CN1199061A - 聚合物颗粒结晶的装置及工艺 - Google Patents

聚合物颗粒结晶的装置及工艺 Download PDF

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CN1199061A
CN1199061A CN98106072A CN98106072A CN1199061A CN 1199061 A CN1199061 A CN 1199061A CN 98106072 A CN98106072 A CN 98106072A CN 98106072 A CN98106072 A CN 98106072A CN 1199061 A CN1199061 A CN 1199061A
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H·雷卡姆
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Abstract

本发明涉及一种聚合物颗粒结晶和干燥的装置及工艺,聚合物颗粒在结晶时的粘着和烧结现象通过一股惰性的气态介质产生的周期性扰动得以避免。

Description

聚合物颗粒结晶的装置及工艺
本发明涉及一个用于聚合物颗粒的结晶装置，以及聚合物颗粒的结晶工艺。
众所周知，有些聚合物颗粒在干燥和/或固体冷凝之前被结晶，以避免结块形成。特别是无定形聚酯颗粒易于胶结，给温度操作和从结晶装置排料带来很大困难。
在现有技术中已有一系列聚合物颗粒的结晶装置。DD-PS-0,150,932；DD-PS-0,147,716以及DE-A3,213,025介绍了通过搅拌部件避免结块形成的聚合物颗粒的结晶装置。这种机械搅拌部件产生颗粒应力和形成更多的粉尘。
其它避免使用机械搅拌部件的聚合物颗粒的结晶装置被公开于FR-A-1,478,224；WO-89/11073以及DE-A-19500383中。
FR-A-1,478,224描述了一种装置，使无定形聚合物颗粒通过一个产物分配器进入一个结晶器，其底板有钻孔。通过这些钻孔使一种气态介质被导入物料床并渗透其中。连接在结晶器之后的是一个干燥器。受这种设计制约的是结晶器和干燥器不可避免地在构造上要分开。
WO-89/11073描述了一种使无定形聚合物颗粒结晶和干燥的、被安放在一个设备中的二级装置。第一级(结晶器)的结构很复杂，要求很多昂贵的、部分活动的部件，特别是把充气表面造成这样的结构，使聚合物颗粒的处理能力不可以简单地改变，因为颗粒在充气表面的停留时间受到结构上的限制。
DE-A19500383介绍的是一个聚酯颗粒连续结晶的装置。载热的气态介质通过筛板被通入颗粒料，它也存在着结晶器和干燥器的结构分离的情况。
因此存在着对这样一种聚合物颗粒干燥装置的需求，它包含一个综合结晶器，并减少了结构上的浪费，将结晶器装入已有的干燥器。此外结晶器不应含有与聚合物颗粒接触的机械活动部件。而且该设计应允许处理量发生改变，无需采取改造措施。
本发明的主题是一个将聚合物颗粒结晶、干燥以及必要时将固体冷凝的装置，它由一个筒状外壳构成，其内包括一个基本垂直竖立的处理区，安装有气体入口接管和气体出口接管，一个不伸进聚合物颗粒料床的聚合物颗粒的入口，和一个聚合物颗粒的出口，其特征在于：在聚合物颗粒料床表面向下达500毫米的区域内安装气体入口接管，通过接管一股惰性的气态介质对物料床产生周期性的扰动。
按本发明的装置由附图1说明。
聚合物颗粒通过接管(1)被加入基本垂直竖立的装置(2)，以稳定的状态填充到处理区(3)直到填充高度在惰性气体入口(4)(又称二次气体入口)以上的500厘米处。通过接管(4)输入的惰性气态介质与通过接管(5)输入的惰性气态介质一起加热聚合物颗粒，使其发生结晶。通过接管(4)以脉动的惰性气体流形式输入介质，从而避免结块形成。输入的惰性气体流通过出口(6)离开装置，在气体净化系统和热交换系统得到净化，调温后再被使用。由于从接管(7)取出已干燥和结晶的聚合物颗粒，在接管(4)下部形成一个所谓的“活塞流(propfenstrmung)”。它由同样湿度和熔融粘度的聚合物颗粒组成。从接管(7)取出的聚合物颗粒可以直接送入挤压机，或者排出用于中间储存。通过接管(5)输入的惰性气态介质实现聚合物颗粒的干燥。
根据需要可以通过外壁对处理区(3)进行冷却或加热。它可以是圆柱形的或者是圆锥形的。
通过连接管(5)用惰性气体吹扫处理区(干燥器)，除去释放出的挥发部分。
用做惰性气体的物质通常是空气和/或氮气，它们的含水量相当于露点等于-20℃或者更低的标准。
通过连接管(4)向处理区(3)以脉动气流的形式输入上述惰性气体。脉动气流将接管(4)上部存在的颗粒层不断搅起，从而阻止结疤和粘结。脉动气流的速度为3米/秒，优选10米/秒。脉冲频率为10-60次气体脉冲/分钟，优选20-40次气体脉冲/分钟。
一个优选的实施形式是在聚合物颗粒填充高度以下100-400毫米，特别是在100-200毫米处安装连接管(4)。一个同样优选的实施形式是使接管(4)伸进到处理区半径的2/3处，得到最佳的效果。
连接管(4)和(5)的数目没有限制，只是受到部分给定的装置结构的限制。
无定形的，含水的聚合物颗粒由一个与接管(1)相连的输送设备送料。进料颗粒量可以通过监视接管(7)的出料量来测定，也可以通过在接管(4)上部500毫米的区间安装的加料位置感受器测定。在连续操作中将填充高度调成恒定的。填充高度可以通过排料量和/或加料量的改变而变化，所以使一个变化的工艺操作成为可能。
本发明的装置的重点是，接管(1)不能插入接管(4)上部的聚合物颗粒物料床内。优选接管(1)底缘和聚合物颗粒物料床上缘的距离在200毫米以上，特别是在200-1000毫米之间。
本发明的装置由此将一个结晶器，一个干燥器以及视需要而定的固体冷凝器结合在一个装置中。连接管(5)和(4)之间的处理区(3)构成干燥器，连接管(4)上部的处理区构成结晶器。由于结晶器的构造简单，可以被方便地装入存在的干燥器中。
上述的装置适合粒状聚合物材料的结晶、干燥和必要时的固体冷凝。其中特别适合粒状聚酯。
原则上所有已知类型的聚酯都可以考虑作为投料用的聚酯物料。此类聚酯主要由芳基二元羧酸和脂肪族二元醇衍生的结构单元组成。常用的芳基二元羧酸结构单元是苯二羧酸、特别是对苯二甲酸和间苯二甲酸以及萘二羧酸的二价基团；常用的二元醇含有2-4个碳原子，其中以乙二醇尤为合适。由下面这种聚酯材料形成的颗粒非常合适，它至少含85mol％的聚对苯二甲酸乙二醇酯，其余的15mol％由二元羧酸单元和二元醇单元构成，它们用作为改性剂，以便专业人员有针对性地对聚合物的物理和化学性质施加影响。
这些二元羧酸单元的例子有：间苯二酸或者脂肪族的二元羧酸如戊二酸、己二酸、癸二酸的基团；作为改性剂的二元醇残基包括长链二元醇，如丙二醇或者丁二醇，二-或三甘醇，或者较少量存在的、分子量为500-2000的聚二醇的残基。
特别优选的聚酯含有至少95mol％的聚对苯二甲酸乙二醇酯，尤其是未经过改性的聚对苯二甲酸乙二醇酯。
本发明其它的主题是聚合物颗粒、尤其是无定形聚酯颗粒的结晶和干燥工艺，包括如下措施：
A)用已知的方法加入无定形聚合物颗粒；
b)用已知的方法将聚合物颗粒结晶；
C)用已知的方法将结晶后的聚合物颗粒干燥；
D)用已知的方法将结晶后和干燥后的聚合物颗粒移出；
其特征在于，结晶和干燥都发生在同一个构造上未分开的处理器中，在结晶期间，结块现象通过一种惰性气态介质对聚合物颗粒产生周期性扰动得以阻止。
在措施B)中提到的结晶通常采用的温度低于180℃，优选120-180℃。
根据措施C)的干燥通常在一种惰性气流中进行，采用140-180℃之间的温度。干燥由逆向引入的、加热的惰性气流进行。由此将颗粒粒子加热到干燥所需的温度，并将形成的不需要的副产物带出反应器。固体冷凝的颗粒粒子通过已知的排出装置带出，从而调节重力作用的连续产物流。
结晶后和干燥后的聚合物颗粒的残余含水量为20ppm水。
聚合物颗粒需要数小时的干燥。依温度和处理量而定干燥时间可长达6小时(在干燥段的停留时间)。结晶时间-也视温度和处理量而定-至少为20分钟(在结晶段的停留时间)。

Claims (13)

1.由一个筒状外壳构成的用于聚合物颗粒结晶、干燥以及必要时固体冷凝的装置(2)，其中包括一个基本垂直的处理区(3)，安装有气体入口接管(4)(5)和气体出口接管(6)，一个聚合物颗粒的入口(1)，它不伸进聚合物颗粒料床中，和一个聚合物颗粒的出口(7)，其特征在于：在聚合物颗粒床表面向下达500毫米的区域内安装气体入口接管(4)，通过接管一股惰性的气态介质对颗粒床产生周期性的扰动。
2.权利要求1的装置，其特征在于：处理区(3)为圆柱形或圆锥形。
3.权利要求1的装置，其特征在于：处理区(3)的下部作为干燥器，处理区(3)的上部作为结晶器。
4.权利要求1的装置，其特征在于：在聚合物颗粒床表面向下100-400毫米的区域内安装气体入口接管(4)，通过接管一股惰性的气态介质对颗粒床产生周期性的扰动。
5.权利要求4的装置，其特征在于：在聚合物颗粒床表面向下100-200毫米的区域内安装气体入口接管(4)，通过接管一股惰性的气态介质对颗粒床产生周期性的扰动。
6.权利要求1的装置用于聚酯，特别是用于聚对苯二甲酸乙二醇酯结晶和干燥的应用。
7.聚合物颗粒，特别是无定形聚酯颗粒的结晶和干燥工艺，包括如下措施：A)无定形聚合物颗粒按已知的方法导入；b)聚合物颗粒按已知的方法结晶；C)已结晶的聚合物颗粒按已知的方法干燥；D)已结晶和干燥的聚合物颗粒按已知的方法排出；其特征在于：结晶和干燥在同一个结构上不分开的处理区进行，结晶期间的结块现象通过一股惰性的气态介质对聚合物颗粒产生周期性的扰动得以阻止。
8.权利要求7的工艺，其特征在于：惰性的气态介质为空气和/或氮气。
9.权利要求7的工艺，其特征在于：周期性的扰动频率为10-60次脉冲/分钟。
10.权利要求9的工艺，其特征在于：周期性的扰动频率为20-40次脉冲/分钟。
11.权利要求7的工艺，其特征在于：结晶温度为120-180℃。
12.权利要求7的工艺，其特征在于：干燥温度为140-180℃。
13.权利要求7的工艺，其特征在于：已结晶和干燥的聚合物颗粒的残余水分为20ppm水。
CN98106072A 1997-03-10 1998-03-09 聚合物颗粒结晶的装置及工艺 Pending CN1199061A (zh)

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