Recovery of dilute acetic acid through
esterification in a reactive distillation column
The recovery of acetic acid from its dilute aqueous solutions is a major problem in both petrochemical and fine chemical
industries. The conventional methods of recovery are azeotropic distillation, simple distillation and liquid–liquid extraction.
Physical separations such as distillation and extraction suffer from several drawbacks. The esterification of an aqueous solution
(30%) of acetic acid with n-butanol/iso-amyl alcohol is a reversible reaction. As excess of water is present in the reaction
mixture, the conversion is greatly restricted by the equilibrium limitations. The esters of acetic acid, namely, n-butyl acetate
and iso-amyl acetate, have a wide range of applications. In view of the appreciable value of these esters, the present work was
directed towards recovery of 30% acetic acid by reaction with n-butanol and iso-amyl alcohol in a reactive distillation column
(RDC) using macroporous ion-exchange resin, Indion 130, as a catalyst bed, confined in stainless steel wire cages. Experiments
were conducted in order to achieve an optimum column configuration for the synthesis of n-butyl acetate/iso-amyl acetate in
an RDC. The effect of various parameters, e.g. total feed flowrate, length of catalytic section, reflux ratio, mole ratio of the
reactants, location of feed points and effect of recycle of water were studied，
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稀醋酸回收在醋酸裂解制醋酐的装置中都有，是早已工业化的生产工艺。
好像大家对已经工业化的生产工艺不了解。
工艺过程如下：
1.萃取
乙酸乙酯、醋酸稀分别进入萃取塔，乙酯进塔底、稀酸进塔顶
2.共沸精馏
出萃取塔顶的萃取相进入共沸精馏塔中上部，塔顶得到合格的醋酸塔顶乙酸乙酯、水共沸物冷凝后分层，酯层作为进入萃取塔的原料，酯水层进入酯水分离塔。
3.酯水分离塔
共沸精馏塔顶冷凝后分层的酯水层进入酯水分离塔，精馏回收乙酯、塔底排出酸性废水。塔顶含水乙酯进入共沸精馏塔顶冷凝后分层罐。
也有用醋酸丁酯代替醋酸乙酯的，差别在于塔的操作参数不同。
[ Last edited by chinajl123 on 2007-5-11 at 10:05 ]
酯化法可以考虑用稀乙酸和甲醇反应。相比于乙醇，甲醇的酯化更容易。有文献报道，10%（wt%）乙酸和甲醇酯化，乙酸转化率可达80%以上。
正解 目前这是最好的办法了 我们这里就可以做 渗透蒸发不是工业化可以应用的方法 膜就是一大问题 提出降温办法的估计没有好好思考 随口说的吧
络合萃取乙酸再蒸馏的方法还没有工业应用，主要是乙酸本身的经济价值不高，对于渗透蒸发处理乙酸水溶液的效果不是很好，由于有机酸易电离的性质，渗透蒸发对这类体系的分离因子不是很高。
使用渗透汽化过程可以实现低浓度的醋酸/水的分离!
渗透汽化仅是一种待改善的技术，尽管有很多优点，但还是不太成熟，目前还处于忽悠国家钱的地位。醋酸和水的分离可以参考醋酸生产过程中的分离过程和对二苯甲酸生产过程中的分离过程，均为精馏法，具体是萃取精馏还是共沸精馏，楼主可以看看这方面的文献，太多了。
请教12楼的朋友：降温在理论上说得过去的，工业上哪些方面不妥？
Recovery of dilute acetic acid through
esterification in a reactive distillation column
The recovery of acetic acid from its dilute aqueous solutions is a major problem in both petrochemical and fine chemical
industries. The conventional methods of recovery are azeotropic distillation, simple distillation and liquid–liquid extraction.
Physical separations such as distillation and extraction suffer from several drawbacks. The esterification of an aqueous solution
(30%) of acetic acid with n-butanol/iso-amyl alcohol is a reversible reaction. As excess of water is present in the reaction
mixture, the conversion is greatly restricted by the equilibrium limitations. The esters of acetic acid, namely, n-butyl acetate
and iso-amyl acetate, have a wide range of applications. In view of the appreciable value of these esters, the present work was
directed towards recovery of 30% acetic acid by reaction with n-butanol and iso-amyl alcohol in a reactive distillation column
(RDC) using macroporous ion-exchange resin, Indion 130, as a catalyst bed, confined in stainless steel wire cages. Experiments
were conducted in order to achieve an optimum column configuration for the synthesis of n-butyl acetate/iso-amyl acetate in
an RDC. The effect of various parameters, e.g. total feed flowrate, length of catalytic section, reflux ratio, mole ratio of the
reactants, location of feed points and effect of recycle of water were studied，