CN1433395A - 生产乙酸乙酯的方法和实施该方法的设备 - Google Patents

生产乙酸乙酯的方法和实施该方法的设备 Download PDF

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CN1433395A
CN1433395A CN00814099A CN00814099A CN1433395A CN 1433395 A CN1433395 A CN 1433395A CN 00814099 A CN00814099 A CN 00814099A CN 00814099 A CN00814099 A CN 00814099A CN 1433395 A CN1433395 A CN 1433395A
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J·科莱纳
J·莱德雷尔
P·莫拉维克
J·哈尼卡
Q·斯梅卡
D·斯卡拉
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Abstract

本发明涉及一种生产乙酸乙酯的方法，该方法是在固体酸性催化剂的存在下，在同时蒸馏分离反应组分期间通过乙醇与乙酸和/或乙酸酐的反应进行的，其中将乙酸或乙酸酐或其混合物与乙醇以2∶1－1∶2.5的摩尔比、以基于催化剂的体积单位一定的量分别引进分成三个区的体系，在反应区内，反应与各组分的蒸馏分离同时进行，乙酸进料被引入反应区或该区上面，乙醇进料被引入反应区或该区下面，在上部分离区，将挥发性混合物分离，然后将其冷却至5－70℃，再将其分离为水和有机相，将具有高乙酸乙酯含量的有机相排出，并将其一部分作为回流返回体系，由此输入组分进料与有机相回流的比例为1∶1－1∶20。本发明的一个主题是实施该方法的装置。

Description

生产乙酸乙酯的方法和实施该方法的设备
发明领域
本发明涉及通过乙酸与乙醇的酯化或者通过乙酸酐与乙醇的反应合成乙酸乙酯的方法，该方法采取在塔内的催化蒸馏，催化蒸馏期间，同时发生在催化活性填料上的反应和反应产物的精馏分离。本发明还涉及实施该方法的设备。
发明背景
乙酸乙酯是通过乙醇和乙酸的反应制备的，该反应除生成乙酸乙酯外，还生成水。或者，乙酸乙酯可以通过乙酸酐与乙醇的反应进行制备，该反应中除乙酸乙酯外，还生成乙酸。生成的乙酸进一步被另一部分乙醇酯化。酯化是一个平衡反应，它通过酸催化剂的存在被促进。因此，主要使用无机酸，优选硫酸或作为其改进的固体酸性催化剂。所述酸性催化剂主要是酸性离子交换剂，或者最终是沸石，或者所谓的固体超酸等。
按照先有技术的方法，通常在反应器内进行反应，从而得到反应混合物的接近平衡的组合物，所述组合物取决于反应组分的起始摩尔比。将由此得到的混合物在蒸馏塔内精馏，蒸馏出具有接近于包含乙醇、乙酸乙酯和水的三元多相共沸物的组成的混合物。因为该反应所生成的水量大于以共沸物的形式被蒸馏的水量，所以将过量水与未反应的乙酸一起从塔沸腾器中排出。由此获得的乙酸必须通过另一蒸馏而再生。接下来，是对由此得到的三元共沸物的有机相进行蒸馏分离，即首先从乙酸乙酯中分离未反应的乙醇，当然需要考虑到这是一个实际上非理想的混合物，其中乙醇和乙酸乙酯形成二元共沸物，此外再与具有最低沸点的水形成三元共沸物。然后通过另一蒸馏塔从分离自第一个塔馏出物的水相蒸馏出溶解的乙酸乙酯和乙醇，再将该醇与乙酸酯的混合物返回到上述工艺中。分离酯化反应组分的方法比较复杂是上述先有技术方法的主要缺点。在使用无机酸作为催化剂的方法中，注意到还有明显的环境和腐蚀问题。
原则上，还已知乙酸的酯化可以在蒸馏塔内、在没有催化剂(chem.Eng.Technol.1997，20，182)或加入均相催化剂即无机酸和一种反应组分(Chemia Stosowana 1989，33，509)的条件下通过乙醇进行。还公开了间歇式塔的使用，所述塔用酸性离子交换剂粒子进行填充，因此这些粒子既作为催化剂也作为塔填料(Separation Science and Technology1992，27，613)。当然，非催化酯化的速率太低无法应用到工业上。使用均相催化剂进料的活性蒸馏带来上述腐蚀问题和对环境的不利之处。填充了酸性催化剂的自由粒子的蒸馏塔由于流体动力学抵抗性高、分离效率差，因而不适用于工业生产。
因此，本发明的目的在于消除先有技术方法的缺点。
发明简述
依照本发明，通过乙醇与乙酸和/或乙酸酐的反应生产乙酸乙酯的方法的要点是：在固体酸性催化剂的存在下，在同时蒸馏分离反应组分期间，将乙酸或乙酸酐或其混合物与乙醇以2∶1-1∶2.5的摩尔比、以用引进的组分基于催化剂体积单位的总流量为0.1-10/小时表示的量分别引进体系，在该体系中，反应和蒸馏分离在三个区内进行，在反应区内，反应与具有不同沸点组分的蒸馏分离同时进行，在两个分离区内，只发生组分的蒸馏分离，由此作为反应副产物产生的水与乙酸乙酯形成低沸点的共沸混合物，从体系中被完全或部分蒸馏。之后，将馏出物冷却至5-70℃，然后将水从乙酸乙酯和馏出物的其它有机组分中分离，并从体系中排出，而主要含有粗乙酸乙酯的馏出物的有机组分被部分返回作为回流，由此将乙酸和/或乙酸酐的进料流与乙醇进料引进体系，以使乙酸和/或乙酸酐进料被引进反应区或在该区上面进入位于乙醇进料处上方的位置，乙醇进料被引进反应区或该区下面，引进塔中的原料组分进料与进入塔顶的有机相回流的比例为1∶1-1∶20，可含有一部分由化学反应所生成的水的、未以馏出物的形式被分离的残余未反应乙酸作为高沸点塔底组分被分离。作为催化剂，可以使用酸性离子交换剂如磺化苯乙烯-二乙烯基苯共聚物，该共聚物含有1-25％重量二乙烯基苯，酸度为1-10毫当量(H+)/g。但是，也可以使用任何其它酸性离子交换树脂或例如酸性沸石和其它已知的酸性催化剂。
本方法的优选实施方案在保持下述特征的情况下进行操作：乙酸与乙醇的摩尔比为1∶1-1∶0.45，或者乙酸酐与乙醇的摩尔比为1∶2-1∶1.5；基于催化剂单位体积，引进组分的进料流量为0.5-5/小时；引进反应的进料组分与有机相回流的比例为1∶1-1∶20。可以使用乙酸或乙酸酐与乙醇的部分反应混合物代替纯的乙酸或乙酸酐进料或其混合物，从而含有乙酸的进料流还可以含有乙酸乙酯和/或水和/或未反应乙醇。
本发明的方法用下述设备进行：该设备包括由三个区组成的塔，其中反应区位于塔的中部，反应区中装有固定在蒸馏塔板上的固体酸性催化剂，或者在优选的实施方案中，固体酸性催化剂固定在已知类型的具有内部槽结构的定向填料上，其中催化剂被固定在形成填料结构的惰性多孔物质的层间，底部分离区和顶部分离区包括惰性浇注填料(inert poured packings)，该惰性浇注填料是已知图样的结构定向填料或蒸馏内置部件，乙酸和/或乙酸酐进料管线连接到反应区的上部或该区上方，乙醇进料管线连接到反应区的底部或该区下方，塔底配备有一个沸腾器，在塔沸腾器中或在塔底排出未反应的乙酸，塔的上部以一个顶结束，所述顶装有一条将馏出蒸汽排入冷凝器的管线，冷凝馏出物管线将冷凝馏出物转移到分离器中，分离器上装有排出管线用于底部馏出水相的移出，还装有用于排放回流的出口管线，以及用于排出馏出有机相的出口管线。
从上述对本发明的描述可以明显看出，本发明的方法使原料组分可能以高于平衡的接近100％的转化率向乙酸乙酯和水转化。特别是如果将乙醇以稍微不足化学计量的量加进体系，则乙醇几乎全部转化为乙酸乙酯，然后以与水易于分离的混合物的形式得到该乙酸乙酯。分离区实现从原料组分即乙酸和乙醇分离反应产物即乙酸乙酯和水的功能，并将所述原料组分返回反应区，由此乙酸乙酯与水一起作为馏出物被连续分离，从该馏出物的有机相分离之后，将主要含乙酸乙酯的水相从体系分离，馏出物的有机部分的一部分作为回流被返回塔内，一部分被排出。
可以将输入组分即乙酸或乙酸酐和乙醇以化学计量比例或以乙酸和/或乙酸酐的摩尔过量装进反应区，以转化几乎全部乙醇。如果本发明方法在大气压下进行，则塔的温度模式是稳定的，以使塔顶温度达到70-74℃。将原料组分加入塔中，使乙醇进入塔的位置低于乙酸和/或乙酸酐进料的位置。在本方法的普通实施方案中，在催化区之下或在其下部加入乙醇。另一方面，将包含乙酸或乙酸酐的进料加入到该区之上或其上部。
离开塔顶的蒸汽冷凝产生混合物，将该混合物冷却至70-5℃，然后分离为水和有机相，由此主要含乙酸乙酯的有机相的一部分作为回流被返回塔顶，另一部分被排出。本发明方法的一个具体特点在于馏出物中乙醇含量低，该含量低于乙酸乙酯-乙醇-水三元共沸物中对应的浓度。这一事实明显促进了随后通过要求不是非常高的蒸馏将馏出产物最终提纯为商业纯度。排出含大量溶解的乙酸乙酯和最后的乙醇的水相。可将溶解的酯和醇从该相中汽提出来，并可以将两种组分都返回该工艺中。从塔沸腾器连续排出过量乙酸。本发明的方法有可能将化学反应产生的所有水以馏出物的形式分离，或者从该体系中将一部分水作为底部产物与未反应的残留乙酸一起排出。
附图简述
附图1为实施本发明方法的装置的示意图。
发明详述
图1的装置包括由3个区组成的塔 1，位于塔 1中部的反应区 2中装有固体催化剂，底部分离区 3和上部分离区 4装有定向填料、惰性浇注填料或蒸馏内置部件。乙酸和/或乙酸酐进料管线 5安装在反应区 2的上部或该区之上，乙醇进料管线 6被连接到反应区 2的底部或该区之下。塔 1的底部以塔底 7结束，该塔底 7配备有沸腾器 8。未反应乙酸排出管线 9与沸腾器 8相连。该塔 1的上部以塔顶10结束。该塔顶 10配备有馏出蒸汽排出管线 11，该管 11将所述蒸汽输送到冷凝器 12。冷凝馏出物的排出管线 13使冷凝器 12与分离器 14相连。该分离器 14的底部装有馏出水相排出管线 15，分离器14的上部装有回流管线 16和非回流馏出有机相即乙酸乙酯排出管线17。
本发明的方法在上述装置中实施，从而乙酸和/或乙酸酐或它们与乙酸乙酯和/或水和/或乙醇的混合物进料通过管线 5进入上部分离区 4的底部或者进入反应区 2的上部，同时乙醇进料通过管线 6进入底部分离区 3的上部或者进入反应区 2的底部，这样含水、乙酸乙酯和残余未反应乙醇的馏出蒸汽从塔顶 10被排出，并进入冷凝器12，然后将它们进一步以冷凝馏出物的形式从冷凝器 12转移至分离器 14，在此馏出水相与馏出有机组分分离。然后将有机组分从分离器 14返回塔 1。本发明实施方案的例子 实施例1
图1表示本发明装置的示意图。在常压下连续操作的催化蒸馏塔 1被分成3个区。塔 1的中部形成反应区 2。在反应区 2下面是底部分离区 3，在反应区 2上面是上部分离区 4。沸腾器 8与塔底 7相连。冷凝器 12与塔顶 10相连。分离器 14与冷凝器 12相连。
反应区 2中填装有含33g乙酸离子交换剂的催化活性填料。浇注填料被填装在底部分离区 3和上部分离区 4中(直径4mm的弧鞍形填料)。分离区 3和 4的长度为0.5m。
本生产方法在于：乙醇进料通过管线 6进入底部分离区 3，乙酸进料通过管线 5进入上部分离区 4。上述两种原料的流量均为0.25mol/小时。馏出蒸汽通过管线 11从塔顶 10被排出，并被转移至冷凝器 12。冷凝馏出物通过管线 13从冷凝器 12进入分离器 14。所生成的反应水以4.2g/小时的流量、以馏出水相的形式通过管 15从分离器 14排出，馏出共沸物的有机相以21g/小时的流量作为粗乙酸乙酯被排出，大部分该有机相作为回流通过管线 16被返回塔 1。未反应乙酸以1.2g/小时的流量通过排出管线 9从沸腾器 8排出，从而在沸腾器 8中保持恒定含量。该配置的反应转化率为92％。实施例2
除原料用乙酸酐代替乙酸外，在与实施例1相同的条件下实施乙酸乙酯合成，所述乙酸酐在预反应器中以等摩尔比与乙醇反应生成乙酸和乙酸乙酯。然后将反应混合物加入到塔 1中代替乙酸。乙醇与乙酸酐的经选择的总摩尔比为1.52。使用回流比1∶6，装置输出0.46mol/小时粗乙酸乙酯，其纯度为91.4％重量。除乙酸乙酯外，产物仅含5.2％重量水和3.4％重量乙醇。分离器 14中分离水相的输出量为3.9ml/小时。实施例3
用包括具有50升容积的沸腾器 8、装有冷凝器 12和分离器 14的塔 1的装置实施由乙酸引起的乙醇酯化。催化蒸馏塔 1包括反应区 2，反应区 2中装有催化活性填料KATAPAKS，该填料具有1.07kg H+形式的酸性离子交换剂。底部分离区 3和上部分离区 4中填装有效率为12的定向填料(底部分离区)，即20块理论塔板。将乙酸以0.73kg/小时的量通过管线 5输送进反应区 2，将乙醇以0.41kg/小时的量通过管线 6输送进底部分离区 3的上边界。将由该反应产生的水从分离器 14通过管线 15排放，将有机相通过管 16回流进塔 1，一部分有机相(0.86kg/小时)作为粗乙酸乙酯通过管 17被排出。通过从管线 9排出未反应乙酸，维持沸腾器 8中的恒定保留。除乙酸乙酯外，产物还含有0.003％重量乙酸、1.4％重量乙醇和1.43％重量水。实施例4
除进料流 5含有66.6％重量乙酸、0.8％重量乙醇、25.4％重量乙酸乙酯和7.2％重量水外，装置和方法皆与实施例3相同。进料速率为0.843kg/小时。通过使乙酸和乙醇混合物通过常规设计的、装有酸性离子交换剂的反应器，使其预先发生部分反应，以获得所述组成的进料。然后以0.84kg/小时的流量从分离器 14排出乙酸乙酯。该纯度为96.1％重量的乙酸乙酯含有2.6％重量水和0.5％重量乙醇。通过气相色谱法未曾发现产物中有乙酸存在。
工业应用
本发明将在化学工业中有用。所获得的产物主要作为生产和使用涂料时的溶剂，以及作为药学和生物技术中的萃取剂。

Claims (9)

1.一种生产乙酸乙酯的方法，该方法是在固体酸性催化剂的存在下、在同时蒸馏分离反应组分期间通过乙醇与乙酸和/或乙酸酐的反应进行的，其特征在于将乙酸或乙酸酐或其混合物与乙醇以2∶1-1∶2.5的摩尔比、以用引进的组分基于催化剂体积单位的总流量为0.1-10/小时表示的量分别引进体系，在该体系中，反应和蒸馏分离在三个区内进行，在反应区内，反应与具有不同沸点组分的蒸馏分离同时进行，在两个分离区内，发生组分的蒸馏分离，由此作为反应副产物产生的水与乙酸乙酯形成低沸点的共沸混合物，从体系中被完全或部分蒸馏，之后将馏出物冷却至5-70℃，然后将水从乙酸乙酯和馏出物的其它有机组分中分离，并从体系中排出，而主要含有粗乙酸乙酯的馏出物的有机组分的一部分作为回流被返回，一部分被排出，将乙醇进料和乙酸或乙酸酐进料或它们的混合物进料引进体系，以使乙酸进料和/或乙酸酐进料和/或它们的混合物进料被引进反应区或在该区上面进入位于乙醇进料处上方的位置，将乙醇进料引进反应区或该区下面，由此引入塔中的原料组分进料与返回反应区的有机相回流的比例为1∶1-1∶20，未反应乙酸作为高沸点底部组分被分离。
2.权利要求1的方法，其特征在于所述原料乙酸或所述原料乙酸酐或它们的混合物也含有乙酸乙酯和/或水和/或乙醇。
3.权利要求1或2的方法，其特征在于将所述乙酸或所述乙酸酐或它们的混合物以与所述乙醇摩尔比为1∶1-1∶0.45的量引进体系。
4.权利要求1或2或3的方法，其特征在于基于催化剂的体积单位，所述被引进的原料组分的总流量为0.5-5/小时。
5.权利要求1或2或3或4的方法，其特征在于所述输入到反应中的组分进料与所述返回反应中的有机相回流的比例为1∶1-1∶20。
6.权利要求1或2或3或4或5的方法，其特征在于作为高沸点底部组分从体系中分离的所述未反应乙酸含有一部分由化学反应所产生的水。
7.一种实施权利要求1-6的方法的装置，其特征在于该装置包括：由三个区组成的塔(1)，其中反应区(2)位于塔(1)的中部，反应区中装有固体酸性催化剂，底部分离区(3)和顶部分离区(4)包含惰性浇注填料、定向填料或蒸馏内置部件，乙酸或乙酸酐进料管线(5)位于反应区(2)的上部或该区上方，乙醇进料管线(6)被引入反应区(2)的底部或该区下方，所述塔(1)的底部以塔底(7)结束，塔底(7)配备有沸腾器(8)，未反应乙酸排出管线(9)从所述沸腾器(8)或所述塔底(7)引出，所述塔(1)的上部以一个顶(10)结束，所述顶(10)装有一个连接到冷凝器(12)的馏出蒸汽排出管线(11)，所述冷凝器(12)通过冷凝馏出物排出管线(13)与分离器(14)相连，所述分离器(14)的底部装有馏出水相排出管线(15)，上部装有回流管(16)和乙酸乙酯排出管线(17)。
8.权利要求7的装置，其特征在于所述固体酸性催化剂坚固地固定在所述反应区(2)中的蒸馏塔板上。
9.权利要求7的装置，其特征在于所述固体酸性催化剂通过处于一个结构中的本身已知的体系固定在所述反应区(2)中，该结构在下述相的逆流移动中使液相和催化剂颗粒接触，还使液体和蒸汽相接触。
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