基于响应面法的粉煤灰氨含量测定过程浸提条件优化研究

doi:10.19964/j.issn.1006-4990.2021-0345

Abstract

Abstract:

For the research on determination of ammonia content in fly ash,a single factor is mostly considered,but the influence of the interaction of various factors on the extraction of the ammonia content of fly ash during the extraction process is ignored.In this study,the extractant concentration（A）,solid-to-liquid ratio（B）,and oscillation time（C） were used as investigating factors,and a response surface test was conducted on the basis of single factor test to establish a regression model.The optimal extraction process was determined through response surface optimization and compared with the measurement results of existing extraction methods.The results showed that the order of influencing factors was B、A、C、AB、BC、AC.The best extraction process was extractant concentration of 0.125 mol/L,solid-liquid ratio （g/mL） of 1∶12.8,the oscillation time of 22 s.Through verification,it was found that there was only a relative error of -2% between the measured value and the predicted value.Compared with the existing extraction method,the optimized extraction method not only greatly shortened the extraction time,but also increased the extraction rate by 73% to 91%,which provided a new method and idea for the accurate determination of ammonia content in fly ash.

Key words: fly ash, ammonia determination, extraction, interaction, BBD response surface methodology

CLC Number:

TQ536.4

LI Yajiao,ZHAO Yiwei,JU Kai,TANG Renlong,LI Longqing,SHAO Xiaoping,ZHANG Gaofeng,REN Wuang. Study on optimization of extraction conditions in process of determination of ammonia content in fly ash based on response surface method[J]. Inorganic Chemicals Industry, 2022, 54(4): 145-151.

Figures/Tables 13

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References 28

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水平	因素
水平	A 浸提剂浓度/ （mol·L^-1）	B 固液比	C 振荡时间/ s
-1	0.075	1∶5	15
0	0.1	1∶10	20
1	0.125	1∶15	25

实验组别	A	B	C	η/（mg·kg^-1）
1	0.075	1∶5	20	60.125
2	0.125	1∶5	20	89.500
3	0.075	1∶15	20	129.000
4	0.125	1∶15	20	191.625
5	0.075	1∶10	15	112.500
6	0.125	1∶10	15	170.250
7	0.075	1∶10	25	138.000
8	0.125	1∶10	25	176.750
9	0.100	1∶5	15	64.625
10	0.100	1∶15	15	128.000
11	0.100	1∶5	25	76.000
12	0.100	1∶15	25	169.125
13	0.100	1∶10	20	176.750
14	0.100	1∶10	20	183.250
15	0.100	1∶10	20	181.000
16	0.100	1∶10	20	165.000
17	0.100	1∶10	20	150.500

来源	R² 校正值	R² 预测值	备注
线性模型	0.510 2	0.352 0
2F1模型	0.393 5	-0.178 3
二次模型	0.939 8	0.921 1	建议采用
三次模型	0.905 1

方差来源	平方和	自由度	均方	F 值	P 值	显著性
模型	30 309.98	9	3 367.78	28.74	0.000 1	显著
A	4 441.53	1	4 441.53	37.9	0.000 5
B	13 407.03	1	13 407.03	114.41	<0.000 1
C	892.53	1	892.53	7.62	0.028 1
AB	276.39	1	276.39	2.36	0.168 5
AC	90.25	1	90.25	0.77	0.409 3
BC	221.27	1	221.27	1.89	0.211 8
A²	200.46	1	200.46	1.71	0.232 2
B²	9 236.85	1	9 236.85	78.83	<0.000 1
C²	950.53	1	950.53	8.11	0.024 8
残差	820.27	7	117.18
失拟差	81.34	3	27.11	0.15	0.926 6	不显著
净误差	738.93	4	184.73
总差	31 130.25	16

浸提方法	浸提工艺条件			备注	氨含量/ （mg·kg^-1）
浸提方法	浸提剂	固液比	时间/ s	备注	氨含量/ （mg·kg^-1）
搅拌^[26]	（1+20）盐酸	1∶10	300	滤液中加入NaOH 溶液调pH至6~7	50
振荡^[14]	0.05 mol/L 硫酸	1∶10	1 800		10.75
振荡^[15]	0.05 mol/L 硫酸	1∶10	1 800	加入掩蔽剂后加 1.5 mL NaOH溶液	13.25
振荡（本研究）	0.125 mol/L 硫酸	1∶12.8	22		197.7

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Inorganic Acid-Base-Salt Committee of CIESC

Study on optimization of extraction conditions in process of determination of ammonia content in fly ash based on response surface method

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