SK静态混合器对工业磷酸脱砷的过程强化研究
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摘要
以五硫化二磷脱砷剂分别开展了搅拌混合及SK静态混合脱除工业磷酸中砷(As)的研究。利用单因素实验、正交实验和响应曲面实验设计,得到了最佳反应条件。结果表明:两种反应器最佳的脱砷剂用量均为理论用量的4倍,脱砷率大于99.8%,净化后的产品砷浓度小于0.5 mg·kg-1,满足国家标准GB 1886.15—2015规定的食品级磷酸指标。搅拌反应器脱砷过程最佳反应温度65℃,反应时间70 min,搅拌速度300 r·min-1;以SK静态混合器进行磷酸脱砷,最佳磷酸流速为0.66m·s-1,反应时间2.4s,单位时间内处理的磷酸量是搅拌反应器的372倍。用SK静态混合器进行磷酸脱砷,具有工艺流程短、结构简单紧凑、可连续操作等优点,可以实现工业磷酸脱砷的过程强化。
The agitation tank and Keltics static mixer were used to remove arsenic(As) from industrial phosphoric acid by using phosphorus pentasulfide(P2S5).The single factor experiments,orthogonal experiment and response suface methodology were conducted to acquire the optimal process conditions.The results showed that the removal efficiencies of both of the two reactors were higher than 98.8% and the content of As were less than 0.5 mg·kg-1 in the purified phosphoric acid,which met the national standard of China GB 1886.15—2015 for food grade phosphoric acid.As the agitation tank was the reactor,the optimum process conditions were that the actual dosage of dearsenifying agent was 4 times of the theoretical dosage,reaction temperature was 65℃,reaction time was 70 min and the stirring speed was 300 r·min-1.As the Keltics static mixer was the reactor,the optimum process conditions were that the actual dosage of dearsenifying agent was 4 times of the theoretical dosage and the phosphoric acid flow was 0.66 m3·s-1.Under this condition,the disposal phosphoric flow was increased greatly,and the reaction time was only 2.4 s and the amount of phosphoric acid treated per unit of time is 372 times that of the stirred reactor.As Keltics static mixer is used to remove arsenic(As) from industrial phosphoric acid,there are many advantages,such as the shorter technological process,the simpler construction,the continuant operation,etc.,which is hopefully to realize the process intensification of dearsenifying As from phosphoric.
The agitation tank and Keltics static mixer were used to remove arsenic(As) from industrial phosphoric acid by using phosphorus pentasulfide(P2S5).The single factor experiments,orthogonal experiment and response suface methodology were conducted to acquire the optimal process conditions.The results showed that the removal efficiencies of both of the two reactors were higher than 98.8% and the content of As were less than 0.5 mg·kg-1 in the purified phosphoric acid,which met the national standard of China GB 1886.15—2015 for food grade phosphoric acid.As the agitation tank was the reactor,the optimum process conditions were that the actual dosage of dearsenifying agent was 4 times of the theoretical dosage,reaction temperature was 65℃,reaction time was 70 min and the stirring speed was 300 r·min-1.As the Keltics static mixer was the reactor,the optimum process conditions were that the actual dosage of dearsenifying agent was 4 times of the theoretical dosage and the phosphoric acid flow was 0.66 m3·s-1.Under this condition,the disposal phosphoric flow was increased greatly,and the reaction time was only 2.4 s and the amount of phosphoric acid treated per unit of time is 372 times that of the stirred reactor.As Keltics static mixer is used to remove arsenic(As) from industrial phosphoric acid,there are many advantages,such as the shorter technological process,the simpler construction,the continuant operation,etc.,which is hopefully to realize the process intensification of dearsenifying As from phosphoric.
引文
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[3]MENG W,CHEN J,WANG X.Removal of arsenic and cadmium with sequential soil washing techniques using Na2EDTA,oxalic and phosphoric acid:optimization conditions,removal effectiveness and ecological risks[J].Chemosphere,2016,156:252-261.
[4]TRABELSI W,TLILI A.Phosphoric acid purification through different raw and activated clay materials(Southern Tunisia)[J].Journal of African Earth Sciences,2017,129:647-658.
[5]江玉明,李道纯,苏元复.萃取法净化磷酸工艺[J].化工学报,1982,33(4):310-318.JIANG Y M,LI D C,SU Y F.A process based upon solvent extraction for the purification of phosphoric acid[J].Journal of Chemical Industry and Engineering(China),1982,33(4):310-318.
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[7]CHUNG J Y,YU S D,HONG Y S.Environmental source of arsenic exposure[J].Journal of Preventive Medicine and Public Health,2014,47(5):253-257.
[8]NIDHEESH P V,ANANTHASINGH T S.Arsenic removal by electrocoagulation process:recent trends and removal mechanism[J].Chemosphere,2017,181:418-432.
[9]张允湘,钟本和.湿法磷酸的净化方法评述[J].磷酸盐工业,2001,(2):21-25.ZHANG Y X,ZHONG B H.Purification of wet-process phosphoric acid[J].Phosphate Industry,2001,(2):21-25.
[10]BISANG J M,BOGADO F,RIVERA M O,et al.Electrochemical removal of arsenic from technical grade phosphoric acid[J].Journal of Applied Electrochemistry,2004,34(4):375-381.
[11]TODOROVA E I,DOMBALOV I P.Production of phosphoric acid with low content of impurities[J].Fertilizer Research,1995,41(2):125-128.
[12]王琴,张人元,张强,等.窑法磷酸中铁、铅、砷的深度净化[J].磷肥与复肥,2015,30(2):4-7.WANG Q,ZHANG R Y,ZHANG Q,et al.Intensive removal of iron,lead and arsenic from kiln phosphoric acid[J].Phosphate&Compound Fertilizer,2015,30(2):4-7.
[13]孟文祥,吴松,陶志,等.以湿法工业级磷酸生产电子级磷酸的脱砷技术[J].磷肥与复肥,2014,29(1):47-48.MENG W X,WU S,TAO Z,et al.Technology of arsenic removal from industrial grade WPA to produce electronic grade phosphoric acid[J].Phosphate&Compound Fertilizer,2014,29(1):47-48.
[14]查坐统,苏毅,李国斌.黄磷精制废液脱砷的实验研究[J].化工科技,2009,17(4):13-16.ZHA Z T,SU Y,LI G B.The experimental study on the arsenic removal of waste liquid of refining yellow phosphorus[J].Science&Technology in Chemical Industry,2009,17(4):13-16.
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[17]PARICHAY K D,LEGRAND J.Drop breakage model in static mixers at low and intermediate Reynolds number[J].Chemical Engineering Science,2005,60:231-238.
[18]王修纲,郭瓦力,吴剑华.静态混合器中液液分散的实验及CFD模拟[J].化工学报,2012,63(3):767-774.WANG X G,GUO W L,WU J H.Experimental and numerical study on liquid-liquid dispersion in static mixer[J].CIESC Journal,2012,63(3):767-774.
[19]VASIC V,JOKIC A,SCIBAN M,et al.Flux intensification during microfiltration of distillery stillage using a kenics static mixer[J].Acta Periodica Technologica,2017,48(48):285-293.
[20]谢迎新,刘敬军,李佳庚,等.静态混合器强化Ce3+臭氧氧化再生反应研究[J].高校化学工程学报,2017,31(6):1318-1326.XIE Y X,LIU J J,LI J G,et al.Study on ozone oxidation regeneration of Ce3+enhanced by a static mixer[J].Journal of Chemical Engineering of Chinese Universities,2017,31(6):1318-1326.
[21]傅鑫亮,闫志勇,蔡巧梅,等.仿柳叶形静态混合元件的流动及混合特性研究[J].热能动力工程,2017,(12):84-89.FU X L,YAN Z Y,CAI Q M,et al.Flow and mixing characteristics in willow leaf-like static mixer[J].Journal of Engineering for Thermal Energy&Power,2017,(12):84-89.
[22]李慧.热法磷酸生产中除雾与连续脱砷技术研究[D].昆明:昆明理工大学,2016.LI H.Defogging and continuous dearsenification in the preparation process of hot-process phosphoric acid[D].Kunming:Kunming University of Science and Technology,2016.
[23]傅凯,邹涛.湿法磷酸净化制备食品级磷酸氢钙的工艺研究[J].化学与生物工程,2003,20(s2):12-13.FU K,ZOU T.Purification and preparation of wet-process phosphoric acid of food grade calcium hydrogen phosphate process[J].Chemical and Biological Engineering,2003,20(s2):12-13.
[24]蒋涛,王丽军.LiH合成反应器的CFD模拟与过程强化[J].化学反应工程与工艺,2017,33(3):215-220.JIANG T,WANG L J.CFD simulation and process intensification of LiH synthesis reactor[J].Chemical Reaction Engineering&Technology,2017,33(3):215-220.
[25]HOBBS D M,MUZZIO F J.Optimization of a static mixer using dynamical systems techniques[J].Chemical Engineering Science,1998,53(18):3199-3213.
[26]BYRDE O,SAWLEY M L.Parallel computation and analysis of the flow in a static mixer[J].Computers&Fluids,1999,28(1):1-18.
[27]MELESHKO V V,GALAKTIONOV O S,PETERS G W M,et al.Three-dimensional mixing in Stokes flow:the partitioned pipe mixer problem revisited[J].European Journal of Mechanics-B/Fluids,1999,18(5):783-792.
[28]KUMAR V,SHIRKE V,Nigam K D P.Performance of Kenics static mixer over a wide range of Reynolds number[J].Chemical Engineering Journal,2008,139(2):284-295.
[29]吴剑华,孟辉波,禹言芳,等.SK型静态混合器壁压脉动信号的多尺度多分形特性[J].化工学报,2009,60(8):1965-1973.WU J H,MENG H B,YU Y F,et al.Multi-scale and multi-fractal characteristics of tube-pressure signals in Kenics static mixer[J].CIESC Journal,2009,60(8):1965-1973.
[30]吴剑华,张春梅,金丹,等.SK型静态混合器湍流性能的实验研究[J].过程工程学报,2008,8(4):714-718.WU J H,ZHANG C M,JIN D,et al.Experimental study on turbulence properties in a Kenics static mixer[J].Chinese Journal of Process Engineering,2008,8(4):714-718.
[31]KHURI A I,MUKHOPADHYAY S.Response surface methodology[J].Wiley Interdisciplinary Reviews:Computational Statistics,2010,2(2):128-149.
[32]TETTEH E K,RATHILAL S.Effects of a polymeric organic coagulant for industrial mineral oil wastewater treatment using response surface methodology(RSM)[J].Water SA,2018,44(2):155-161.
[33]林天扬,王春红,YOUSFANI S H S,等.碱处理提取竹黄纤维的响应曲面优化[J].复合材料学报,2018,35(4):876-884.LIN T Y,WANG C H,YOUSFANI S H S,et al.Study on extraction technology of bamboo fiber by response surface[J].Acta Materiae Compositae Sinica,2018,35(4):876-884.
[34]ZHANG H,WANG Z,XU S Y.Optimization of processing parameters for cloudy ginkgo(Ginkgo biloba Linn.)juice[J].Journal of Food Engineering,2007,80(4):1226-1232.
[35]LI Y W,PENG J H,LIANG G A,et al.Optimization of processing parameters for microwave drying of selenium-rich slag using incremental improved back-propagation neural network and response surface methodology[J].Journal of Central South University,2011,18(5):1441-1447.
[2]STANKIEWICZ A,MOULIJN J A.化工装置的再设计--过程强化[M].王广全,刘学军,陈金花,译.北京:国防工业出版社,2012.STANKIEWICZ A,MOULIJN J A.Re-engineering the Chemical Processing Plant:?Process Intensification[M].WANG G Q,LIU X J,CHEN J H,trans.Beijing:National Defence Industry Press,2012.
[3]MENG W,CHEN J,WANG X.Removal of arsenic and cadmium with sequential soil washing techniques using Na2EDTA,oxalic and phosphoric acid:optimization conditions,removal effectiveness and ecological risks[J].Chemosphere,2016,156:252-261.
[4]TRABELSI W,TLILI A.Phosphoric acid purification through different raw and activated clay materials(Southern Tunisia)[J].Journal of African Earth Sciences,2017,129:647-658.
[5]江玉明,李道纯,苏元复.萃取法净化磷酸工艺[J].化工学报,1982,33(4):310-318.JIANG Y M,LI D C,SU Y F.A process based upon solvent extraction for the purification of phosphoric acid[J].Journal of Chemical Industry and Engineering(China),1982,33(4):310-318.
[6]江莉,王翊民,迟百宏.我国食品级磷酸产业发展现状[J].化工管理,2013,19:39-40.JIANG L,WANG Y M,CHI B H.Development status of China's food grade phosphoric acid industry[J].Chemical Industry Management,2013,19:39-40.
[7]CHUNG J Y,YU S D,HONG Y S.Environmental source of arsenic exposure[J].Journal of Preventive Medicine and Public Health,2014,47(5):253-257.
[8]NIDHEESH P V,ANANTHASINGH T S.Arsenic removal by electrocoagulation process:recent trends and removal mechanism[J].Chemosphere,2017,181:418-432.
[9]张允湘,钟本和.湿法磷酸的净化方法评述[J].磷酸盐工业,2001,(2):21-25.ZHANG Y X,ZHONG B H.Purification of wet-process phosphoric acid[J].Phosphate Industry,2001,(2):21-25.
[10]BISANG J M,BOGADO F,RIVERA M O,et al.Electrochemical removal of arsenic from technical grade phosphoric acid[J].Journal of Applied Electrochemistry,2004,34(4):375-381.
[11]TODOROVA E I,DOMBALOV I P.Production of phosphoric acid with low content of impurities[J].Fertilizer Research,1995,41(2):125-128.
[12]王琴,张人元,张强,等.窑法磷酸中铁、铅、砷的深度净化[J].磷肥与复肥,2015,30(2):4-7.WANG Q,ZHANG R Y,ZHANG Q,et al.Intensive removal of iron,lead and arsenic from kiln phosphoric acid[J].Phosphate&Compound Fertilizer,2015,30(2):4-7.
[13]孟文祥,吴松,陶志,等.以湿法工业级磷酸生产电子级磷酸的脱砷技术[J].磷肥与复肥,2014,29(1):47-48.MENG W X,WU S,TAO Z,et al.Technology of arsenic removal from industrial grade WPA to produce electronic grade phosphoric acid[J].Phosphate&Compound Fertilizer,2014,29(1):47-48.
[14]查坐统,苏毅,李国斌.黄磷精制废液脱砷的实验研究[J].化工科技,2009,17(4):13-16.ZHA Z T,SU Y,LI G B.The experimental study on the arsenic removal of waste liquid of refining yellow phosphorus[J].Science&Technology in Chemical Industry,2009,17(4):13-16.
[15]戴石清.用五硫化二磷精制热法磷酸[J].无机盐工业,1986,(6):11-14.DAI S Q.Purification of hot-process phosphoric acid using phosphorus pentasulfide[J].Inorganic Chemicals Industry,1986,(6):11-14.
[16]HOBBS D M,SWANSON P D,MUZZIO F J.Numerical characterization of low Reynolds number flow in the Kenics static mixer[J].Chemical Engineering Science,1998,53(8):1565-1584.
[17]PARICHAY K D,LEGRAND J.Drop breakage model in static mixers at low and intermediate Reynolds number[J].Chemical Engineering Science,2005,60:231-238.
[18]王修纲,郭瓦力,吴剑华.静态混合器中液液分散的实验及CFD模拟[J].化工学报,2012,63(3):767-774.WANG X G,GUO W L,WU J H.Experimental and numerical study on liquid-liquid dispersion in static mixer[J].CIESC Journal,2012,63(3):767-774.
[19]VASIC V,JOKIC A,SCIBAN M,et al.Flux intensification during microfiltration of distillery stillage using a kenics static mixer[J].Acta Periodica Technologica,2017,48(48):285-293.
[20]谢迎新,刘敬军,李佳庚,等.静态混合器强化Ce3+臭氧氧化再生反应研究[J].高校化学工程学报,2017,31(6):1318-1326.XIE Y X,LIU J J,LI J G,et al.Study on ozone oxidation regeneration of Ce3+enhanced by a static mixer[J].Journal of Chemical Engineering of Chinese Universities,2017,31(6):1318-1326.
[21]傅鑫亮,闫志勇,蔡巧梅,等.仿柳叶形静态混合元件的流动及混合特性研究[J].热能动力工程,2017,(12):84-89.FU X L,YAN Z Y,CAI Q M,et al.Flow and mixing characteristics in willow leaf-like static mixer[J].Journal of Engineering for Thermal Energy&Power,2017,(12):84-89.
[22]李慧.热法磷酸生产中除雾与连续脱砷技术研究[D].昆明:昆明理工大学,2016.LI H.Defogging and continuous dearsenification in the preparation process of hot-process phosphoric acid[D].Kunming:Kunming University of Science and Technology,2016.
[23]傅凯,邹涛.湿法磷酸净化制备食品级磷酸氢钙的工艺研究[J].化学与生物工程,2003,20(s2):12-13.FU K,ZOU T.Purification and preparation of wet-process phosphoric acid of food grade calcium hydrogen phosphate process[J].Chemical and Biological Engineering,2003,20(s2):12-13.
[24]蒋涛,王丽军.LiH合成反应器的CFD模拟与过程强化[J].化学反应工程与工艺,2017,33(3):215-220.JIANG T,WANG L J.CFD simulation and process intensification of LiH synthesis reactor[J].Chemical Reaction Engineering&Technology,2017,33(3):215-220.
[25]HOBBS D M,MUZZIO F J.Optimization of a static mixer using dynamical systems techniques[J].Chemical Engineering Science,1998,53(18):3199-3213.
[26]BYRDE O,SAWLEY M L.Parallel computation and analysis of the flow in a static mixer[J].Computers&Fluids,1999,28(1):1-18.
[27]MELESHKO V V,GALAKTIONOV O S,PETERS G W M,et al.Three-dimensional mixing in Stokes flow:the partitioned pipe mixer problem revisited[J].European Journal of Mechanics-B/Fluids,1999,18(5):783-792.
[28]KUMAR V,SHIRKE V,Nigam K D P.Performance of Kenics static mixer over a wide range of Reynolds number[J].Chemical Engineering Journal,2008,139(2):284-295.
[29]吴剑华,孟辉波,禹言芳,等.SK型静态混合器壁压脉动信号的多尺度多分形特性[J].化工学报,2009,60(8):1965-1973.WU J H,MENG H B,YU Y F,et al.Multi-scale and multi-fractal characteristics of tube-pressure signals in Kenics static mixer[J].CIESC Journal,2009,60(8):1965-1973.
[30]吴剑华,张春梅,金丹,等.SK型静态混合器湍流性能的实验研究[J].过程工程学报,2008,8(4):714-718.WU J H,ZHANG C M,JIN D,et al.Experimental study on turbulence properties in a Kenics static mixer[J].Chinese Journal of Process Engineering,2008,8(4):714-718.
[31]KHURI A I,MUKHOPADHYAY S.Response surface methodology[J].Wiley Interdisciplinary Reviews:Computational Statistics,2010,2(2):128-149.
[32]TETTEH E K,RATHILAL S.Effects of a polymeric organic coagulant for industrial mineral oil wastewater treatment using response surface methodology(RSM)[J].Water SA,2018,44(2):155-161.
[33]林天扬,王春红,YOUSFANI S H S,等.碱处理提取竹黄纤维的响应曲面优化[J].复合材料学报,2018,35(4):876-884.LIN T Y,WANG C H,YOUSFANI S H S,et al.Study on extraction technology of bamboo fiber by response surface[J].Acta Materiae Compositae Sinica,2018,35(4):876-884.
[34]ZHANG H,WANG Z,XU S Y.Optimization of processing parameters for cloudy ginkgo(Ginkgo biloba Linn.)juice[J].Journal of Food Engineering,2007,80(4):1226-1232.
[35]LI Y W,PENG J H,LIANG G A,et al.Optimization of processing parameters for microwave drying of selenium-rich slag using incremental improved back-propagation neural network and response surface methodology[J].Journal of Central South University,2011,18(5):1441-1447.