CN105175260B - 醋酸仲丁酯—异丁醇共沸混合物连续萃取精馏分离方法 - Google Patents

醋酸仲丁酯—异丁醇共沸混合物连续萃取精馏分离方法 Download PDF

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CN105175260B
CN105175260B CN201510335515.1A CN201510335515A CN105175260B CN 105175260 B CN105175260 B CN 105175260B CN 201510335515 A CN201510335515 A CN 201510335515A CN 105175260 B CN105175260 B CN 105175260B
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extractant
butyl acetate
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isobutanol
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马守涛
孙国新
姜占坤
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University of Jinan
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/48—Separation; Purification; Stabilisation; Use of additives
    • C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/48—Separation; Purification; Stabilisation; Use of additives
    • C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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Abstract

本发明公开了一种醋酸仲丁酯—异丁醇共沸混合物的连续萃取精馏分离方法。该方法以丙二醇，丁二醇或以任意比例组成的混合物，萃取精馏塔的操作条件，萃取剂与进料的质量比为0.5:1‑10:1，控制连续萃取精馏塔和溶剂回收塔塔顶不同温度和不同回流比，由萃取精馏塔塔顶采出异丁醇，溶剂回收塔塔顶采出醋酸仲丁酯，塔底的萃取剂进入到萃取精馏塔中循环使用。本发明的优点在于用萃取剂破坏醋酸仲丁酯—异丁醇共沸体系，分离出高纯醋酸仲丁酯、异丁醇产品。连续精馏效率高，产率大，溶剂回收简单。

Description

醋酸仲丁酯—异丁醇共沸混合物连续萃取精馏分离方法
技术领域
本发明涉及一种醋酸仲丁酯—异丁醇共沸混合物的连续萃取精馏分离方法，属于醋酸仲丁酯—异丁醇共沸混合物的分离技术。
背景技术
萃取精馏是一种特殊精馏分离技术，适用于共沸体系的分离。通过往精馏塔的顶部连续加入萃取剂以改变原组分的相对挥发度来达到分离的目的。连续萃取精馏融合连续精馏和萃取精馏的优点，具有操作灵活，分离能力大，效率高等特点，适用于大批量共沸体系和近沸体系的分离。醋酸仲丁酯的化学结构式为：C6H12O，工业上应用广泛。醋酸仲丁酯(SBAC)属于乙酸丁酯的四种同分异构体之一，为无色，易燃，带有水果香味的液体，并且可以溶解多种树脂和有机物。醋酸仲丁酯广泛应用于医药、涂料、油墨、胶黏剂、固化剂、清洗剂、稀释剂、树脂生产和乙酸脱水等行业中。对于乙酸脱水工业生产上目前主要采用乙酸乙酯、乙酸异丙酯、乙酸丁酯、乙酸异丁酯作为萃取剂或共沸剂。作为乙酸丁酯的同分异构体醋酸仲丁酯替代以上酯类有着能耗低、性价比高、溶剂损耗小、毒性低、替换工艺简单等优点，因此醋酸仲丁酯有可能替代以上几种酯类成为新的乙酸废水回收的溶剂。而工业上用乙酸与仲丁醇生产醋酸仲丁酯时，在原料中常常混有异丁醇，且醋酸仲丁酯与仲丁醇会产生共沸，这对后期产品与原料的分离产生了一定的困难，因此开发醋酸仲丁酯—异丁醇共沸混合物的分离方法具有重要的意义。有关萃取精馏方面的文章和专利很多，尚未公开发表甲醋酸仲丁酯—异丁醇共沸体系萃取精馏分离方面的资料。
发明内容
本发明的目的在于提供一种醋酸仲丁酯—异丁醇共沸混合物连续萃取精馏分离方法，该方法分离出的醋酸仲丁酯、异丁醇产品纯度高。
本发明是通过下述技术方案加以实现的。采用包括萃取精馏塔、溶剂回收塔、加热釜、冷凝器、产品罐和泵构成的连续萃取精馏装置，连续萃取精馏分离醋酸仲丁酯—异丁醇共沸混合物，其特征包括以下过程：以丙二醇、丁二醇或二者以任意比例组成的混合物为萃取剂，萃取精馏塔和溶剂回收塔在以下条件下进行操作，在常压或减压进入萃取精馏塔的萃取剂与进料比例为0.5:1-10:1，原料从萃取精馏塔的下部进入，萃取剂从萃取精馏塔的上部进入，进料的温度为20-60℃，萃取剂的温度为50-80℃；当塔顶温度为100-120℃时，塔顶馏出物为异丁醇，回流比为3:1-10:1，馏出物进入产品罐V-0101，塔底温度为130-150℃时，将醋酸仲丁酯—萃取剂馏出物进入溶剂回收塔，进料温度为20-60℃，从塔的中部进料，当溶剂回收塔塔顶温度为110-130℃时，控制回流比为3:1-10:1，由塔顶采出醋酸仲丁酯，进入产品罐V-0102；当塔底的温度为高于140℃时塔底采出纯度较高的萃取剂，再沸比为5:1-10:1，馏出的萃取剂用泵进入萃取精馏塔循环使用。从而能进行连续萃取精馏分离。
具体流程（见附图）：将醋酸仲丁酯—异丁醇混合物加入到加热釜中，开启加热釜的热源和冷凝水，待萃取精馏塔顶有回流并且塔顶温度稳定后，萃取剂从塔的上部进入萃取精馏塔，当塔顶产品的纯度达到要求时，塔顶采出的异丁醇进入产品罐，塔底馏出的醋酸仲丁酯—萃取剂进入溶剂回收塔的中部，当溶剂回收塔的塔釜内液位达到二分之一时，开启溶剂回收塔的加热釜的热源和冷凝水。当溶剂回收塔的塔顶温度稳定后，塔顶馏出的醋酸仲丁酯产品进入产品罐，塔底馏出的萃取剂与新鲜的萃取剂进入萃取精馏塔的上部，原料一直不断的进入萃取精馏塔。从而达到连续精馏分离的最佳运行状态。
本发明的优点在于使用合理有效的萃取剂破坏醋酸仲丁酯—异丁醇共沸体系，分离出高纯度的醋酸仲丁酯、异丁醇，采用连续萃取精馏，分离效果好，产率大。
附图说明
图1 连续萃取精馏装置：T-0101 萃取精馏塔，T-0102溶剂回收塔，E-0101萃取精馏塔塔顶冷凝器、E-0102萃取精馏塔塔底再沸器、E-0103溶剂回收塔塔顶冷凝器、E-0104溶剂回收塔塔底再沸器、V-0101萃取精馏塔塔顶储罐、V-0102溶剂回收塔塔顶储罐、P-0101溶剂回收塔回流泵。
具体实施方式
实施例1：采用连续精馏装置，在萃取精馏塔的加热釜中投入共沸混合物醋酸仲丁酯—异丁醇500L（其中异丁醇为76%，醋酸仲丁酯为24%，均为摩尔百分数），试验所选的萃取剂为丙二醇，开启萃取精馏塔的热源和冷凝器的冷凝水，待萃取精馏塔塔顶温度稳定后，回流一段时间，在萃取精馏塔的上部加入萃取剂丙二醇，萃取剂与进料的比为2:5，当萃取精馏塔的温度为100-120℃时，将在萃取精馏塔塔顶馏出异丁醇产品，回流比为3:1。萃取精馏塔的塔底温度为130-150℃时，将塔底馏出的醋酸仲丁酯—萃取剂引入到溶剂回收塔的上部，再沸比为1:5，此时向萃取精馏塔中连续加入原料和萃取剂，进料速度分别为100L/h、40L/h。溶剂回收塔塔顶有回流且温度保持在110-130℃基本不变时，塔顶采出醋酸仲丁酯。采出的回流比为2:1；当溶剂回收塔塔底温度高于140℃时，由塔底馏出纯度较高的萃取剂用泵打入到萃取精馏塔，从达到连续精馏分离的目的。
实施例2：实验装置和操作方法同实施例1，萃取剂采用丁二醇
实施例3：实验装置和操作方法同实施例1，萃取剂采用丙二醇和丁二醇的等体积混合物。

Claims (2)

1.一种醋酸仲丁酯—异丁醇共沸混合物的连续萃取精馏分离方法，该方法采用包括萃取精馏塔、溶剂回收塔、加热釜、冷凝器和产品罐构成的萃取精馏装置，以丙二醇、丁二醇或二者以任意比例混合物为萃取剂, 连续萃取精馏分离醋酸仲丁酯—异丁醇共沸混合物。
2.如权利要求1所述的一种醋酸仲丁酯—异丁醇共沸混合物连续萃取精馏分离方法，其特征包括以下过程：萃取精馏塔和溶剂回收塔在以下条件下进行操作：在常压或减压进入萃取精馏塔的萃取剂与原料进料比例为0.5:1-10:1，原料从萃取精馏塔的下部进入，萃取剂从萃取精馏塔的上部进入，原料进料的温度为20-60℃，萃取剂的温度为50-80℃；当塔顶温度为100-120℃时，塔顶馏出物为异丁醇，回流比为3:1-10:1，馏出物进入产品罐V-0101，塔底温度为130-150℃时，将醋酸仲丁酯-萃取剂馏出物进入溶剂回收塔，醋酸仲丁酯-萃取剂馏出物进料温度为20-60℃，从塔的中部进料，当溶剂回收塔塔顶温度为110-130℃时，控制回流比为3:1-10:1，由塔顶采出醋酸仲丁酯，进入产品罐V-0102；当塔底的温度高于140℃时塔底采出纯度较高的萃取剂，再沸比为5:1-10:1，馏出的萃取剂用泵进入萃取精馏塔循环使用，从而能进行连续萃取精馏分离。
CN201510335515.1A 2015-06-17 2015-06-17 醋酸仲丁酯—异丁醇共沸混合物连续萃取精馏分离方法 Expired - Fee Related CN105175260B (zh)

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CN105968006B (zh) * 2016-05-24 2019-01-25 济南大学 一种乙酸丙酯-烯丙醇混合物的分离方法
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