醋酸废水络合萃取处理技术及理论研究
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摘要
随着我国经济的发展,糠醛行业得到飞速发展,该行业排放的醋酸废水也不断增加,稀浓度醋酸废水的治理成为制约糠醛行业发展的一块绊脚石。而醋酸是一种重要的化工原料,具有广泛的用途。因此,将醋酸从其稀溶液中回收利用,杜绝排放废水对环境的污染,不仅节约资源,而且保护环境。所以本课题的研究既有学术价值又有实际意义。
本文综述了含醋酸废水处理的各种方法及发展现状。着重介绍了络合萃取法处理醋酸废水,此法是在含醋酸废水中加入萃取剂,使醋酸主要以络合物的方式从废水中提取,然后再用反萃剂把醋酸从废水中反萃出。这样,废水中的醋酸几乎可以完全提取,同时,萃取剂能反复利用。本文的研究内容和成果如下所述:
1、对醋酸废水进行络合萃取处理研究,工艺的首要条件是通过条件试验探索,找出最佳的络合萃取剂体系组成。通过研究该法处理醋酸废水过程中,筛选出TBPO(自配)为络合萃取剂、磺化煤油为稀释剂。
2、详细测定了平衡时间、磺化煤油占有机相的体积百分比、温度、相比、萃取剂浓度、水溶液中醋酸的浓度等因素对络合萃取平衡的影响。在此基础上,确定了影响醋酸络合萃取的最佳值。为了找到各因素最佳组合下的最优分配比,采用了正交实验法。实验结果如下:温度为20℃,萃取剂浓度为3.5 mol/L,磺化煤油占有机相的体积百分比50%,相比为1。同时用统计软件对醋酸水溶液络合正交实验结果进行方差分析,结果表明:预测较好。
3、由于单级萃取不能达到预定的目标,本工艺采用多级逆流萃取方法。通过模型法和实验法确定逆流级数为5,萃取率达到了99%,废水中的醋酸几乎完全被回收,分离出的醋酸废水满足了《污水综合排放标准》——GB8978—1996的三级排放标准。
4、采用氢氧化钠为反萃剂对负载有机相进行反萃,反萃后得到萃取剂经多次实验验证,能反复利用;得到的溶液经浓缩结晶得到醋酸钠晶体,经化验分析符合Q/NH18—1999标准。
With China's economic development, furfural industries have developed rapidly, the industry's emissions will continue to increase waste water containing acetic acid,containing-acetic acid wastewater treatment constraints furfural industry as a stumbling block to development. The acetic acid is an important chemical raw material and has a wide range of use. Reusing acetic acid form its dilute solution and constrainting wastewater to pollute environment are not only save resources, but also protect environment. Therefore, the study of this subject has both practical and academic value.
This paper reviews treatment methods and the development status of the acetic acid waste water.Focusing on the complex extraction treatment acetate wastewater,this method is to put extraction agent to the waste water containing acetic acid, make acetic acid extracted from waste water mainly in the way of complex compound. And then stripping out of the acetic acid from waste water by using stripping agent. In this way, the acetic acid from waste water is almost entirely extracted. At the same time, the extraction agent can be repeatedly used.The study contents and results of this paper are as follows:
1. On the study of extraction treatment of Acetic Acid wastewater. The first condition of technology is through the tests to find the best system of extractant. Through studing this method to treat Acetic Acid Waste Water, filtrating TBPO extraction agent,kerosene thinner.
2. It tests in detail the effect some factors on complex extraction equilibration,the factors include equilibration time、the volume percent of kerosene to organic phase、tempertuare、phase ratio、extractant concentration、acetic acid concentration and so on. In order to find the best distribution ratio under combination of the factors,and adopt orthogonal test .The test result is as below: temperature 20°C, extractant concentration 3.5 mol/L, the volume ratio of kerosene 50%, phase ratio.Meanwhile using statistical software to make analysis of variance for orthogonal test result of acetic acid wastewater.The result indicate forecast result is better.
3. Because single-stage extraction cannot meet the target,the technology adopt multi-stage counter-current extraction.And make sure that the stage is 5 through the model method and test,the extraction rate achieve 99%, the acetic acid in wastewater is almost recovered, the separated wastewater can meet《wastewater discharge standards》-- GB8978—1996 for Grade III.
4. Adopting sodium hydroxide as stripping agent to strip load organic phase, and obtaining extractant after stripping can be repeatedly used by test verification; Sodium acetate crystals from crystal enrichment of separated solution can meet the standards Q/NH18-1999 through laboratory analysis.
本文综述了含醋酸废水处理的各种方法及发展现状。着重介绍了络合萃取法处理醋酸废水,此法是在含醋酸废水中加入萃取剂,使醋酸主要以络合物的方式从废水中提取,然后再用反萃剂把醋酸从废水中反萃出。这样,废水中的醋酸几乎可以完全提取,同时,萃取剂能反复利用。本文的研究内容和成果如下所述:
1、对醋酸废水进行络合萃取处理研究,工艺的首要条件是通过条件试验探索,找出最佳的络合萃取剂体系组成。通过研究该法处理醋酸废水过程中,筛选出TBPO(自配)为络合萃取剂、磺化煤油为稀释剂。
2、详细测定了平衡时间、磺化煤油占有机相的体积百分比、温度、相比、萃取剂浓度、水溶液中醋酸的浓度等因素对络合萃取平衡的影响。在此基础上,确定了影响醋酸络合萃取的最佳值。为了找到各因素最佳组合下的最优分配比,采用了正交实验法。实验结果如下:温度为20℃,萃取剂浓度为3.5 mol/L,磺化煤油占有机相的体积百分比50%,相比为1。同时用统计软件对醋酸水溶液络合正交实验结果进行方差分析,结果表明:预测较好。
3、由于单级萃取不能达到预定的目标,本工艺采用多级逆流萃取方法。通过模型法和实验法确定逆流级数为5,萃取率达到了99%,废水中的醋酸几乎完全被回收,分离出的醋酸废水满足了《污水综合排放标准》——GB8978—1996的三级排放标准。
4、采用氢氧化钠为反萃剂对负载有机相进行反萃,反萃后得到萃取剂经多次实验验证,能反复利用;得到的溶液经浓缩结晶得到醋酸钠晶体,经化验分析符合Q/NH18—1999标准。
With China's economic development, furfural industries have developed rapidly, the industry's emissions will continue to increase waste water containing acetic acid,containing-acetic acid wastewater treatment constraints furfural industry as a stumbling block to development. The acetic acid is an important chemical raw material and has a wide range of use. Reusing acetic acid form its dilute solution and constrainting wastewater to pollute environment are not only save resources, but also protect environment. Therefore, the study of this subject has both practical and academic value.
This paper reviews treatment methods and the development status of the acetic acid waste water.Focusing on the complex extraction treatment acetate wastewater,this method is to put extraction agent to the waste water containing acetic acid, make acetic acid extracted from waste water mainly in the way of complex compound. And then stripping out of the acetic acid from waste water by using stripping agent. In this way, the acetic acid from waste water is almost entirely extracted. At the same time, the extraction agent can be repeatedly used.The study contents and results of this paper are as follows:
1. On the study of extraction treatment of Acetic Acid wastewater. The first condition of technology is through the tests to find the best system of extractant. Through studing this method to treat Acetic Acid Waste Water, filtrating TBPO extraction agent,kerosene thinner.
2. It tests in detail the effect some factors on complex extraction equilibration,the factors include equilibration time、the volume percent of kerosene to organic phase、tempertuare、phase ratio、extractant concentration、acetic acid concentration and so on. In order to find the best distribution ratio under combination of the factors,and adopt orthogonal test .The test result is as below: temperature 20°C, extractant concentration 3.5 mol/L, the volume ratio of kerosene 50%, phase ratio.Meanwhile using statistical software to make analysis of variance for orthogonal test result of acetic acid wastewater.The result indicate forecast result is better.
3. Because single-stage extraction cannot meet the target,the technology adopt multi-stage counter-current extraction.And make sure that the stage is 5 through the model method and test,the extraction rate achieve 99%, the acetic acid in wastewater is almost recovered, the separated wastewater can meet《wastewater discharge standards》-- GB8978—1996 for Grade III.
4. Adopting sodium hydroxide as stripping agent to strip load organic phase, and obtaining extractant after stripping can be repeatedly used by test verification; Sodium acetate crystals from crystal enrichment of separated solution can meet the standards Q/NH18-1999 through laboratory analysis.
引文
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[2]王炼翃.利用醋酸废水生产醋酸钠工艺的研究与应用[J].广西轻工业,2007,2:22-24
[3]赵音延,秦炜,戴猷元.利用醋酸稀溶液生产绿色化学品-醋酸钙镁盐的研究[J].化学工程,2003,31(1):63-75
[4]贾彦雷.稀水溶液中有机羧酸的萃取分离研究[硕士学位论文].天津大学,2004
[5]张培辉,韦奇.水-甲酸-乙酸混合物的恒沸分馏[J].华东化工学院学报,1993,19(4):427-431
[6]Donald F O,Brooklyn Y N.Process for dehydration of acetic acid and other lower fatter acids[P].US:1936,8(4):2050-2234
[7]Costantini G,Serafini M,Paoli P.Process for the recovery of the solvent and of the by-produced methylacetate in the synthesis of terephthalic acid[P].U S:4,250,330,1980-02-10
[8]Parten W D,Urealan M.Dehydration of acetic acid by azeotropic distillation in the production an aromatic acid[P].WO:9606065,1996-02-29
[9]Berg L.Dehydration of acetic acid by extractive distillation[P].U S:5,167,744,1992-12-1
[10]Yildirim M E,Demiral H.Recovery of acetic acid from waste streams by extractior distillation[J].Water Science and Technology,47(10):183-188
[11]胡兴兰,苗文俊,周荣琪.萃取精馏法分离醋酸/水的工艺模拟,天然气化工(C1 化学与化工),2004,29(1):37-39
[12]李新利,唐聪明.萃取精馏分离醋酸/水溶液溶剂研究进展及机理分析[J].天然气化工(C1 化学与化工),2005,30(06):63-66
[13]Saha B,Chopade S P,Mahajani,S M.Recovery of dilute acetic through esterification in areactive distillation column[J].Catalysis Today,2000,60(1-2):147-157
[14]白鹏,刘劲松,杨志才.回收废醋酸催化精馏过程的研究[J].四川大学学报(工程科学版),2002,34(5):63-65
[15]Liu J-S,Yang Z-C,Bai P.Simulation of catalytic distillation on for removal of dilute acetic acid from wastewater[J].Moder Chemical Industry,2003,23(SUPPL):159-162
[16]Tsurumaru N.Method of recovering acetic acid from aqueous solution of acetate[P].J P:59,029,633,1984-02-16
[17]Bianchi C L,Ragaini V,Pirola C,et al.A new method to clean industrial water from acetic acidvia esterification[J].Applide Catalysis B:Environmental,2003,40(2):93-99
[18]刘春生,程云,严红燕等.酯化法处理底含量醋酸水溶液[J].辽宁石油化工大学学报,2004,24(3):18-20
[19]秦炜,王东,戴猷元.超声场对树脂吸附醋酸动力学影响的机理研究[J].清华大学学报(自然科学版),2001,41(4/5):28-31
[20]Ganguly S K,Goswami A N.Surface diffusion kinetics in the adsorption of acetic acidon activated carbon Source[J].Separation Science and Technology,1996,31(9):1267-1278
[21]Cloete F L D,Marais A P.Recovery of very dilute acetic acid using ion exchange,Industrial and Engineering Chemistry Research[J].1995,34(7):2464-2467
[22]简日春.从乙二醇制程水中去除甲酸、乙酸的方法和装置[P].CN:98117614.3,1998-08-20
[23]Li N N.Separating hydrocarbons with liquid membranes[P].U S:3,410,794,1968-11-12
[24]倪邦庆,马新胜,施亚钧.液膜法连续处理含醋酸废水[J].无锡轻工大学学报,1998,18(4):51-55
[25]Durmaz-Hilmroglu N,Yildirim AE,Sakaoglu A S,et al.Acetic acid dehydration by pervaporation[J].Chemical Engineering and Processing,2001,40(3):263-267
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