CN1282680C - 微孔弹性聚氨基甲酸酯泡沫体 - Google Patents
微孔弹性聚氨基甲酸酯泡沫体 Download PDFInfo
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- CN1282680C CN1282680C CNB021522014A CN02152201A CN1282680C CN 1282680 C CN1282680 C CN 1282680C CN B021522014 A CNB021522014 A CN B021522014A CN 02152201 A CN02152201 A CN 02152201A CN 1282680 C CN1282680 C CN 1282680C
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
- C08G18/4837—Polyethers containing oxyethylene units and other oxyalkylene units
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2110/00—Foam properties
- C08G2110/0008—Foam properties flexible
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2110/00—Foam properties
- C08G2110/0041—Foam properties having specified density
- C08G2110/0066—≥ 150kg/m3
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2110/00—Foam properties
- C08G2110/0083—Foam properties prepared using water as the sole blowing agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2410/00—Soles
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
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Abstract
本发明是有关一种微孔弹性聚氨基甲酸酯泡沫体，其密度小于1000千克/立方米且肖氏A硬度为至少75。
Description
本申请是申请号为97195854.8、国际申请日为1997年6月2日的PCT申请的分案申请。
技术领域
本发明涉及微孔弹性聚氨基甲酸酯泡沫体及其制备方法。
背景技术
传统聚氨基甲酸酯弹性物是由配方制得，配方中硬性嵌段-含量约30至40重量％(硬性嵌段-含量在此定义为聚异氰酸酯，增链剂以及视需要之交联剂的数量总和，其相对于聚合物总量之重量百分率)。
具较高硬性嵌段-含量的配方是难以加工的，且所得产物有非常高的硬度。
已经有用包含高量4，4′-MDI与高EO-含量的聚醚多元醇的配方来制备弹性聚氨基甲酸酯泡沫体，例子可见EP-A 547764、EP-A 547765与EP-A 549120。
亦知有从具低环氧乙烯(EO)-含量的聚醚多元醇来制备弹性聚氨基甲酸酯的方法，例子可见US-A 5122548与EP-A 13487。
发明内容
令人惊讶地是，现在已经发现可能制造的微孔聚氨基甲酸酯弹性泡沫体，其具有非常高硬性嵌段-含量，却没有过高的硬度，而在宽的密度范围中仍是容易加工的。
因此，根据本发明提供一种用来制备微孔弹性聚氨基甲酸酯泡沫体的方法，其反应混合物包括：聚异氰酸酯成份、多元醇组合物、增链剂、水及视需要之交联剂，其中聚异氰酸酯成份包含至少85重量％的4，4′-二苯甲烷二异氰酸酯或其变体；多元醇组合物则包含至少一种含有氧乙烯残基的聚氧亚烷或其变体；多元醇组合物则包含至少一种含有氧乙烯残基的聚氧亚烷基多元醇，该多元醇组合物之平均标称羟基官能度为2至6、平均羟基当量至少1300且平均氧乙烯成份介于50至85重量％之间；以及平均羟基当量从15至250之增链剂；硬性嵌段-含量是大于45重量％。
用于本发明方法中的聚异氰酸酯组分含量基本上可由纯4，4′-二苯甲烷二异氰酸酯或二异氰酸酯与一或多种其它有机聚异氰酸酯，尤其是其它二苯甲烷二异氰酸酯异构物的混合物所组成，例如2，4′-异构物视需要与2，2′-异构物结合。该聚异氰酸酯组分亦可为一种MDI变体，其是从含至少85重量％4，4′-二苯甲烷二异氰酸酯之聚异氰酸酯组合物衍生而来。MDI变体在本领域中是众所皆知的，为了与本发明一致使用，特别包括液态产物，其是藉由将脲酮亚胺(uretonimine)和/或碳化二亚胺基导入该聚异氰酸酯组合物和/或与一或多种多元醇反应而得到。
当作聚异氰酸酯组份优选的为含有至少90重量％4，4′-二苯甲烷二异氰酸酯的聚异氰酸酯组合物。最优选的有至少95重量％4，4′-二苯甲烷二异氰酸酯之聚异氰酸酯组合物。
用于此处之“平均标称羟基官能度”一词是指：在出现于其中之聚氧亚烷基多元醇平均官能度与用于其制备中引发剂平均官能度(每分子的活性氢原子数)是相同的假设下(尽管实际上因为一些终端未饱和使用使得它通常会较少)，多元醇组合物的平均官能度(每分子的羟基数目)。多元醇组合物的平均标称羟基官能度优选的为从2至4，最优选的聚氧亚烷基多元醇为二醇或三醇。
该组合物可包含单一聚氧亚烷基多元醇，其优选的为具所需平均标称羟基官能度、羟基当量与氧乙烯含量的聚(氧亚乙基-氧亚丙基)多元醇。这类多元醇在本领域中为已知的，且可以传统方法藉由将环氧乙烷与环氧丙烷同时且/或依序地任意与具有2至6活性氢原子的引发剂诸如水、多元醇、羟胺或聚胺及类似物反应而得。多元醇引发剂的例子有：乙二醇、二乙二醇、丙二醇、二丙二醇、1，3-丙二醇、新戊二醇、1-丁二醇、1，5-戊二醇、1，6-己二醇、丙三醇、三羟甲基丙烷、赤藓醇、木糖醇、葡萄糖、果糖、甘露糖醇或山梨糖醇。
或者是，多元醇组合物可包含二或多种多元醇的混合物，使得总组合物具有所要求的平均标称羟基官能度、平均羟基当量与氧乙烯含量其它多元醇可选自：聚醚、聚酯、聚硫醚、聚碳酸酯、聚缩醛、聚烯或聚硅氧烷。
聚醚多元醇可为，例如，含小于50重量％或大于85重量％氧乙烯残基的聚氧亚丙基多元醇、聚氧亚乙基多元醇或聚(氧亚乙基-氧亚丙基)多元醇。
可用的聚酯多元醇包括：二元醇诸如乙二醇、丙二醇、二乙二醇、1-丁二醇、新戊二醇、1，6-己二醇或环己烷二甲醇或这些二元醇的混合物的羟基终端反应产物，以及二羟酸或其形成的酯的衍生物，例如琥珀酸、戊二酸与己二酸或其二甲基酯、癸二酸、邻苯二甲酸酐、四氯化邻苯二甲酸酐或对苯二甲酸二甲基酯或其混合物的反应产物。
聚酰胺酯可藉由将胺基醇诸如乙醇胺包含在聚酯化混合物中而得到。
可用的聚硫醚多元醇包括将硫二甘醇单独或与其它乙二醇、环氧烷类、二羟酸、甲醛、氨基醇或氨基羟酸浓缩后所得的产物。
可用的聚碳酸酯多元醇包括将二醇诸如1，3-丙二醇、1-丁二醇、1，6-己二醇二乙二醇或四乙二醇与碳酸二芳基酯，比如碳酸二苯酯，或与光气反应所得的产物。
可用的聚缩醛多元醇包括将二醇诸如二乙二醇，三乙二醇或己二醇与甲醛反应而制备得到的那些物质。适合的聚缩醛也可以藉由将环状缩醛聚合而制得。
适合的聚烯多元醇包括羟基终端的丁二烯均-或共聚合物，而适当的聚硅氧烷多元醇包括聚二甲基硅氧烷二醇。
可用的其它多元醇包括上述类型多元醇的加成或浓缩聚合物的分散是或溶液。这些已改性多元醇，通常指作“聚合物”多元醇，已详细说明于先前技术中，并包括将一或多种乙烯单体，例如苯乙烯或丙烯腈在聚合多元醇例如聚醚多元醇中的就地聚合反应，或藉由聚异氰酸酯与氨基-和/或羟官能基化合物的就地反应，比如三乙醇胺，在聚合多元醇中的反应所得的产物。
优选的是，多元醇组合物平均羟基当量至少有1500。多元醇组合物的平均氧乙烯含量优选的为60～85重量％。
适当的低分子量增链剂包括：脂肪族二醇，比如乙二醇、1，3-丙二醇、2-甲基-1，3-丙二醇、1，4-丁二醇、1，5-戊二醇、1，6-己二醇、1，2-丙二醇、1，3-丁二醇、2，3-丁二醇、1，3-戊二醇，1，2-己二醇、3-甲基戊烷-1，5-二醇、2，2-二甲基-1，3-丙二醇、二乙二醇、二丙二醇与三丙二醇，以及氨基醇诸如乙醇胺、N-甲基二乙醇胺、N-乙基-二乙醇胺与类似物。优选的为乙二醇。
以异氰酸酯-反应性化合物总重量为基准，适宜水量为小于2重量％，且优选小于1重量％。
另一方面，本发明涉及微孔弹性聚氨基甲酯酯泡沫体，其密度小于1000千克/立方米及肖氏(Shore)A硬度至少75。优选的密度小于800千克/立方米及肖氏A硬度至少80。最优选的是微孔弹性聚氨基甲酸酯泡沫体密度小于600千克/立方米及肖氏A硬度至少85。
另一方面，本发明提供的反应体系包括：
(i)含至少85重量％4，4′-二苯甲烷二异氰酸酯或其变体的聚异氰酸酯；
(ii)包含至少一种含氧乙烯残基的聚氧亚烷基多元醇的多元醇组合物，该多元醇组合物平均标称羟基官能度为2至6，平均羟基当量至少1300且平均氧乙烯含量从50至85重量％；
(iii)平均羟基当量从15至250之增链剂；
(iv)水，及视需要之
(v)传统弹性体配方中的一或多种添加剂。
本反应体系是用来制造微孔弹性聚氨基甲酸酯泡沫体。
“反应体系”一词是定义为一个体系，其中聚异氰酸酯放在于一个与异氰酸酯-反应性成分分开的容器中。
本反应体系之异氰酸酯指数，计算包括多元醇组合物、水与任何其它异氰酸酯-反应性物种，例如增链或交联剂，可能低至85或高至120。优选的是，异氰酸酯指数介于90与110之间。
硬性嵌段-含量优选的至少占总组合物重量之50％。
可添加具平均官能度3或更多的低分子量异氰酸酯-反应性化合物，比如甘油、五赤藓醇或三乙醇胺来当作交联剂。
形成泡沫体的反应混合物可包含一或多种传统用于这些反应混合物的添加剂。这些添加剂包括催化剂，例如叔胺与锡化合物，表面活性剂与泡沫稳定剂，例如硅氧烷-氧化烯共聚合物，阻燃剂，有机与无机填充剂，颜料，以及内脱模剂。
本制程可根据“一次射出”、“半预聚合物”或“预聚合物”方法来执行。
藉由本发明方法可制造大范围的弹性产物。
由本发明方法产生的弹性体可用于各式各样的应用，例如鞋底与舵轮。
具体实施方式
本发明是藉由下列实施例来说明，其中所有份数、百分率与比率都是重量比。
包括下列物质的名词以用来区别反应组分，于实施例中不另外区别。
名词
聚异氰酸酯I：纯4，4′-MDI(Suprasec MPR；可购自ICI PLC；Suprasec为ICI PLC的商标)。
聚异氰酸酯II：经脲酮亚胺改性的MDI(Suprasec 2020；可购自ICI PLC；Suprasec为ICI PLC的商标)。
多元醇A：Arcol 2580，一种具无规氧乙烯与氧丙烯残基的聚醚三醇，具有76％氧乙烯含量及OH-值42毫克KOH/克，可购自ARCO；ARCOL是ARCO之商标。
多元醇B：具10％EO-尖端(tip)与OH-值36毫克KOH/克的EO-PO三醇。
多元醇C：具75％无规EO-基且MW＝4000的EO/PO二醇。
催化剂：Dabco EG(Dabco的33％EG溶液，可得自爱尔产物(AirProducts)；Dabco是爱尔产物之商标)。
EG：乙二醇。
DEG：二乙二醇。
实施例1-3与比较实施例1-4
弹性物是在一个15×10×1厘米的模型中用传统方法由下表配方塑模成型。
第一表
| 实施例1 | 实施例2 | 实施例3 | 比较实施例1 | 比较实施例2 | 比较实施例3 | 比较实施例4 | |
| 多元醇A | 100 | 100 | - | 100 | - | - | - |
| 多元醇B | - | - | - | - | 100 | 100 | 100 |
| 聚醇C | - | - | 100 | - | - | - | - |
| EG | 16.3 | 14 | 20 | 7.23 | 7.46 | 16.56 | 14.2 |
| DEG | - | 14 | - | - | - | - | 14.2 |
| 催化剂 | 0.5 | 0.5 | 0.7 | 1 | 1 | 0.5 | 0.5 |
| 水 | 0.3 | 1 | 0.7 | 0.3 | 0.3 | 0.3 | 1 |
| 聚异氰酸酯I | 指数100 | 指数100 | - | 指数100 | 指数100 | 指数100 | 指数100 |
| 聚异氰酸酯II | - | - | 指数100 | - | - | - | - |
| 硬性嵌段含量(重量％) | 50 | 50 | 57 | 35 | 35 | 50 | 50 |
| 性质 | |||||||
| 密度(千克/立方米) | 702 | 536 | 420 | 650 | 651 | 易碎材料 | 易碎材料 |
| 肖氏A硬度 | 89 | 90 | 85 | 42 | 72 | ||
| 阿斯卡(ASKER)C硬度 | 93 | 90 | 89 | 66 | 82 | 无泡沫体 | 无泡沫体 |
| 球体反弹 | 36 | 26 | N.M.(*) | 64 | 57 |
N.M.(*)：未测得
这些实施例显示在高硬性嵌段配方中利用具高氧乙烯含量的多元醇得到具有价值性质的弹性物，其达高硬度仍具加工性，而以含低氧乙烯含量的多元醇配方则是不可能或非常困难的。
Claims (3)
1.一种微孔聚氨基甲酸酯弹性泡沫体，其密度至少为420千克/立方米以及小于1000千克/立方米，其肖氏A硬度为至少75，且其含有至少50重量％的硬性嵌段。
2.根据权利要求1的微孔聚氨基甲酸酯弹性泡沫体，其密度小于800千克/立方米且肖氏A硬度为至少80。
3.根据权利要求2的微孔聚氨基甲酸酯弹性泡沫体，其密度小于600千克/立方米且肖氏A硬度为至少85。
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| GB8908490D0 (en) * | 1989-04-14 | 1989-06-01 | Ici Plc | Prepolymers |
| EP0547765B1 (en) * | 1991-12-17 | 1997-06-11 | Imperial Chemical Industries Plc | Polyurethane foams |
| EP0912623B1 (en) * | 1996-06-27 | 2001-12-05 | Huntsman International Llc | Microcellular elastomeric polyurethane foams |
-
1997
- 1997-06-02 EP EP97927102A patent/EP0912623B1/en not_active Expired - Lifetime
- 1997-06-02 BR BR9709988A patent/BR9709988A/pt not_active IP Right Cessation
- 1997-06-02 WO PCT/EP1997/002853 patent/WO1998000450A1/en not_active Ceased
- 1997-06-02 DE DE69708875T patent/DE69708875T2/de not_active Expired - Lifetime
- 1997-06-02 CA CA002258677A patent/CA2258677C/en not_active Expired - Fee Related
- 1997-06-02 AU AU31712/97A patent/AU725188B2/en not_active Ceased
- 1997-06-02 JP JP50378098A patent/JP3910214B2/ja not_active Expired - Fee Related
- 1997-06-02 ES ES97927102T patent/ES2169398T3/es not_active Expired - Lifetime
- 1997-06-02 PL PL97330920A patent/PL188405B1/pl not_active IP Right Cessation
- 1997-06-02 CN CNB021522014A patent/CN1282680C/zh not_active Expired - Fee Related
- 1997-06-02 DK DK97927102T patent/DK0912623T3/da active
- 1997-06-02 PT PT97927102T patent/PT912623E/pt unknown
- 1997-06-02 CN CN97195854A patent/CN1111555C/zh not_active Expired - Fee Related
- 1997-06-02 TR TR1998/02707T patent/TR199802707T2/xx unknown
- 1997-06-04 TW TW086107683A patent/TW445271B/zh not_active IP Right Cessation
- 1997-06-10 US US08/872,037 patent/US5968993A/en not_active Expired - Lifetime
- 1997-06-25 ID IDP972178A patent/ID17547A/id unknown
- 1997-06-27 AR ARP970102878A patent/AR007666A1/es active IP Right Grant
-
2006
- 2006-05-23 JP JP2006142753A patent/JP4680130B2/ja not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| EP0912623B1 (en) | 2001-12-05 |
| DE69708875D1 (en) | 2002-01-17 |
| PL188405B1 (pl) | 2005-01-31 |
| US5968993A (en) | 1999-10-19 |
| CA2258677A1 (en) | 1998-01-08 |
| JP3910214B2 (ja) | 2007-04-25 |
| AR007666A1 (es) | 1999-11-10 |
| CA2258677C (en) | 2008-05-13 |
| AU725188B2 (en) | 2000-10-05 |
| JP2000513404A (ja) | 2000-10-10 |
| DK0912623T3 (da) | 2002-03-04 |
| CN1422882A (zh) | 2003-06-11 |
| DE69708875T2 (de) | 2002-06-20 |
| JP2006219682A (ja) | 2006-08-24 |
| EP0912623A1 (en) | 1999-05-06 |
| CN1111555C (zh) | 2003-06-18 |
| CN1223674A (zh) | 1999-07-21 |
| BR9709988A (pt) | 1999-08-10 |
| TR199802707T2 (xx) | 1999-03-22 |
| AU3171297A (en) | 1998-01-21 |
| TW445271B (en) | 2001-07-11 |
| PL330920A1 (en) | 1999-06-07 |
| WO1998000450A1 (en) | 1998-01-08 |
| PT912623E (pt) | 2002-04-29 |
| ES2169398T3 (es) | 2002-07-01 |
| JP4680130B2 (ja) | 2011-05-11 |
| ID17547A (id) | 1998-01-08 |
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