CN1962718A - 用于制造聚酯的方法和装置 - Google Patents

用于制造聚酯的方法和装置 Download PDF

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CN1962718A
CN1962718A CNA2006101541908A CN200610154190A CN1962718A CN 1962718 A CN1962718 A CN 1962718A CN A2006101541908 A CNA2006101541908 A CN A2006101541908A CN 200610154190 A CN200610154190 A CN 200610154190A CN 1962718 A CN1962718 A CN 1962718A
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B·施塔克
O·胡斯特尔特
G·德姆
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Abstract

本发明涉及一种用于按照直接酯化对苯二甲酸和乙二醇的方法来制造聚酯的改进的方法和改进的装置，其中，在加入搅拌容器之前，在对苯二甲酸加热装置中对粉末状的对苯二甲酸进行预加热。由此可提高设备的生产能力。

Description

用于制造聚酯的方法和装置
技术领域
本发明涉及一种根据权利要求1和8的前序部分所述的、用于按照直接酯化法制造聚酯的方法和装置。在直接酯化法中通过用乙二醇对对苯二甲酸进行直接酯化获得聚酯。在汉堡大学Guido Krause 2003年的论文“Chemisches Recycling von Polyethylentherephthalat undPolymethylmetacrylat”中说明了，直接酯化是当今聚酯制造的优选途径。
背景技术
在专利文献US4110316中说明了一种开头所述类型的方法和装置。为了制造聚酯，在搅拌容器中制造乙二醇和粉末状对苯二甲酸的悬浮体(Aufschlmmung)。泵吸这种乙二醇-对苯二甲酸混合物，并在这里再大气压力下将其加热到280℃至315℃。在酯化反应器中加热所述混合物需要时间。
发明内容
本发明的目的是，这样改善开头所述类型的方法和装置，从而可提高制造设备的产量。
在方法方面，根据本发明通过根据权利要求1的特征来实现所述目的。本发明的核心在于，在加入搅拌容器之前，加热粉末状的对苯二甲酸。由此可降低在酯化反应器中的停留时间，并提高制造设备的产量。
权利要求2说明了，通过间接升温来加热对苯二甲酸。由于不需要采用气体来直接加热，这是特别经济的。气体特别是氮气的制备与这里建议的方法相比是非常复杂的，因为必须用过滤器净化所述气体，或者对于氮气必须安装循环系统。
权利要求3给出了一种不需要移动部件的优选实施形式。
权利要求4给出了对于对苯二甲酸特别合适的加热温度。
权利要求5允许特别经济地进行加热，因为化学设备中常见的蒸汽非常容易获得。
权利要求6允许在惰性气氛下特别经济地进行所述方法，所述惰性气氛基本上由氮气组成。
权利要求7允许连续地和均匀地排空搅拌容器中的散料热交换器。
根据本发明，前面所述涉及装置的目的通过权利要求8来实现。
装置权利要求9和10给出了散料热交换器特别优选的实施形式。
附图说明
从下面根据附图对实施例的说明中可以得出本发明其它的优点、特征和细节。其中：
图1以示意图示出具有对苯二甲酸加热装置的改进的聚酯制造工艺。
具体实施方式
图1所示的对苯二甲酸加热装置具有一接收容器1，用处于氮气气氛下的对苯二甲酸填充所述接收容器。通过输入机构2例如球阀、活门或滑动闸门，可以用对苯二甲酸填充散料热交换器3。
所述散料热交换器3包括一上部缓冲段4，一中部热交换段5和一下部输出段6。所述段4、5和6分别具有圆形横截面。
热交换段5具有一壳体7，在所述壳体的内部空间中分别以一定的距离彼此平行地设置只是用虚线示出的热交换管9。即所述内部空间8是构造成管束的热交换空间。所述热交换管9以其上端固定在入口管底部10中，而以其下端固定在出口管底部11中。即所述内部空间8由管底部10或者说11封闭。
用于蒸汽的输入管接头12直接在入口管底部10的下方通入热交换段5的壳体7的内部空间8。用于冷凝物的排出管接头13直接在出口管底部11的上方从壳体7的内部空间8中通出。内部空间8中可以这样地分别横向于热交换管9的纵向彼此以一定距离地安装有用于支承热交换管9的转向区段，从而通过输入管接头12输入的蒸汽总是横向于热交换管9的纵向曲折地穿过所述内部空间8向下流到排出管接头13。
热交换段5可以不是利用蒸汽而是利用调温液体运行。
在利用蒸汽运行时，适宜的是，保持内部空间8中的压力和温度恒定。为此所需的调节附件和减压阀在图1中没有示出。同样通常连接在排出管接头13上的冷凝物排出口在图1中也没有示出。
通常所述热交换段5设计成如EP0444338B1所示和所说明的那样。在这种情况下，热交换段5由相互平行布置的热交换板组成，在所述热交换板之间有对苯二甲酸。
下部的输出段6设计成向下逐渐变细的锥形漏斗的形状。越过封闭机构14，例如球阀、活门或滑动闸门，通过下降通道15可将粉末状的对苯二甲酸排出到搅拌容器16中。在搅拌容器中有乙二醇。所述液态的乙二醇和粉末状的对苯二甲酸借助于利用马达18驱动的搅拌机构17相混合，接下来利用泵19泵送到图1中未示出的酯化反应器中。
在下文中将说明散料热交换器3不连续的运行方式。通过输入机构2在较短的时间内用粉末状的对苯二甲酸填充散料热交换器3。此时排出机构14关闭。填充过程的终止可以借助填充位置极限报警器20检测，填充过程的特征是用对苯二甲酸填充热交换段5中的热交换管9，所述填充位置极限报警器位于上部的缓冲段4内。填充过程之后，关闭输入机构2。
这样就间接地加热了位于热交换段5中的热交换管9中的对苯二甲酸。停留时间为1至60分钟，优选为3至30分钟。蒸汽温度在120℃至300℃的范围内，优选在140℃至250℃的范围内。此时，在确定的停留时间之后打开排出机构14，并通过下降管道15将加热的对苯二甲酸排出到搅拌容器16中。通过称重单元21确定和平衡(bilanzieren)输送给酯化过程的对苯二甲酸的量。通过另外一个直接在下部管底部11附近安装在下部出口段6中的填充位置极限开关22，关闭排出机构14，由此用已经加热的对苯二甲酸尽可能完全地填满排出段6。除此以外，也可以仅通过称重单元调节填充和排空过程。
在对苯二甲酸的加热过程期间，如果输入机构2和排出机构14都封闭，则散料热交换器3可通过氮气输入管道23泵填。这样的泵填有这样的优点，即可借助于过压加速热交换段5的排空过程。常见的过压在0.05至2bar的范围内，优选在0.05至1bar的范围内。这样在排空时，过压释放到搅拌容器16中，所述搅拌容器通常同样处于氮气气氛下。氮气输入部也可以设置在下部段6中。
在散料热交换器3的排空过程之后，重复上述运行循环，即重新打开输入机构2等。
除了不连续的运行，散料热交换器3也可以原则上连续地运行。对于连续的运行，封闭机构14例如可以设计成叶轮闸门(Zellenradschleuse)或输送蜗杆。在这种情况下可以取消封闭机构2，而散料热交换器3可以直接与接收容器1相连，即上部入口管底部10此时直接与接收容器1相连。

Claims (10)

1.用于通过直接酯化对苯二甲酸和乙二醇来制造聚酯的方法，其特征在于，在添加到搅拌容器(16)中之前对粉末状的对苯二甲酸进行加热。
2.按照权利要求1的方法，其特征在于，通过间接加热来加热对苯二甲酸。
3.按照权利要求1或2的方法，其特征在于，对苯二甲酸的间接加热在散料热交换器(3)中进行。
4.按照上述权利要求中任一项的方法，其特征在于，将对苯二甲酸从环境温度加热到80℃至250℃，优选加热到100℃至200℃。
5.按照权利要求3或4的方法，其特征在于，在散料热交换器中用蒸汽间接加热对苯二甲酸。
6.按照权利要求3至5中任一项的方法，其特征在于，用氮气使散料热交换器惰性化。
7.按照权利要求3至5中任一项的方法，其特征在于，在对苯二甲酸的加热过程期间用过压加载散料热交换器。
8.用于通过直接酯化对苯二甲酸和乙二醇来制造聚酯的装置，其特征在于，
-具有用于加热对苯二甲酸的散料热交换器(3)，
-具有布置在散料热交换器(3)后面、用于搅拌已加热的对苯二甲酸的搅拌容器(16)。
9.按照权利要求8的装置，其特征在于，所述散料热交换器(3)构造成具有上部的缓冲段(3)、下部的出口段(6)和位于中间的管束。
10.按照权利要求8的装置，其特征在于，所述散料热交换器(3)设计成板式热交换器，并具有至少两个相互平行布置的板。
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CN101869818A (zh) * 2010-06-13 2010-10-27 浙江逸盛石化有限公司 降低对苯二甲酸配料罐内压的方法和装置
CN102089072A (zh) * 2008-07-11 2011-06-08 帝斯曼知识产权资产管理有限公司 半结晶聚合物的热处理方法

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CN101869818A (zh) * 2010-06-13 2010-10-27 浙江逸盛石化有限公司 降低对苯二甲酸配料罐内压的方法和装置
CN101869818B (zh) * 2010-06-13 2012-08-22 浙江逸盛石化有限公司 降低对苯二甲酸配料罐内压的方法和装置

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