CN1035546C - 聚合物熔体直接连续改性的方法及装置 - Google Patents

聚合物熔体直接连续改性的方法及装置 Download PDF

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CN1035546C
CN1035546C CN91109835A CN91109835A CN1035546C CN 1035546 C CN1035546 C CN 1035546C CN 91109835 A CN91109835 A CN 91109835A CN 91109835 A CN91109835 A CN 91109835A CN 1035546 C CN1035546 C CN 1035546C
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维尔纳·施蒂比
丹尼尔·博尔尼
汉斯·吕克特
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Ames Infinta Co ltd
Inventa AG fuer Forschung und Patentverwertung
Uhde Inventa Fischer AG
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Abstract

本发明描述了一种聚合物熔体直接、连续地灵活改性的方法及装置，即通过从要改性的熔体流中分离出来的侧流熔体，在一专门设计的双螺杆挤出机中分散原先加入熔体的添加剂，然后，添加剂熔体汇集物与需改性的熔体流回混。

Description

聚合物熔体直接连续改性的方法及装置
本发明涉及一种在侧流中加入添加剂使聚合物熔体直接连续改性的方法，这种方法就产物转换而言具有很高的灵活性。
由于多种原因，聚合物熔体必须用添加剂进行改性。一个原因是由于合成聚合物的均相结构没有显示光的任何折射和反射的可能，因此聚合物熔体几乎是透明的。因此为适应众多不同的应用，需要在聚合物熔体中加入诸如二氧化钛(TiO2)、硫化锌(ZnS)或碳黑之类的颜料。特别在合成纤维方面，必须在不吸引人的、色译黯淡的合成纤维的纺丝前去掉熔体，特别是当合成纤维被在衣料领域中使用时，会产生不佳的效果。光的折射可通过加入较少量的白色颜料，一般为二氧化钛来实现。然而，为了其他目的，例如在生产抗起球纤维或例如带黄色的聚合物光学增白，通过加入添加剂来使聚合物改性也是已知的。
随着连续缩聚工厂产量的增加，只有具备高度灵活性的生产线才是经济的。通常，各种不同类型的产品同时生产，例如纤维和颗粒同时在一条生产线上生产必须是可能的。在这种情况下，不同产品的转换，如消光、上光或着色的完成必须在尽可能的最短时间内无损耗地实现。这些要求仅仅依靠现有生产条件是不能满足的。
现有技术是采用原熔体进行熔融改性的方法。该原理在德国公开专利1,604,368中进行了描述。一原批颗粒的熔体和含有高比例的添加剂以一确定的比例在下游与要改性的聚合物熔体混和。虽然这一方法对于所完成的转换提供了高度灵活性，但存在下列缺点：原批颗粒在熔化前必须干燥。其次，在重新熔化时颗粒要经受附加的热和机械载荷。该方法的第三个缺点是增加处理费用。另外一个缺点是颗粒有外部污染的危险。在室内进行原批生产的情况下，另一外加的缺点是聚合物颗粒必须从生产过程中取出。原批颗粒从别处获得的缺点：是与所用的聚合物之间的差异，在最终产品的应用性能上将有不好的效果。
另一种改性工艺在《化学工程进展》期刊第78(1982)1，62-64页上进行了描述。与在聚合物熔体的下游加入添加剂的方法不同，在这种方法中聚合物颗粒和最好是反应性的添加剂被同时加入第一挤出段。该方法的缺点是：一方面颗粒间的添加剂有压实的危险，另一方面为均匀和分散的需要而所施加的高剪切应力导致了聚合物的粘度大大的、不可控制的减低。
另一现有技术的方法在《化学和纺织工业》期刊1(1986)第24至29页上进行了描述。在这种方法中，一部分流体从主熔体流中分出，该主熔体流是从缩聚端反应器中排出的，一添加剂在下游并入该分熔体中。该充入添加剂的熔体又重新回到熔体主流中。这种方法在添加剂转换中也具有高度灵活性，但也存在几个主要缺点。一个缺点是，尽管是抽成真空的，在聚合物熔体中仍含有挥发性成份，例如乙二醇和水蒸汽或齐聚物在加入添加剂的过程中将逸出加料漏斗。这样导致了添加剂的自由流动性降低，并形成块状。添加剂结块已不能均匀地加入熔体中，且在纺丝过程中引起过滤器堵塞，成为纤丝的弱点。另外，一连续、均匀计量的添加剂由于熔体的热对流而受损坏，使通常是自由落下的添加剂颗粒在进料口停止。另一个缺点是添加剂上料的挤出口必须小，以减少熔体从开口中溢出的危险。结果，添加剂的数量被限制了。
本发明的目的在于克服现有技术中的前述缺点，开发一种使聚合物直接、连续改性的方法及装置。
采用本发明的方法，聚合物熔体，较佳是聚酯、聚酰胺或聚烯烃熔体，更佳的是聚酯熔体，可通过加入添加剂来改性。这种添加剂可以是可溶解的或不溶解的，矿物或有机颜料，诸如硫化锌、二氧化硅、二氧化钛，较佳是二氧化钛，或是其他改善产品性能的熔体改性添加剂，诸如光学增白剂，光和热稳定剂，较佳是光学增白剂。
在本发明的方法中，应明确添加剂，也可是一种添加剂混和物，最初是加在第一挤出段，熔体流在第二段进入。然后，添加剂为聚合物熔体所浸润，混和物通过排气段，然后以已知的方式均匀分散并送至挤出机出口。最初加入其本身的添加剂，被尽可能大地填充在封闭的挤出机中的聚合物熔体所浸润，其优点在于设有挥发性熔体组分可向后移动对添加剂的进料产生不利影响。这可通过安排在下游的抽真空来实现，甚至可从添加剂中带走挥发性组分，如湿气。为避免没有浸润的添加剂在熔体进入前压实或结块，在该段中螺杆的螺纹高度必须减小。根据实验，螺杆直径减小0.2至4毫米，较好是0.5至2毫米，就能适应这种需要，0.5至1毫米最适合于以二氧化钛作为添加剂和以聚酯或聚酰胺作为聚合物的消光剂。
添加剂——聚合物的混合物的分散及传输是以传统的方法在挤出机的剩余段中通过合适的螺杆实现的。
在本发明的方法中，由聚合物熔体浸润以便与其混合的添加剂可满足一特殊的压力试验，在该试验中每分钟通过一限定网格宽度的过滤器的模拟熔体产量在30分钟前后就确定了。
确保用于工业领域的聚对苯二酸酯熔体和聚酰胺6熔体。
90％残留量的挤出和注射成型
60％残留量的纤维和细丝的纺丝
40％残留量的POY和FOY纱压力试验：
在与聚合物熔体具有相同粘度的，以相应的温度进行改性的样品中，如聚乙二醇，添加剂被分散、加热至测量温度，并通过一11至13微米的标定宽度过滤器过滤。流过过滤器的物质就产生了，m1在5至6分钟的时间段t1，m2在35至36分钟的时间段t2，物质产量的下降百分率由m1和m2之间的差异决定。
图1的流程图描述了本发明的方法。在图中，(1)表示熔体主流，(2)表示任选的要进行改性的部分熔流，(3)表示要进行改性的熔体侧流，(4)表示供料泵，(5)表示添加剂进料装置，(6)表示双螺杆挤出机，其中(7)为计量段，(8)为熔体进入段，(9)为浸润段，(10)为排气段及(11)为分散段，(12)表示排气装置，(13)表示回料泵，(14)表示改性过的侧流，(15)表示固定混和部件，(16)表示纺丝点，(17)表示未改性的部分熔体流及(18)表示造粒机。
聚合物熔体主流根据所需不同产品类型的数量分成几部分熔体流：如图1例子中制成任选的消光或不消光熔体以直接纺丝(16)的产品和未改性的原料颗粒(17)的产品。从任选的要改性的部分熔体流(2)中分出一熔体侧流(3)，并通过计量进料泵(4)加入到双螺杆挤出机(6)中，该挤出机(6)设有特殊设计的螺杆并具有一系列处理段7—11。在挤出机第一段中(计量段7)，添加剂通过进料装置(5)(以固体形式计量)进入并传送到第二段(熔体进入段8)，在该段中部分熔体流直接加入添加剂，并在挤出机第三段(浸润段9)浸润，所述部分熔流被传送并在挤出机第四段(排气段10)通过排气装置(12)排气，然后在挤出机第五段(分散段11)中以该领域中专业人员熟知的现有技术进行分散。以这种方式获得的添加剂——熔体汇集物通过回料泵(13)重新计量进入需改性的部分熔体流(2)，并在固定混和部件(15)内均匀地回混。
采用本发明的方法和装置，聚合物熔体可以毫不困难地用重量为0.01至16％，最好为0.04至0.6％，最佳为0.4％的添加剂进行改性。
图2所示为一Berstorf生产的ZE40A型的相互旋转的双螺杆挤出机的实施例，具有加热和冷却段：(21)计量段、(22)熔体进入段、(23)排气段、(24)至(28)分散段、(29)螺杆端、(30)添加剂计量、(31)聚合物熔体进料和(32)排气。
实现本发明方法的装置包括至少一进料泵(4)，一专门设计的双螺杆挤出机(6)，该机带有添加剂进料装置(5)、排气装置(12)和处理段(7)至(11)，一回料泵(13)和一固定混和部件(15)，添加剂进料装置(5)最好是下落管，专门设计的双螺杆挤出机(6)最好是相互旋转的双螺杆挤出机，具有在挤出机第一段(计量段7)专门设计的螺杆，其直径减小0.2至4毫米，较佳为0.5至2毫米，最佳为0.5至1毫米，在挤出机第二段(熔体进料段8)具有一已知的传送部件，在挤出机第三段(浸润段9)设有捏和及减速部件，在挤出机第四段(排气段10)装有已知的传送部件，在挤出机第五段(分散段11)交替设有已知的传送和捏和部件，且计量段7在采用温度敏感添加剂时可冷却。
本发明方法及装置的优点在于：具有高度灵活性。添加剂的转换可在几乎没有损耗的情况下立即实现，且不需昂贵的清洗操作和在没有鉴别的情况下不会生成劣质产品；不需要另外的载体聚合物，这样将不会产生影响最终产品使用性能的缺点；封闭的过程使得在生产过程中没有复杂的问题介入，如在室内的原批生产之类的问题；在添加剂进料过程中不会出现聚合物熔体和/或挥发性馏份的溢出；熔体不会结块改性且延长了过滤器的使用寿命；具有比现有技术中所需的较低的螺杆速度；添加剂不需预先干燥且只需最小的、恒定的聚合物熔体粘度的减小；挤出机的添加剂的加料口尺寸可以与整个螺杆截面一样大；添加剂进料或熔体的产量没有限制；添加剂连续、均匀地计量进入挤出机第一段不存在热传导问题；在使用温度敏感添加剂时挤出机第一段可进行冷却；不需要采用现有技术中的辅助方法。
下面的例子是本发明未加限定的实施例。实例1
0.72kg/h二氧化钛(Sachtleben，LOCR-S-U型)计量进入第一段，冷却至50℃，用如图2所示带有螺杆构形的双螺杆挤出机和，在挤出机第一段，由直径减小0.5毫米的螺杆传送入挤出机第二段。与此同时，一部分需进行改性的熔流(120kg/h)从聚对苯二甲酸乙二醇酯熔体主流中分离出来，且在所述的部分熔流中又有9kg/h的侧流接着分离出来并直接加到最初加入挤出机第二段的二氧化钛中。根据下列的机器设定数据，二氧化钛进一步加入聚合物熔体，引用的料筒温度通过冷却或加热达到。所得到的二氧化钛——消光侧流熔体汇集物含有的量为二氧化钛重量的8％，而所对应的最终颜料含量在改性的部分熔流中占二氧化钛重量的0.6％。
进入挤出机第二段的聚对苯二甲酸乙二醇酯熔体侧流的温度：
                              290℃
挤出机速度：                  250rpm
挤出机动力消耗：              8.8A
供电电压：                    385V
挤出机反压力：                40bar
离开挤出机后改性的聚对苯二甲
酸乙二醇酯熔体侧流的温度：    270℃
料筒温度：
第一段：                      50℃
第二段：                      225℃
第三段：                      265℃
第四段：                      265℃
第五段：                      270℃
第六段：                             270℃
第七段：                             270℃
第八段：                             270℃
端部                                 265℃实例2
0.32kg/h二氧化钛(Kronos，AVF9009型)计量进入第一段，冷却至50℃，用如图2所示带有螺杆构形的双螺杆挤出机和，在挤出机第一段，由直径减小1毫米的螺杆传送入挤出机第二段。与此同时，一部分需进行改性的熔流(53kg/h)从聚酰胺6熔体主流中分离出来，且在所述的部分熔流中又有8kg/h的侧流接着分离出来并直接加到最初加入挤出机第二段的二氧化钛中。根据下列的机器设定数据，二氧化钛进一步加入聚酰胺熔体，引用的料筒温度通过冷却或加热达到。得到的二氧化钛—变化的聚酰胺侧流熔体汇集物含有的量为二氧化钛重量的4％，而所对应的最终颜料含量在改性的部分熔流中占二氧化钛重量的0.6％。
进入挤出机第二段的聚酰胺6侧流
熔体的温度：                         280℃
挤出机速度：                         150rpm
挤出机动力消耗：                     9A
供电电压：                           230V
挤出机反压力：                       40bar
离开挤出机后改性的聚酰胺6
侧流熔体的温度：                     277℃
料筒温度：
第一段：                             50℃
第二段：                             225℃
第三段：                             263℃
第四段：                             265℃
第五段：                             270℃
第六段：                             270℃
第七段：                             270℃
第八段：                             265℃
端部                                 265℃实例3
以下列设定的数据按实例1类推用二氧化钛改性聚对苯二甲酸乙二醇酯侧流：
螺杆直径在挤出机第一段减小：         1mm
聚对苯二甲酸乙二醇酯熔体主流：       3000kg/h
聚对苯二甲酸乙二醇酯熔体侧流：       75kg/h
二氧化钛(Sachtleben先生，
         LOCR-S-U型)：               12kg/h
改性的侧流中二氧化钛含量：           16％(重)
改性的部分熔流中二氧化钛最终含量：   0.4％(重)
进入挤出机第二段的聚对苯二甲酸
乙二醇酯熔体侧流的温度：             292℃
挤出机速度：                         250rpm
挤出机动力消耗：                     21A
供电电压：                           240V
挤出机反压力：                       20bar
离开挤出机后改性的聚对苯二甲
酸乙二醇酯熔体侧流的温度：           281℃
料筒温度：
第一段：                            30℃
第二段：                            240℃
第三段：                            260℃
第四段：                            260℃
第五段：                            260℃
第六段：                            260℃
第七段：                            260℃
第八段：                            260℃
端部                                260℃实例4
以下列设定的数据按实例1类推用光学增白剂(Eastmann Ko-dak先生，光导发亮剂OPT1型)改性聚对苯二甲酸乙二醇酯侧流：
螺杆直径在挤出机第一段减小          0.5mm
聚对苯二甲酸乙二醇酯熔体主体：      120kg/h
聚对苯二甲酸乙二醇酯熔体侧流：      9kg/h
光学增白剂：                        36kg/h
改性的侧流中光学增白剂含量：        0.4％(重)
改性的部分熔体流中光学增白剂
最终含量：                          0.3％(重)
进入挤出机第二段的聚对苯二甲酸
乙二醇酯熔体侧流的温度：            290℃
挤出机速度：                        250rpm
挤出机动力消耗：                    8.8A
供电电压：                          385V
挤出机反压力：                      40bar
离开挤出机后改性的聚对苯二甲酸乙
二醇酯熔体侧流及光学增白剂的温度：270℃
料筒温度：
第一段：                      50℃
第二段：                      225℃
第三段：                      265℃
第四段：                      265℃
第五段：                      270℃
第六段：                      270℃
第七段：                      270℃
第八段：                      270℃
端部                          265℃

Claims (25)

1.聚合物熔体与添加剂在要改性的熔体的侧流中，通过加入和分散至少一种添加剂而直接、连续改性的方法，所加入的添加剂随后与添加剂熔体汇集物及要改性的熔流回混，其特征在于：在侧流中，在具有一系列处理阶段的双螺杆挤出机中，添加剂a)通过一添加剂进料装置计量并进入挤出机第一段(计量段)，b)传送入挤出机第二段，在该段中聚合物侧流熔体加入到原先进入的添加剂中(熔体进入段)，c)在挤出机第三段浸润(浸润段)，d)在挤出机第四段传送并通过排气装置排气(排气段)，e)在挤出机第五段均匀分散(分散段)，f)重新加入未改性的熔流和g)与后者均匀回混，螺杆直径在计量段被减小。
2.如权利要求1所述的方法，其特征在于，添加剂有如下特征：
添加剂每分钟滴加入原料并在与所需改性的聚合物熔体具有相同粘度的样品中扩散的量，在恒压情况下经过标定宽度为11至13微米的过滤器过滤30分钟后，不超过60％。
3.如权利要求1所述的方法，其特征在于，添加剂有如下特征：
添加剂每分钟滴加入原料并在与所需改性的聚合物熔体具有相同粘度的样品中扩散的量，在恒压情况下经过标定宽度为11至13微米的过滤器过滤30分钟后，不超过40％。
4.如权利要求1所述的方法，其特征在于，所改性的聚合物熔体为聚酰胺熔体。
5.如权利要求1所述的方法，其特征在于，所改性的聚合物熔体为聚酯熔体。
6.如权利要求1至5中之一项所述的方法，其特征在于，所采用的添加剂为矿物颜料。
7.如权利要求1至5之一项所述的方法，其特征在于，所采用的添加剂为易溶解的或不溶解的有机化合物。
8.如权利要求1至5之一项所述的方法，其特征在于，所采用的添加剂为二氧化钛。
9.如权利要求1至5中之一项所述的方法，其特征在于，所采用的添加剂为易溶解或不溶解的、改善产品性能的熔融改性的添加剂。
10.如权利要求1至5中之一项所述的方法，其特征在于，所采用的添加剂为光学增白剂。
11.如权利要求1至5中之一项所述的方法，其特征在于，需改性的聚合物熔体用重量为其0.01％至16％的添加剂进行改性。
12.如权利要求1至5中之一项所述的方法，其特征在于，需改性的聚合物熔体用重量为其0.04至0.6％的添加剂进行改性。
13.如权利要求1至5中之一项所述的方法，其特征在于，需改性的聚合物熔体用重量为其0.4％的添加剂进行改性。
14.如权利要求1至5中之一项所述的方法，其特征在于，聚合物熔体用二氧化钛进行改性，螺杆在计量段中直径减小0.5至1毫米。
15.实现如权利要求1所述的聚合物熔体与添加剂在要改性的熔流的侧流中，通过加入和分散至少一种添加剂而直接、连续改性的方法的装置，所加入的添加剂随后与添加剂熔体汇集物及要改性的熔体流回混，其特征在于，装置在侧流中包括，至少一进料泵，一螺杆直径在计量段减小的双螺杆挤出机，该挤出机包括添加剂进料装置和排气装置及一回收进料泵，以及在改性过的熔体流中的固定混合部件。
16.如权利要求15所述的装置，其特征在于，双螺杆挤出机具有一计量段、一熔体进入段、一浸润段、一排气段和一分散段。
17.如权利要求15或16所述的装置，其特征在于，在双螺杆挤出机的计量段，螺杆直径减小了0.2至4毫米。
18.如权利要求15或16所述的装置，其特征在于，在双螺杆挤出机的计量段，螺杆直径减小了0.5至2毫米。
19.如权利要求15或16所述的装置，其特征在于，在双螺杆挤出机的计量段，螺杆直径减小了0.5至1毫米。
20.如权利要求15所述的装置，其特征在于，添加剂进料装置为一直落管。
21.如权利要求16所述的装置，其特征在于，计量段可以冷却。
22.如权利要求15所述的装置，其特征在于，双螺杆挤出机为一相互旋转的双螺杆挤出机。
23.如权利要求15或16所述的装置，其特征在于，双螺杆挤出机熔体进入段具有一传送部件。
24.如权利要求15或16所述的装置，其特征在于，双螺杆挤出机的浸润段具有减速和捏和部件。
25.如权利要求15或16所述的装置，其特征在于，双螺杆挤出机的分散段具有交替的传送和捏和部件。
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US5458478A (en) 1995-10-17
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KR920008117A (ko) 1992-05-27
DE4039857A1 (de) 1992-04-23
IT1249461B (it) 1995-02-23
DE4039857C2 (zh) 1993-08-19
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