CN1047182C - 软泡沫体的生产方法 - Google Patents

软泡沫体的生产方法 Download PDF

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CN1047182C
CN1047182C CN94192384A CN94192384A CN1047182C CN 1047182 C CN1047182 C CN 1047182C CN 94192384 A CN94192384 A CN 94192384A CN 94192384 A CN94192384 A CN 94192384A CN 1047182 C CN1047182 C CN 1047182C
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G·J·布雷斯
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Hentzman ICI Chemical Product Co., Ltd.
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Abstract

一种制备聚氨酯软泡沫体的方法，包括使一种NCO值为5-10%(重量)的预聚物，即由含有至少85%(重量)4，4′-二苯甲烷二异氰酸酯或其变种的过量多异氰酸酯与平均名义羟基官能度为2.5-3.5、平均羟基当量重量为1000-3000，以及氧亚乙基含量为50-85%(重量)的多元醇反应而得到的反应产物与水反应，水的用量按每100重量份预聚物计为至少20重量份。

Description

软泡沫体的生产方法
通过有机多异氰酸酯如甲苯二异氰酸酯(TDI)或二苯甲烷二异氰酸酯(MDI)与聚醚多元醇在发泡剂存在下反应来生产聚氨酯软泡沫体的方法是很成熟的。所述聚醚通常是从环氧丙烷衍生出的聚氧亚丙基多元醇或从环氧丙烷和环氧乙烷的各种组合衍生出的聚(氧亚丙基-氧亚/乙基)多元醇。其中氧亚乙基基团构成总氧亚烷基链段次要部分的、以环氧乙烷封端的聚氧亚丙基多元醇是特别重要的，因为它们对异氰酸酯具有提高了的反应活性。参见例如EP-10850、EP-22617和EP-11121。
氧亚乙基含量较高，例如50％(重量)或更高的多元醇常常用作辅助添加剂以确保泡沫体具有开孔结构。但是，这些聚醚不能以很高的浓度与通常的异氰酸酯一起使用，因为此时它们不是具有开孔效果，而是导致闭孔泡沫体。现已发现，如果用纯的4,4′-MDI或其衍生物作为多异氰酸酯的话，就可从含有高浓度的具有高氧亚乙基含量的多元醇的配方成功地制得具有有价值的性能的软泡沫体。
US-4365025公开了使用高浓度的具有高氧亚乙基含量的多元醇的方法，然而却劝阻人们使用MDI。较早提交的EP-A-547765公开了使用基本上纯的4,4′-MDI和高浓度的具有高氧亚乙基含量的多元醇的方法，但是水的用量很少。
因此，本发明提供一种制备软聚氨酯泡沫体的方法：使NCO值为5-10％(重量)的预聚物，即由含有至少85％，较好至少90％，更好至少95％(重量)4,4′-二苯甲烷二异氰酸酯或其变种的过量多异氰酸酯与平均名义羟基官能度为2.5-3.5，平均羟基当量重量为1000-3000，以及氧亚乙基含量为50-85％(重量)的多元醇反应而得到的反应产物与水反应，水的用量按每100重量份预聚物计为至少20重量份。
本发明方法中所用的多异氰酸酯组分主要包括纯的4,4′-二苯甲烷二异氰酸酯或这种二异氰酸酯与一种或多种其它有机多异氰酸酯，尤其其它二苯甲烷二异氰酸酯异构体，例如2,4′-异构体的混合物，任选地结合有2,2′-异构体。该多异氰酸酯组分也可以是一种由含有至少85％(重量)4,4′-二苯甲烷二异氰酸酯的多异氰酸酯组合物衍生出的MDI变种。MDI变种在本技术中是众所周知的，对于可按照本发明使用的，特别包括通过将uretonimine和/或碳化二亚胺基团引入到所述多异氰酸酯组合物中和/或通过使这种组合物与一种或多种多元醇反应而得到的液体产物。较好是，该多异氰酸酯的官能度为2.05或更小，最好为2.00，而且最好是4,4′-MDI。
为了得到2.5-3.5的平均名义羟基官能度，可以使用名义羟基官能度为3的多元醇，或者平均名义羟基官能度为2-6的多元醇混合物，只要该混合物的官能度在2.5-3.5范围以上就行。
所述多元醇是一种聚氧亚烷基多元醇，较好是一种聚(氧亚乙基-氧亚丙基)多元醇，且应具有所要求的官能度、当量重量和氧亚乙基含量。这样的多元醇在本技术中是已知的，可按传统方法通过使环氧乙烷和环氧丙烷同时和/或依次以任何顺序与一种含有2-6个活泼氢原子的引发剂如水、多元醇、羟基胺和多胺或这些引发剂的混合物反应制得。
“平均名义羟基官能度”这一术语在此用来表示多元醇组合物的平均官能度(每个分子中的羟基数)，其中假设这里所存在的聚氧亚烷基多元醇的平均官能度与其制备时所用的引发剂的平均官能度(每个分子中活泼氢原子的数目)相等，虽然实际上由于某种程度的端部不饱和而往往略微小些。较好是，该多元醇组合物的平均名义羟基官能度为3。数均当量重量较好是1000-2000。最好的多元醇，其名义羟基官能度为3，平均羟基当量重量为1200-1600。
如果希望的话，聚氧亚烷基多元醇(或当使用这类多元醇的混合物时，一种或多种聚氧亚烷基多元醇)可以含有分散的聚合物颗粒。这种聚合物改性的多元醇在先有技术中已有详细叙述，而且包括由一种或多种乙烯单体，如丙烯腈和苯乙烯，在聚氧亚烷基多元醇中就地聚合或由一种多异氰酸酯和一种氨基-或羟基官能化合物，例如三乙醇胺，在聚氧亚烷基多元醇中就地反应而得到的产物。
所述的预聚物习惯上通过使多异氰酸酯和多元醇以能得到5-10％(重量)NCO值的相关量在较好为40-80℃的温度下反应来制备。这样制备的预聚物在环境条件下为液体。可以在如此制备的顶聚物中添加少量(最多30％(重量))的MDI或其变种，只要接所用的所有多异氰酸酯计算的4,4′-MDI含量仍能保持在85％(重量)以上以及所添加的多异氰酸酯的平均异氰酸酯官能度小于2.2就行。
所述预聚物在25℃的粘度较好至多为10,000mPa·S。
该预聚物与水反应，水的用量为每100重量份预聚物至少用20重量份水，较好用20-500，最好用25-400重量防水。
发泡反应混合物可以含有一种或多种制备软泡沫体中所用的添加剂。这类添加剂包括：催化剂，如叔胺和锡化合物，表面活性剂和泡沫稳定剂，如硅氧烷-氧亚烷基共聚物和氧亚乙基/氧亚丙基共聚物，链增长剂，如低分子量二醇和二胺，交联剂，如三乙醇胺，消毒剂，阻火剂，有机和无机填料，颜料，抑制所谓沸泡(boiling-foam)效应的试剂，如聚二甲基硅氧烷，以及内脱模剂等。但是，有价值的软泡沫体可以不用任何这些添加剂而制得。每100重量份预聚物除了加至多5重量份泡沫稳定剂外，较好不加任何添加剂。最好是不使用任何添加剂。如果要使用的话，较好将这些添加剂与水进行预混合。
该反应体系可用来制备具有优良性能的软泡沫体，方法极其简单。令人惊奇的是，这种预聚物的粘度低，在制造软泡沫体时易于处理和加工，所制得的泡沫体具有理想的颜色(白色)和开孔结构，容易压瘪，而且永久压缩形变值低于20％(ASTM D 3574-77,Test D，干燥50％)，尤其不用表面活性剂时更是如此。用于制备预聚物的化学品的纯度和单纯性确保了由其制得的软泡沫体只含最少量的可浸出物质，这就使得这种泡沫体在需要与人体接触的场合，如在医药和卫生方面特别有用。
该泡沫体可以制成块料，模制品等形式，用作减震材料、尿布、海棉、伤口敷料及塞头等。
下列实例说明本发明但不限制本发明。实例中所有份额、百分数及比例均指重量
下列材料术语用来说明实例中没有说明的反应组分。
术语：
A2580是指Arcol 2580，是一种含有无规氧亚乙基和氧亚丙基链段的聚醚三醇，其中氧亚乙基含量为77％，分子量约为4000，可从Arco公司购得。Arcol是Arco公司的商标。
多异氰酸酯1是一种uretonimine改性的4,4′-MDI，其NCO含量为29.3％，官能度为2.12。
多异氰酸酯2：含有约80％(重量)的4,4′-MDI，官能度为2.01。
DC-193是一种可从道康宁(DOW Corning)公司得到的硅氧烷表面活性剂。
实例1-3
使70重量份A2580和30重量份4,4′-MDI反应制备一种预聚物。使该预聚物与表1中所列组分反应制备一种软泡沫体。预聚物的NCO值为7.85％(重量)，粘度为6000mPa·S。
                 表1实例                              1        2        3预聚物                           100      100      90多异氰酸酯1/                      -        -       10多异氰酸酯2(1∶1/W∶W)DC-193                            -        -       0.1水                               300      50       25
该泡沫体泡孔细少，白色透明。实例3得到的泡沫体的密度为55Kg/M3(ISO 1855)；压缩载荷挠度(40％)为4.1 KPa(ISO3386)，滞后损耗为23％(ISO 3386)。
实例4-11
将多异氰酸酯和多元醇混合，让其起反应，从而制备预聚物。然后让预聚物与水(预聚物/水的重量比=100/60)反应，以便制得软泡沫体。详见表2数据。
                         表2实例                4              5             6            7           8          9          10          11异氰酸酯        4,4′-MDI      4,4′-MDI     4,4′-MDI    4,4′-MDI   4,4′-MDI  4,4′-MDI     IS01      4,4′-MDI(重量份)          (30)           (30)           (33)        (31.7)      (27.4)      (49)      (30.6)       (17)多元醇          多元醇1         多元醇2       多元醇3      多元醇4      多元醇     A2580      A2580       A2580(重量份)          (70)           (70)           (67)        (68.3)      (72.5)      (51)      (69.4)       (83)预聚物的NCO值   无法制备         7.85           7.85         7.85        7.85       14.8        7.7         3.2％重量           预聚物预聚物粘度         -             7200           13500      ＞50000       3600       1300      14800      ＞100000mPa·S                                                       太粘                  不稳定                   固体
                                                                               MDI沉淀泡沫体性能         -         合格泡沫体       合格泡沫体      -        不稳定泡    得不到   泡孔更封闭，    得不到
                                          但难以加工               沫体，撕裂  泡沫体   难以压瘪，难    泡沫体
                                                                   强度很低             以混合和加工多元醇1:4000 MW,100％ EO，名义官能度(f)=3多元醇。多元醇2:4000 MW,75％ EO-封端，f=3,EO/PO多元醇。多元醇3:2500 MW,75％ EO 无规，f=3,EO/PO多元醇。多元醇4:4000 MW,75％ EO 无规，f=4,EO/PO多元醇。多元醇5:4000 MW,75％ EO 无规，f=2,EO/PO多元醇。ISO1:4-4′-MDI/聚合的MDI为63/37(W/W)的共混物，t=2.20。实例12
使实例1中制备的预聚物与水反应(预聚物/水的重量比=100/70)。所制得的泡沫体为白色软泡沫体，密度为100Kg/M3，压缩变定(ASTM D 3574-77,Test D，干燥50％)为12％，容易压瘪。

Claims (7)

1、一种制备聚氨酯软泡沫体的方法，包括使一种NCO值为5-10％(重量)的预聚物，即由含有至少85％(重量)4,4′-二苯甲烷二异氰酸酯或其变种的过量多异氰酸酯与平均名义羟基官能度为2.5-3.5、平均羟基当量重量为1000-3000，以及氧亚乙基含量为50-85％(重量)的多元醇反应而得到的反应产物与水反应，水的用量按每100重量份预聚物计为至少20重量份。
2、按照权利要求1的方法，其中所述多元醇是聚(氧亚乙基-氧亚丙基)多元醇。
3、按照权利要求1或2的方法，其中所述多元醇的名义羟基官能度为3，平均羟基当量重量为1200-1600。
4、按照权利要求1或2的方法，其中所述多异氰酸酯含有至少90％(重量)4,4′-二苯甲烷二异氰酸酯。
5、按照权利要求1或2的方法，其中多异氰酸酯含有至少95％(重量)4,4′-二苯甲烷二异氰酸酯。
6、按照权利要求1或2的方法，其中多异氰酸酯的官能度至多为2.05。
7、按照权利要求1或2的方法，其中所述预聚物在25℃的粘度至多为10,000mPa·S。
CN94192384A 1993-06-08 1994-05-24 软泡沫体的生产方法 Expired - Fee Related CN1047182C (zh)

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AU6971194A (en) 1995-01-03
GR3024820T3 (en) 1998-01-30
GB9311838D0 (en) 1993-07-28
DE69405242D1 (de) 1997-10-02
CN1124966A (zh) 1996-06-19
JPH09501958A (ja) 1997-02-25
MY111107A (en) 1999-08-30
AU678258B2 (en) 1997-05-22
JP2005344122A (ja) 2005-12-15
HK1002143A1 (en) 1998-07-31
CA2161694A1 (en) 1994-12-22
GB9409544D0 (en) 1994-06-29
EP0707607A1 (en) 1996-04-24
JP3789470B2 (ja) 2006-06-21
ATE157377T1 (de) 1997-09-15
EP0707607B1 (en) 1997-08-27
TW301661B (zh) 1997-04-01
US5489620A (en) 1996-02-06
CA2161694C (en) 2004-01-27
DE69405242T2 (de) 1998-01-02

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