CN1535291A - 用于制备高粘性或高度稳定的缩聚物和去单体化的pa6的方法 - Google Patents
用于制备高粘性或高度稳定的缩聚物和去单体化的pa6的方法 Download PDFInfo
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- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
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- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
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Abstract
本发明涉及运用垂直反应阶段制备高粘性或高度稳定的缩聚物和去单体化的PA6的方法和设备。根据该方法将缩聚物熔体从预备阶段注入反应阶段上端并通过分配装置和扩增表面的部件分配。借助惰性气体或真空从流动的缩聚物熔体中将共同反应物的产物废料去除并在缩聚物熔体水平面之上脱离反应阶段。产品在底槽的留滞时间如此选择,即在反应阶段较下端存在处于化学平衡的缩聚物,将其中一部分注回反应阶段上端,而剩余部分相应于所选择的物料通过量排离反应阶段用于进一步应用。
Description
本发明涉及以权利要求1的属概念中所述的方式制备高粘性或高度稳定的缩聚物和去单体化的PA6的方法以及实施该方法的设备。
为了提高缩聚物粘性,已知在双螺旋挤压机中进行除气。然而,这类双螺旋挤压机为价格昂贵和易磨损的构件,并且由此可达到的除气程度是受到限制的。
同样已知的是,后缩合方法在近乎水平设置的后缩合器中进行。其中缩聚合熔体持续地从一水平面中经本身转动的内部机械装置暴露于熔体水平面以上的环境中并除气。经除气的产物被排出。然而在此方法中不能保证足够准确的产物留滞时间,由此出现成品缩聚物的质量损害。根本无法在缩聚合过程的后期调节化学平衡。此外用于此的装置复杂,特别是对外界环境的密闭问题悬而未决,由此对于不耐受氧气的缩聚物受到损坏。
本发明的任务在于,创造一种文端所述类型的方法以及实施该方法的设备,该方法或设备使得在低花费下大幅提高粘性成为可能。
所述任务是通过权利要求1或4所给出的技术特征解决的。
本发明有益的实施方案和进一步构造由从属权利要求给出。
通过位于在垂直设置的反应阶段下端的部分缩聚物熔体的回注和由此通过一部分所述熔体的泵抽回送以简单的方式达到粘性的提高和/或内酰胺的降低,因为为了有效地去除缩聚合产物废料将熔体多次导入高效除气的阶段。在反应阶段中的留滞时间在此为了达到缩聚物的化学平衡分别进行设置,由此足够地随后形成缩聚物产物废料并可以在除气室位于熔体水平面的上方排出。排除缩聚物产物废料可以借助惰性气体或在真空中进行。
来源于预备阶段和来源于注回的缩聚物合流产生不处于化学平衡状态的缩聚物,因为共同反应物的产物废料的量被设置于预备阶段缩聚物的化学平衡之下,因此在此发生缩聚合反应。只要在合流后有足够的留滞时间予以支配,缩聚合熔体的粘性在合流后不仅因为混合,而且因为发生缩聚合反应而上升。因此在合流后直至缩合后的反应阶段通过管道延长而制造额外的留滞时间是有益处的。
在附图中展示了本发明的一个具体实施例,其显示了用于实施根据本发明的方法的反应阶段的优选实施形式。
在附图中所显示的反应阶段包括垂直反应釜1,其上端具有用于导入由预备阶段提供的缩聚物熔体的导入管7,在此,在导入管7上可以安设泵P1。
在反应釜1中安设了扩增表面的部件3,在扩增表面的部件之上安置了用于将缩聚物熔体导向部件3的分配器2,分配器的入口与导入管7相连接。
在反应釜1的下端是两个串联连接的计量装置P2、P3,其例如以可控制的泵的形式安装,其间与回流管6的一端相连接,回流管的另一端与分配器2的入口相连,在此这种连接也可以优选用一个导入管连接在接合点9上。在计量装置P3后面的流出方向也可以形成一个调节阀。
在结合点9之后有利的是,在导入管上使用一个静态混合器10,并且静态混合器10包括其后至多到达分配器2的导管如此设置,以使通过缩聚合而上升粘性的留滞时间延长。在结合点9之后的管道7的横截面因此大于在结合点9之前的管道7的横截面加上回流管6的横截面的总和。
也可以在结合点9之后再安入一个反应釜(没有图示),其完全注满缩聚物并从结合点10至缩聚合阶段的入口流经产物。始于反应釜出口处的导入管7终止于分配器2并以任意的直径连入分配器2。
反应釜1较上端具有至少一个出气口4并在底槽具有一个水平面测量装置5,其输出信号可以用于控制计量装置P3或可替代地也可以控制泵P1。
回流管6能够使位于反应釜1下端的一部分缩聚物熔体回注,并因此将这种熔体的一部分泵抽回送以简单的方式达到粘性的提高和/或内酰胺的降低,因为该熔体多次经扩增表面的部件3导送并高效除气,以便有效地去除缩聚合产物废料。在反应釜1中的留滞时间将分别设置用以达到缩聚物化学平衡和/或在基于PA 6生产PA 6-缩聚物或共聚多酰胺多聚物的情形下用以达到内酰胺的降低。由此随后形成足够的缩聚物产物废料并可以在除气室中的熔体水平面的上方通过出气口4去除。
缩聚物产物废料的去除可以通过导管8在接近熔体表面借助惰性气体的导入或在真空中进行。
对于用于提高粘性的缩聚合反应,熔体在反应釜3中的留滞时间可以为3小时,在此作为实施例可以经计量装置P2、P3设置泵抽回送通过反应釜1的物料量的50%。在此所述使用量通过经水平面测量装置5测量的填料水平的提高而提高50%
用于获取较高度稳定的缩聚物可以在预备阶段加入稳定剂。
当该方法用于去除PA6的内酰胺时,不升高水平面,而是可以通过泵抽回送100%的物料通过量达到约4.5%的内酰胺的降低。
出气口4可以只用图式表明的装置回收与惰性气体和水结合的单体。
Claims (7)
1.运用垂直反应阶段制备高粘性或高度稳定的缩聚物和去单体化的PA6的方法,其特征在于,将缩聚物熔体从预备阶段注入反应阶段上端并通过分配装置和扩增表面的部件分配,借助惰性气体或真空从流动的缩聚物熔体中将共同反应物的产物废料去除并在缩聚物熔体水平面之上脱离反应阶段,产品在底槽的留滞时间如此选择,即在反应阶段较下端存在处于化学平衡的缩聚物,将其中一部分注回反应阶段上端,而剩余部分相应于所选择的物料通过量排离反应阶段用于进一步应用。
2.根据权利要求1的方法,其特征在于,回注部分相应于反应阶段物料流通量的50%。
3.根据权利要求1或2的方法,其特征在于,用于提高粘性,缩聚反应的产物留滞时间长达5小时,并且在新鲜产物与回注的产物合并后的产物留滞时间长达1小时。
4.用于实施该方法的设备,其特征在于,反应釜(1),其中安设了扩增表面的部件(3),在扩增表面的部件之上安置了用于将缩聚物熔体导向部件(3)的分配器(2),其中在反应釜(1)上端至少具有一个出气口(4),在底槽具有一个水平测量装置(5)并且在反应釜(1)下端装有两个串联连接的计量装置(P2、P3),其间与回流管(6)的一端相连接,回流管的另一端与分配器(2)的入口相连。
5.根据权利要求4的设备,其特征在于,至少计量装置中的一个通过泵(P2、P3)形成。
6.根据权利要求4或5的设备,其特征在于,缩聚物熔体从预备阶段通过泵(P1)导入分配器(2),该泵可控制用于调节流经反应釜(1)的物料流通量。
7.根据权利要求4-6之一的设备,其特征在于,在泵(P1)后面的流向上,回流管(6)接口于导入管(7)上的结合点(9),并在导入管(7)上的结合点(9)后面、分配器(2)之前安设一个静态混合器(10)和/或一个具有进口和出口的反应釜。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE2001126133 DE10126133B4 (de) | 2001-05-29 | 2001-05-29 | Verfahren und Vorrichtung zur Herstellung von hochviskosen oder hochstabilisierten Polykondensaten und entmonomerisiertem PA 6 |
DE10126133.0 | 2001-05-29 |
Publications (2)
Publication Number | Publication Date |
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CN1535291A true CN1535291A (zh) | 2004-10-06 |
CN1249125C CN1249125C (zh) | 2006-04-05 |
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Application Number | Title | Priority Date | Filing Date |
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CN 02814690 Expired - Fee Related CN1249125C (zh) | 2001-05-29 | 2002-05-17 | 用于制备高粘性或高度稳定的缩聚物和去单体化的pa6的方法 |
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EP (1) | EP1406948A1 (zh) |
CN (1) | CN1249125C (zh) |
DE (1) | DE10126133B4 (zh) |
RU (1) | RU2295545C2 (zh) |
UA (1) | UA76471C2 (zh) |
WO (1) | WO2002096975A1 (zh) |
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US6906164B2 (en) | 2000-12-07 | 2005-06-14 | Eastman Chemical Company | Polyester process using a pipe reactor |
US7943094B2 (en) | 2006-12-07 | 2011-05-17 | Grupo Petrotemex, S.A. De C.V. | Polyester production system employing horizontally elongated esterification vessel |
US7649109B2 (en) | 2006-12-07 | 2010-01-19 | Eastman Chemical Company | Polyester production system employing recirculation of hot alcohol to esterification zone |
US7863477B2 (en) | 2007-03-08 | 2011-01-04 | Eastman Chemical Company | Polyester production system employing hot paste to esterification zone |
US7858730B2 (en) | 2007-07-12 | 2010-12-28 | Eastman Chemical Company | Multi-level tubular reactor with dual headers |
US7847053B2 (en) | 2007-07-12 | 2010-12-07 | Eastman Chemical Company | Multi-level tubular reactor with oppositely extending segments |
US7868129B2 (en) | 2007-07-12 | 2011-01-11 | Eastman Chemical Company | Sloped tubular reactor with spaced sequential trays |
US7872089B2 (en) | 2007-07-12 | 2011-01-18 | Eastman Chemical Company | Multi-level tubular reactor with internal tray |
US7872090B2 (en) | 2007-07-12 | 2011-01-18 | Eastman Chemical Company | Reactor system with optimized heating and phase separation |
US7842777B2 (en) | 2007-07-12 | 2010-11-30 | Eastman Chemical Company | Sloped tubular reactor with divided flow |
US7829653B2 (en) | 2007-07-12 | 2010-11-09 | Eastman Chemical Company | Horizontal trayed reactor |
US7868130B2 (en) | 2007-07-12 | 2011-01-11 | Eastman Chemical Company | Multi-level tubular reactor with vertically spaced segments |
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GB1313592A (en) * | 1970-04-28 | 1973-04-11 | Toray Industries | Method and apparatus of a continuous polymerization |
DE2461902A1 (de) * | 1974-12-31 | 1976-07-08 | Zimmer Ag | Verfahren und vorrichtung zum entfernen von verdampfbaren bestandteilen aus polyamidschmelzen |
DD265151A1 (de) * | 1987-09-30 | 1989-02-22 | Schwarza Chemiefaser | Schmelzentgaser zur kontinuierlichen polymerisation von polyamid-6 aus epsilon-kaprolaktam |
DE4039857A1 (de) * | 1990-10-19 | 1992-04-23 | Inventa Ag | Verfahren und vorrichtung zur direkten, kontinuierlichen modifizierung von polymerschmelzen |
DE19506407B4 (de) * | 1995-02-23 | 2006-08-10 | Karl-Heinz Wiltzer | Verfahren und Vorrichtung zur Herstellung von hochviskosen oder hochstabilisierten, reaktionsstabilen Polyamiden und zur kontinuierlichen Entmonomerisierung von Polyamiden |
DE19531989A1 (de) * | 1995-08-30 | 1997-05-15 | Polymer Eng Gmbh | Verfahren zur kontinuierlichen Herstellung eines dimerarmen Polyamid 6 |
DE19607723C2 (de) * | 1996-02-29 | 2002-10-24 | Polymer Eng Gmbh | Verfahren und Vorrichtung zur kontinuierlichen Extraktion von polymeren Granulaten |
DE19841376A1 (de) * | 1998-09-10 | 2000-03-16 | Lurgi Zimmer Ag | Verfahren zur Einspeisung von Additiven in einen Polymerschmelzestrom |
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2001
- 2001-05-29 DE DE2001126133 patent/DE10126133B4/de not_active Expired - Lifetime
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2002
- 2002-05-17 CN CN 02814690 patent/CN1249125C/zh not_active Expired - Fee Related
- 2002-05-17 EP EP02738083A patent/EP1406948A1/de not_active Withdrawn
- 2002-05-17 UA UA20031212941A patent/UA76471C2/uk unknown
- 2002-05-17 RU RU2003137774/04A patent/RU2295545C2/ru not_active IP Right Cessation
- 2002-05-17 WO PCT/EP2002/005441 patent/WO2002096975A1/de active Application Filing
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Publication number | Publication date |
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EP1406948A1 (de) | 2004-04-14 |
RU2003137774A (ru) | 2005-05-20 |
RU2295545C2 (ru) | 2007-03-20 |
UA76471C2 (en) | 2006-08-15 |
CN1249125C (zh) | 2006-04-05 |
DE10126133A1 (de) | 2003-01-02 |
WO2002096975A1 (de) | 2002-12-05 |
DE10126133B4 (de) | 2007-03-29 |
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