small particle size of the existing phosphorus removal adsorbent, the application of the adsorption phosphorus removal process in practical engineering is realized. In this study, polyurethane filler was used as carrier, water-soluble polyurethane was used as medium, and hydrated calcium silicate was loaded onto polyurethane filler to make supported phosphorus removal filler. Effect of prepared methods on phosphate removal efficiency of the phosphorus removal filler was studied to obtain the optimum preparation conditions. The change of microstructure and chemical groups of hydrated calcium silicate before and after loading onto polyurethane carriers was revealed by scanning electron microscope (SEM) and Fourier transform infrared spectrometer (FTIR). Effect of operation parameters on phosphate removal efficiency of adsorption bed using phosphorus removal filler as packing materials was investigated through single factor experiment. Based on the results obtained from the single factor experiment, an ideal experimental design was carried out based on central composite design (CCD) with response surface methodology (RSM). The results showed that, the optimum conditions for the preparation of phosphorus removal filler were 50 ml waterborne polyurethane with concentration of 100 g/L, and the hydrated calcium silicate dosage of 12 g. SEM and FTIR observations showed that the pore structure and the chemical groups of hydrated calcium silicate changed slightly after loading onto the filler. The variance analysis of the predication model indicated that HRT(X ₁), influent ρ (PO₄ ^3--P)(X ₂), temperature(X ₃), initial pH(X ₄) and the interaction between X ₁ X ₂, X ₁ X ₄, X ₂ X ₃ and X ₂ X ₄ had significant influence on the response value(P<0.05) while the interaction between X ₁ X ₃ had non-significant impacts on the response value. The optimum conditions obtained were HRT 79.77 min, influent ρ(PO₄ ^3--P) 1.70 mg/L, temperature 34.04℃ and initial pH 9.68. Under the optimized conditions, the phosphate removal efficiency of the adsorption bed was found to be 93.46%.

Key words: novel phosphorus removal filler, phosphate removal adsorption bed, response surface methodology (RSM), process optimization

中图分类号:

X 52

张千, 刘向阳, 陈旺, 吴恒, 肖芃颖, 吉芳英, 李宸, 念海明. 新型除磷填料的制备及除磷吸附床运行参数的优化[J]. 化工学报, 2019, 70(3): 1099-1110.

Qian ZHANG, Xiangyang LIU, Wang CHEN, Heng WU, Pengying XIAO, Fangying JI, Chen LI, Haiming NIAN. Preparation of a novel phosphorus removal filler and optimization of phosphate removal adsorption bed process[J]. CIESC Journal, 2019, 70(3): 1099-1110.

图/表 13

图1 试验装置示意图

Fig.1 Scheme of experimental device

表1 单因素试验中的运行参数

Table 1 Operation parameters in each single factor experiment

Factor	Level
Factor	HRT/min	Influent ρ( $P O 4 3 -$ -P)/(mg/L)	Tempera-ture/℃	Initial pH
HRT/min	40—90	6	30	9
influent ρ( $P O 4 3 -$ -P)/(mg/L)	70	0.5—2.5	30	9
temperature/℃	70	6	17—40	9
initial pH	70	6	30	6—11

表1 单因素试验中的运行参数

Table 1 Operation parameters in each single factor experiment

Factor	Level
Factor	HRT/min	Influent ρ( $P O 4 3 -$ -P)/(mg/L)	Tempera-ture/℃	Initial pH
HRT/min	40—90	6	30	9
influent ρ( $P O 4 3 -$ -P)/(mg/L)	70	0.5—2.5	30	9
temperature/℃	70	6	17—40	9
initial pH	70	6	30	6—11

表2 响应曲面模型的变量及其范围

Table 2 Variables and corresponding range of response surface methodology model

Code	Variable	Code level
Code	Variable	-α	-1	0	1	+α
X ₁	HRT/min	50	60	70	80	90
X ₂	influent ρ( $P O 4 3 -$ -P)/(mg/L)	0.5	1	1.5	2	2.5
X ₃	temperature/℃	16	23	30	37	44
X ₄	initial pH	7	8	9	10	11

表2 响应曲面模型的变量及其范围

Table 2 Variables and corresponding range of response surface methodology model

Code	Variable	Code level
Code	Variable	-α	-1	0	1	+α
X ₁	HRT/min	50	60	70	80	90
X ₂	influent ρ( $P O 4 3 -$ -P)/(mg/L)	0.5	1	1.5	2	2.5
X ₃	temperature/℃	16	23	30	37	44
X ₄	initial pH	7	8	9	10	11

表3 制备除磷填料的正交试验结果

Table 3 Orthogonal test results of phosphorus removal filter

Sample	ρ(waterborne polyurethane)/(g/L)	Volume of waterborne polyurethane/ ml	Dosage of hydrated calcium silicate/g	Phosphate removal rate/%
1	100	50	4	95.7
2	100	100	8	96.6
3	100	150	12	97.9
4	100	200	16	98.3
5	200	50	8	95.9
6	200	100	4	91.5
7	200	150	16	97.6
8	200	200	12	96.6
9	300	50	12	99.6
10	300	100	16	99.2
11	300	150	4	72.2
12	300	200	8	88.0
13	400	50	16	91.6
14	400	100	12	92.8
15	400	150	8	74.7
16	400	200	4	44.1
K ₁	388.5	382.8	303.5
K ₂	381.6	380.1	355.2
K ₃	359.0	342.4	386.9
K ₄	303.2	327	386.7
k ₁	97.1	95.7	75.9
k ₂	95.4	95.0	88.8
k ₃	89.8	85.6	96.7
k ₄	75.8	81.8	96.7
R	21.3	13.9	20.8
major-minor order of test factor		A>C>B
optimal level	A1	B1	C3
optimal combination		A1B1C3

图2 除磷填料和水化硅酸钙静态除磷效果对比

Fig.2 Comparison of phosphorus removal efficiency between hydrated calcium silicate and phosphorus removal filler

图3 水化硅酸钙与填料上负载的水化硅酸钙的SEM照片

Fig.3 SEM images of calcium silicate and calcium silicate supported on filter

图4 水化硅酸钙负载前后的红外测试谱图

Fig.4 Infrared spectra of calcium silicate hydrate before and after loading on carrier

图5 运行参数对除磷吸附床除磷效果的影响

Fig.5 Influence of operation parameters on phosphorus removal performance of phosphorus removal adsorption bed

表4 中心复合设计与试验结果

Table 4 Factors and levels for central composite design

Standard order	X ₁	X ₂	X ₃	X ₄	$P O 4 3 -$ -P removal efficiency /%
Standard order	X ₁	X ₂	X ₃	X ₄	Measured value	Predicted value
22	70	1.5	44	9	91.00	90.37
17	50	1.5	30	9	78.12	78.79
8	80	2	37	8	88.84	89.47
5	60	1	37	8	86.58	85.90
9	60	1	23	10	85.87	85.23
2	80	1	23	8	86.82	86.90
18	90	1.5	30	9	92.48	91.31
16	80	2	37	10	92.59	92.73
3	60	2	23	8	73.58	72.73
12	80	2	23	10	88.94	89.61
24	70	1.5	30	11	91.12	90.85
19	70	0.5	30	9	86.02	85.54
28	70	1.5	30	9	91.02	91.01
25	70	1.5	30	9	91.01	91.01
13	60	1	37	10	88.99	89.76
14	80	1	37	10	88.59	88.67
7	60	2	37	8	78.54	79.26
30	70	1.5	30	9	90.95	91.01
23	70	1.5	30	7	83.96	83.73
10	80	1	23	10	86.99	87.54
1	60	1	23	8	80.99	81.37
4	80	2	23	8	86.59	86.34
6	80	1	37	8	87.09	88.03
27	70	1.5	30	9	91.03	91.01
29	70	1.5	30	9	91.02	91.01
21	70	1.5	16	9	82.59	82.71
26	70	1.5	30	9	91.00	91.01
20	70	2.5	30	9	80.99	80.97
15	60	2	37	10	86.59	85.75
11	60	2	23	10	78.89	79.22

表4 中心复合设计与试验结果

Table 4 Factors and levels for central composite design

Standard order	X ₁	X ₂	X ₃	X ₄	$P O 4 3 -$ -P removal efficiency /%
Standard order	X ₁	X ₂	X ₃	X ₄	Measured value	Predicted value
22	70	1.5	44	9	91.00	90.37
17	50	1.5	30	9	78.12	78.79
8	80	2	37	8	88.84	89.47
5	60	1	37	8	86.58	85.90
9	60	1	23	10	85.87	85.23
2	80	1	23	8	86.82	86.90
18	90	1.5	30	9	92.48	91.31
16	80	2	37	10	92.59	92.73
3	60	2	23	8	73.58	72.73
12	80	2	23	10	88.94	89.61
24	70	1.5	30	11	91.12	90.85
19	70	0.5	30	9	86.02	85.54
28	70	1.5	30	9	91.02	91.01
25	70	1.5	30	9	91.01	91.01
13	60	1	37	10	88.99	89.76
14	80	1	37	10	88.59	88.67
7	60	2	37	8	78.54	79.26
30	70	1.5	30	9	90.95	91.01
23	70	1.5	30	7	83.96	83.73
10	80	1	23	10	86.99	87.54
1	60	1	23	8	80.99	81.37
4	80	2	23	8	86.59	86.34
6	80	1	37	8	87.09	88.03
27	70	1.5	30	9	91.03	91.01
29	70	1.5	30	9	91.02	91.01
21	70	1.5	16	9	82.59	82.71
26	70	1.5	30	9	91.00	91.01
20	70	2.5	30	9	80.99	80.97
15	60	2	37	10	86.59	85.75
11	60	2	23	10	78.89	79.22

表5 回归模型的方差分析

Table 5 Analysis of variance(ANOVA) for regression model

Source	Sum of squares	df	Mean square	F value	P value
Model	691.57	13	53.20	101.47	<0.0001
X ₁	235.25	1	235.25	448.70	<0.0001
X ₂	31.33	1	31.33	59.75	<0.0001
X ₃	88.01	1	88.01	167.87	<0.0001
X ₄	76.11	1	76.11	145.17	<0.0001
X ₁ X ₂	65.21	1	65.21	124.37	<0.0001
X ₁ X ₃	11.56	1	11.56	22.05	0.0002
X ₁ X ₄	10.37	1	10.37	19.78	0.0004
X ₂ X ₃	3.98	1	3.98	7.59	0.0141
X ₂ X ₄	6.89	1	6.89	13.14	0.0023
X ₁ ²	60.86	1	60.86	116.08	<0.0001
X ₂ ²	103.05	1	103.05	196.56	<0.0001
X ₃ ²	34.15	1	34.15	65.14	<0.0001
X ₄ ²	23.70	1	23.70	45.21	<0.0001
residual	8.39	16	0.52
lack of fit	8.38	11	0.76	918.35	<0.0001
pure error	4.150×10^-3	5	8.300×10^-4

图6 HRT、进水 P O 4 3 - -P浓度、温度以及初始pH之间的交互效应对磷酸盐去除率影响的等高线图和响应曲面图

Fig.6 Contour and response surface plots for interaction effects of HRT, influent P O 4 3 - -P concentration, temperature and initial pH on phosphate removal efficiency

表6 磷酸盐去除率的优化结果

Table 6 Optimization results for phosphate maximum removal efficiency

Solution No.	HRT/min	Influent ρ( $P O 4 3 -$ -P)/(mg/L)	Temperature/℃	Initial pH	Phosphate removal efficiency/%	Desirability
1	79.77	1.70	34.04	9.68	93.46	1.000
2	79.75	1.70	33.98	9.68	93.4579	1.000
3	79.90	1.70	34.01	9.67	93.4578	1.000
4	79.97	1.71	34.01	9.67	93.4576	1.000
5	79.48	1.70	34.15	9.69	93.4573	1.000
6	76.75	1.70	33.87	9.69	93.4572	1.000
7	80.00	1.69	32.80	9.59	93.4221	0.998
8	80.00	1.70	33.80	9.27	93.3107	0.992

表6 磷酸盐去除率的优化结果

Table 6 Optimization results for phosphate maximum removal efficiency

Solution No.	HRT/min	Influent ρ( $P O 4 3 -$ -P)/(mg/L)	Temperature/℃	Initial pH	Phosphate removal efficiency/%	Desirability
1	79.77	1.70	34.04	9.68	93.46	1.000
2	79.75	1.70	33.98	9.68	93.4579	1.000
3	79.90	1.70	34.01	9.67	93.4578	1.000
4	79.97	1.71	34.01	9.67	93.4576	1.000
5	79.48	1.70	34.15	9.69	93.4573	1.000
6	76.75	1.70	33.87	9.69	93.4572	1.000
7	80.00	1.69	32.80	9.59	93.4221	0.998
8	80.00	1.70	33.80	9.27	93.3107	0.992

图7 除磷吸附床持续运行的除磷效果

Fig.7 Phosphate removal performance of adsorption bed during continuous operation

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新型除磷填料的制备及除磷吸附床运行参数的优化

Preparation of a novel phosphorus removal filler and optimization of phosphate removal adsorption bed process

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