Optimization of reactive extraction-crystallization process based on response surface methodology

doi:10.11949/j.issn.0438-1157.20151171

Abstract

Abstract:

The preparation of calcium carbonate and hydrogen chloride from calcium chloride and carbon dioxide by the reactive extraction-crystallization coupled process is an effective way for the utilization of alkaline waste liquid. In this paper, Box-Behnken Design (BBD) in response surface methodology was used to design the experiments to investigate the effects of concentration of calcium chloride (CaCl₂), volume fraction of extractant, phase ratio, and temperature on the conversion of CaCl₂, concentration of hydrogen chloride (HCl) in organic phase, and the average particle size of calcium carbonate (CaCO₃) in the reactive extraction-crystallization coupled process, respectively. Three quadratic models were developed to correlate the variables to the response values and were proved to be significant. The optimal values were found as follows: conversion of CaCl₂ 95.08% and 92.35%, concentration of HCl in organic phase 1.126 mol·L^-1 and 1.123 mol·L^-1, and average particle size of CaCO₃ 48.71 μm and 49.14 μm. The small errors between the predicted and experimental values showed that the established models were accurate and reliable for the analysis and prediction of the reactive extractioncrystallization process.

Key words: wastewater treatment, crystallization, solvent extraction, response surface methodology, process optimization

摘要：

氯化钙与二氧化碳通过反应-萃取-结晶工艺制备碳酸钙和氯化氢气体是制碱废液资源化利用的有效途径。用响应曲面中的Box-Behnken Design(BBD)设计实验,考察了氯化钙浓度、萃取剂体积分数、相比和温度4 个因素对反应-萃取-结晶耦合工艺中氯化钙转化率、有机相中氯化氢浓度以及产物碳酸钙的平均粒度的影响及交互作用,并分别建立了三响应值与影响因素间的回归方程。三响应预测最佳值分别为:氯化钙转化率95.08%、有机相氯化氢浓度1.126 mol·L^-1、碳酸钙平均粒度48.71 μm;相应的实验值分别为92.35%、1.123 mol·L^-1 和49.14μm。预测值与实验值接近,误差较小,说明建立的模型对于反应-萃取-结晶工艺的分析和预测准确可靠。

关键词: 废水处理, 结晶, 溶剂萃取, 响应曲面法, 工艺优化

CLC Number:

TQ09

LI Yunzhao, SONG Xingfu, SUN Yuzhu, SUN Ze, YU Jianguo. Optimization of reactive extraction-crystallization process based on response surface methodology[J]. CIESC Journal, 2016, 67(2): 588-597.

李云钊, 宋兴福, 孙玉柱, 孙泽, 于建国. 基于响应曲面法的反应-萃取-结晶工艺优化[J]. 化工学报, 2016, 67(2): 588-597.

References 21

[1]	杨润庭, 张克强. 我国纯碱行业发展现状及市场分析[J]. 纯碱工业, 2012, 1(1):9-11. DOI:10.3969/j.issn.1005-8370.2012.01.003. YANG R T, ZHANG K Q. The development situation and market analysis of soda industry in China[J]. Soda Industry, 2012, 1(1):9-11. DOI:10.3969/j.issn.1005-8370.2012.01.003.
[2]	茅爱新. 氨碱法纯碱生产中废液及碱渣的综合利用[J]. 化学工业与工程技术, 2001, 22(2):31-32. MAO A X. Comprehensive utilization of waste liquid and soda dregs in soda production by ammonia-soda process[J]. Journal of Chemical Industry & Engineering, 2001, 22(2):31-32.
[3]	KASIKOWSKI T, BUCZKOWSKI R, CICHOSZ M. Utilisation of synthetic soda-ash industry by-products[J]. International Journal of Production Economics, 2008, 112(2):971-984. DOI:10.1016/j.ijpe. 2007.08.003.
[4]	STEINHAUSER G. Cleaner production in the Solvay process:general strategies and recent developments[J]. Journal of Cleaner Production, 2008, 16(7):833-841. DOI:10.1016/j.jclepro. 2007. 04. 005.
[5]	张开仕, 曾凤春. 盐酸法生产饲料级磷酸氢钙新工艺研究[J]. 无机盐工业, 2007, 39(4):23-25. DOI:10.3969/j.issn.1006-4990. 2007.04.008. ZHANG K S, ZENG F C. Study on new process for producing feed-grade calcium hydrogen phosphate by hydrochloric acid method[J]. Inorganic Chemicals Industry, 2007, 39(4):23-25. DOI:10.3969/j.issn. 1006-4990.2007.04.008.
[6]	郭玉川, 钮敏, 许树琴. 氯化钙废液联产碳酸钙及氯化铵技术[J]. 河北科技大学学报, 2003, 24(1):59-64. DOI:10.3969/j.issn. 1008-1542. 2003.01.016. GUO Y C, NIU M, XU S Q. New technology of hydrochloric acid as raw materials for production feed-grade DCP simultaneously calcium carbonate and ammonium chloride linked output[J]. Journal of Hebei University of Science and Technology, 2003, 24(1):59-64. DOI:10.3969/j.issn.1008-1542.2003.01.016.
[7]	DAVE R H, GHOSH P K. Efficient recovery of potassium chloride from liquid effluent generated during preparation of schoenite from kainite mixed salt and its reuse in production of potassium sulfate[J]. Industrial & Engineering Chemistry Research, 2006, 45(5):1551-1556. DOI:10.1021/ie050433g.
[8]	KASIKOWSKI T, BUCZKOWSKI R, LEMANOWSKA E. Cleaner production in the ammonia-soda industry:an ecological and economic study[J]. Journal of Environmental Management, 2004, 73(4):339-356. DOI:10.1016/j.jenvman. 2004.08.001.
[9]	KASIKOWSKI T, BUCZKOWSKI R, DEJEWSKA B, et al. Utilization of distiller waste from ammonia-soda processing[J]. Journal of Cleaner Production, 2004, 12(7):759-769. DOI:10.1016/S0959-6526(03)00120-3.
[10]	SYNOWIEC P M, BUNIKOWSKA B. Application of crystallization with chemical reaction in the process of waste brine purifying in evaporative sodium chloride production[J]. Industrial & Engineering Chemistry Research, 2005, 44(7):2273-2280. DOI:10.1021/ie040118e.
[11]	GAO C Z, DONG Y, ZHANG H J, et al. Utilization of distiller waste and residual mother liquor to prepare precipitated calcium carbonate[J]. Journal of Cleaner Production, 2007, 15(15):1419-1425. DOI:10.1016/j.jclepro.2006.06.024.
[12]	MAO X L, SONG X F, LU G M, et al. Effects of metal ions on crystal morphology and size of calcium sulfate whiskers in aqueous HCl solutions[J]. Industrial & Engineering Chemistry Research, 2014, 53(45):17625-17635. DOI:10.1021/ie5030134.
[13]	LI Y Z, SONG X F, CHEN G L, et al. Preparation of calcium carbonate and hydrogen chloride from distiller waste based on reactive extraction-crystallization process[J]. Chemical Engineering Journal, 2015, 278:55-61. DOI:10.1016/j.cej.2014.12.058.
[14]	LI Y Z, SONG X F, CHEN G L, et al. Extraction of hydrogen chloride by a coupled reaction-solvent extraction process[J]. Frontiers of Chemical Science and Engineering, 2015, 9(4):479-487. DOI:10.1007/s11705-015-1512-8.
[15]	李云钊, 宋兴福, 孙玉柱, 等. 反应萃取结晶过程制备碳酸钙的晶型转变与结晶机理[J]. 化工学报, 2015, 66(10):4007-4015. DOI:10.11949/j.issn.0438-1157.20150373. LI Y Z, SONG X F, SUN Y Z, et al. Polymorph transformation and formation mechanism of calcium carbonate during reactive extraction-crystallization process[J]. CIESC Journal, 2015, 66(10):4007-4015. DOI:10.11949/j.issn.0438-1157.20150373.
[16]	LI Y Z, SONG X F, SUN S Y, et al. Extraction equilibrium of hydrochloric acid at low concentrations between water and N235 in isoamyl alcohol solution:experiments and simulation[J]. Journal of Chemical and Engineering Data, 2015, 66(10):3000-3008. DOI:10.1021/acs.jced.5b00409.
[17]	DOUGLAS C M. Design and Analysis of Experiments[M]. 6th ed. Beijing:Posts &Telecom Press, 2009:347-349.
[18]	陆燕, 梅乐和, 陆悦飞, 等. 响应面法优化工程菌产细胞色素P450BM-3的发酵条件[J]. 化工学报, 2006, 57(5):1187-1192. DOI:10.3321/j.issn:0438-1157.2006.05.027. LU Y, MEI L H, LU Y F, et al. Optimization of P450 BM-3 activity produced by gene engineering strain by response surface methodology[J]. Journal of Chemical Industry and Engineering (China), 2006, 57(5):1187-1192. DOI:10.3321/j.issn:0438-1157. 2006.05.027.
[19]	蒋绍阶, 冯欣蕊, 李晓恩, 等. 响应面法优化制备PACPDMDAAC杂化絮凝剂及其表征[J]. 化工学报, 2014, 65(2):731-736. DOI:10.3969/j.issn.0438-1157.2014.02.051. JIANG S J, FENG X R, LI X E, et al. Preparation of PAC-PDMDAAC hybrid flocculant by response surface method and its characterization[J]. CIESC Journal, 2014, 65(2):731-736. DOI:10.3969/j.issn.0438-1157.2014.02.051.
[20]	SHAN X, QIN W, WANG S, et al. Dependence of extraction equilibrium on apparent basicity of extractant[J]. Industrial & Engineering Chemistry Research, 2006, 45(26):9075-9079. DOI:10.1021/ie060814+.
[21]	TAN I A W, AHMAD A L, HAMEED B H. Optimization of preparation conditions for activated carbons from coconut husk using response surface methodology[J]. Chemical Engineering Journal, 2008, 137(3):462-470. DOI:10.1016/j.cej.2007.04.031.

Related Articles 15

[1]	Hongxin YU, Shuangquan SHAO. Simulation analysis of water crystallization process [J]. CIESC Journal, 2023, 74(S1): 250-258.
[2]	Yu FU, Xingchong LIU, Hanyu WANG, Haimin LI, Yafei NI, Wenjing ZOU, Yue LEI, Yongshan PENG. Research on F₃EACl modification layer for improving performance of perovskite solar cells [J]. CIESC Journal, 2023, 74(8): 3554-3563.
[3]	Xiaodan SU, Ganyu ZHU, Huiquan LI, Guangming ZHENG, Ziheng MENG, Fang LI, Yunrui YANG, Benjun XI, Yu CUI. Optimization of wet process phosphoric acid hemihydrate process and crystallization of gypsum [J]. CIESC Journal, 2023, 74(4): 1805-1817.
[4]	Weiyi SU, Jiahui DING, Chunli LI, Honghai WANG, Yanjun JIANG. Research progress of enzymatic reactive crystallization [J]. CIESC Journal, 2023, 74(2): 617-629.
[5]	Yuming CHEN, Wei LI, Xiang YAN, Jingdai WANG, Yongrong YANG. Research progress on regulation of aggregation structure for nascent polyethylene [J]. CIESC Journal, 2023, 74(2): 487-499.
[6]	Xuan ZHOU, Mengya LI, Jie SUN, Zhenkai CEN, Qiangsan LYU, Lishan ZHOU, Haitao WANG, Dandan HAN, Junbo GONG. The regulation mechanism of additives on the amino acid crystal growth [J]. CIESC Journal, 2023, 74(2): 500-510.
[7]	Xueying NAI, Peng WU, Yuan CHENG, Jianfei XIAO, Xin LIU, Yaping DONG. Study on hydrothermal crystallization kinetics of magnesium oxysulfate nanowires [J]. CIESC Journal, 2022, 73(7): 3038-3044.
[8]	Guoxin SUN, Mengxuan GOU, Cheng ZHOU, Pei CHANG, Gaohong HE, Xiaobin JIANG. Membrane distillation crystallization coupling process for the treatment of high concentration Na⁺//NO $3 -$ , SO $4 2 -$ -H₂O solution [J]. CIESC Journal, 2022, 73(7): 3078-3089.
[9]	Chunhui LI, Hui HE, Mingjian HE, Meng ZHANG, Yang GAO, Caishan JIAO. Extraction kinetics of Ce(Ⅳ) from nitric acid solutions using ionic liquid [J]. CIESC Journal, 2022, 73(4): 1606-1614.
[10]	Yaoming CHEN,Feng XU,Xionglin LUO. A coordinated optimal margin design method for chemical process based on relative gain and priority [J]. CIESC Journal, 2022, 73(3): 1280-1290.
[11]	Haiqing YIN, Yiming MA, Xuxing WAN, Weibing DONG, Yulong ZHANG, Songgu WU. Research of lithium carbonate three-phase reactive crystallization process [J]. CIESC Journal, 2022, 73(3): 1207-1220.
[12]	Pengzhi BEI, Wenying LI. An energy decomposition analysis-based extractant selection [J]. CIESC Journal, 2022, 73(2): 739-746.
[13]	Xuemei CHEN, Tong WANG, Yubo GAO, Dingcheng PENG, Yuting LUO. Efficient solar interfacial evaporation using laser-induced graphene [J]. CIESC Journal, 2022, 73(12): 5648-5659.
[14]	Pengcheng JING, Litao CHEN, Chuanliang YAN, Chuanxiang JIANG, Yuxiang XIA, Changhong YU, Haotian WANG. Study on growth process of semiclathrate hydrate on the surface of TBAB solution droplets suspended by ultrasonic [J]. CIESC Journal, 2022, 73(11): 4893-4902.
[15]	Zheng WANG, Feng XU, Xionglin LUO. Full-cycle optimization of acetylene conversion distribution for acetylene hydrogenation beds-in-series reactor [J]. CIESC Journal, 2022, 73(10): 4551-4564.