CN113717051A - 一种乙酸丁酯的制备方法 - Google Patents
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Abstract
本发明提供了一种乙酸丁酯的制备方法，原料乙酸、丁醇及回收酯经计量放入酯化釜，在催化剂的作用下，通过蒸汽加热，生成乙酸丁酯和水，并在酯化塔内形成共沸物，从塔顶蒸出，经冷凝冷却后，进入分离器进行分离，经精馏从塔顶组分中分离出醇、水、酯混合物，经过冷凝器冷却后，进入分离器分离，酯相进入精馏缓冲槽，得到的头酯的一部分返回酯化塔，另一部分重回流到精馏塔里；水相进入回收塔，精馏塔底得到酯含量、酸度、水分都合格的成品，经冷却后进入计量槽。所述水相为含有酯和醇的废水，进入回收塔后，经蒸馏分离，从塔顶回收得到一定含量的头酯，头酯返回酯化塔，回收后的废水从塔底排掉。
Description
技术领域
本发明涉及一种乙酸丁酯的制备方法。
背景技术
乙酸丁酯是是优良的有机溶剂，广泛用于硝化纤维清漆中，在人造革、织物及塑料加工过程中用作溶剂，也用于香料工业。作为香料，大量用于配制香蕉、梨、菠萝、杏、桃及草莓、浆果等型香精。亦可用作天然胶和合成树脂等的溶剂。偶用于果香型香精中，主要取其扩散力好的性能，更适宜作头香香料使用，但用量宜少，以免单独突出而影响效果。可大量用于如杏子、香蕉、桃子、生梨、凤梨、悬钩子、草莓等食用香精中。、优良的有机溶剂，对醋酸丁酸纤维素、乙基纤维素、氯化橡胶、聚苯乙烯、甲基丙烯酸树脂以及许多天然树脂如栲胶、马尼拉胶、达玛树脂等均有良好的溶解性能。广泛应用于硝化纤维清漆中，在人造革、织物及塑料加工过程中用作溶剂，在各种石油加工和制药过程中用作萃取剂，也用于香料复配及杏、香蕉、梨、菠萝等各种香味剂的成分。用于火棉胶、硝化纤维、清漆、人造革、医药、塑料及香料工业中.是一种优良的有机溶剂，能够溶解松香、聚醋酸乙烯、聚丙烯酸酯、聚氯乙烯、氯化橡胶、杜仲胶、聚甲基丙烯酸甲酯等。胡倩合成乙酸丁酯的方法主要存在以下不足：1、采用浓硫酸做催化剂，虽然反应活性快，但存在着设备腐蚀严重、副反应多的缺点；回流有机相中水含量较高，常用成品乙酸丁酯带水，浪费了成品产量。
发明内容
本发明提供了一种乙酸丁酯的制备方法，原料乙酸、丁醇及回收酯经计量放入酯化釜，在催化剂的作用下，通过蒸汽加热，生成乙酸丁酯和水，并在酯化塔内形成共沸物，从塔顶蒸出，经冷凝冷却后，进入分离器进行分离，水相一部分回流，一部分进入回收塔以回收所溶解的酯和醇，酯相一部分回流到酯化塔，其余进入粗酯缓冲槽预热后，进入精馏塔，经精馏从塔顶组分中分离出醇、水、酯混合物，经过冷凝器冷却后，进入分离器分离，酯相进入精馏缓冲槽，得到的头酯的一部分返回酯化塔，另一部分重回流到精馏塔里；水相进入回收塔，精馏塔底得到酯含量、酸度、水分都合格的成品，经冷却后进入计量槽。所述水相为含有酯和醇的废水，进入回收塔后，经蒸馏分离，从塔顶回收得到一定含量的头酯，头酯返回酯化塔，回收后的废水从塔底排掉。具体的方案如下：
一种乙酸丁酯的制备方法，步骤如下：
1)原料乙酸、丁醇及回收酯经计量放入酯化釜；
2)在催化剂的作用下，通过蒸汽加热，生成乙酸丁酯和水，并在酯化塔内形成共沸物，从塔顶蒸出；
3)经冷凝冷却后，进入分离器进行分离，水相一部分回流，一部分进入回收塔以回收所溶解的酯和醇，酯相一部分回流到酯化塔，其余进入粗酯缓冲槽预热后，进入精馏塔；
4)经精馏从塔顶组分中分离出醇、水、酯混合物，经过冷凝器冷却后，进入分离器分离，酯相进入精馏缓冲槽，得到的头酯的一部分返回酯化塔，另一部分重回流到精馏塔里；水相进入回收塔；
5)精馏塔底得到酯含量、酸度、水分都合格的成品，经冷却后进入计量槽；
6)所述水相为含有酯和醇的废水，进入回收塔后，经蒸馏分离，从塔顶回收得到一定含量的头酯，头酯返回酯化塔，回收后的废水从塔底排掉。
进一步的，所述酯化塔内的温度T(℃)为115-125摄氏度，压力P(MPa)为0.2-0.5MPa。
进一步的，所述催化剂为强酸性大孔阳离子交换树脂Amberlyst-15和Zr(SO4)2/TiO2固体酸的混合物，其中Amberlyst-15和Zr(SO4)2/TiO2的质量比为m:1，且所述酯化塔内的温度T和压力P满足以下关系式，0.61*m＝(R+9.6*P)/T。
进一步的，其中R＝95-97，m＝1.36-1.38。
本发明具有如下有益效果：
1)、通过本发明的工艺步骤，乙酸丁酯的产率和选择性高，充分利用各工艺步骤中的产物进行回收利用，操作简单，成本低廉；
2)、进一步的发明人发现，采用复合催化剂代替浓硫酸催化剂，能够避免浓硫酸对于设备的腐蚀，并且乙酸的转化率(％)和乙酸丁酯的选择性(％)相比较浓硫酸作为催化剂更高；
3)、进一步发明人发现，针对特定的催化剂，控制酯化塔内的压力和温度，使其满足特定的关系式时，0.61*m＝(R+9.6*P)/T，其乙酸的转化率(％)和乙酸丁酯的选择性(％)非常高。
附图说明
图1为乙酸丁酯的生产工艺流程图
具体实施方式
本发明下面将通过具体的实施例进行更详细的描述，但本发明的保护范围并不受限于这些实施例。
实施例
1)原料乙酸、丁醇及回收酯经计量放入酯化釜；
2)在催化剂的作用下，通过蒸汽加热，生成乙酸丁酯和水，并在酯化塔内形成共沸物，从塔顶蒸出；
3)经冷凝冷却后，进入分离器进行分离，水相一部分回流，一部分进入回收塔以回收所溶解的酯和醇，酯相一部分回流到酯化塔，其余进入粗酯缓冲槽预热后，进入精馏塔；
4)经精馏从塔顶组分中分离出醇、水、酯混合物，经过冷凝器冷却后，进入分离器分离，酯相进入精馏缓冲槽，得到的头酯的一部分返回酯化塔，另一部分重回流到精馏塔里；水相进入回收塔；
5)精馏塔底得到酯含量、酸度、水分都合格的成品，经冷却后进入计量槽；
6)所述水相为含有酯和醇的废水，进入回收塔后，经蒸馏分离，从塔顶回收得到一定含量的头酯，头酯返回酯化塔，回收后的废水从塔底排掉。
所述催化剂为强酸性大孔阳离子交换树脂Amberlyst-15和Zr(SO4)2/TiO2固体酸的混合物，其中Amberlyst-15和Zr(SO4)2/TiO2的质量比m：1，m为1.36-1.38，催化剂用量为醇用量的1wt％。
所述酯化塔内的温度T(℃)为115-125摄氏度，压力P(MPa)为0.2-0.5MPa，且满足以下关系式，0.61*m＝(R+9.6*P)/T，其中R＝95-97。
乙酸的转化率(％)＝(乙酸的用量-反应产物中乙酸的含量)÷乙酸的用量×100％
乙酸丁酯的选择性(％)＝乙酸丁酯的实际产量÷乙酸丁酯的理论产量×100％
实施例和对比例的实验数据见表1
表1
尽管本发明的内容已经通过上述优选实施例作了详细介绍，但是应当认识到上述的描述不应被认为是对本发明的限制。
Claims (4)
1.一种乙酸丁酯的制备方法，步骤如下：
1)原料乙酸、丁醇及回收酯经计量放入酯化釜；
2)在催化剂的作用下，通过蒸汽加热，生成乙酸丁酯和水，并在酯化塔内形成共沸物，从塔顶蒸出；
3)经冷凝冷却后，进入分离器进行分离，水相一部分回流，一部分进入回收塔以回收所溶解的酯和醇，酯相一部分回流到酯化塔，其余进入粗酯缓冲槽预热后，进入精馏塔；
4)经精馏从塔顶组分中分离出醇、水、酯混合物，经过冷凝器冷却后，进入分离器分离，酯相进入精馏缓冲槽，得到的头酯的一部分返回酯化塔，另一部分重回流到精馏塔里；水相进入回收塔；
5)精馏塔底得到酯含量、酸度、水分都合格的成品，经冷却后进入计量槽；
6)所述水相为含有酯和醇的废水，进入回收塔后，经蒸馏分离，从塔顶回收得到一定含量的头酯，头酯返回酯化塔，回收后的废水从塔底排掉。
2.如上述权利要求1所述的制备方法，所述酯化塔内的温度T(℃)为115-125摄氏度，压力P(MPa)为0.2-0.5MPa。
3.如上述权利要求2所述的制备方法，所述催化剂为强酸性大孔阳离子交换树脂Amberlyst-15和Zr(SO4)2/TiO2固体酸的混合物，其中Amberlyst-15和Zr(SO4)2/TiO2的质量比为m:1，且所述酯化塔内的温度T和压力P满足以下关系式，0.61*m＝(R+9.6*P)/T。
4.如上述权利要求所述的制备方法，其中R＝95-97，m＝1.36-1.38。
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