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CN110603305A - 可湿固化的聚氨酯热熔树脂组合物 - Google Patents

可湿固化的聚氨酯热熔树脂组合物 Download PDF

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CN110603305A
CN110603305A CN201780090459.7A CN201780090459A CN110603305A CN 110603305 A CN110603305 A CN 110603305A CN 201780090459 A CN201780090459 A CN 201780090459A CN 110603305 A CN110603305 A CN 110603305A
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polyol
adhesive composition
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polyurethane hot
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施锐
白晨艳
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Dow Global Technologies LLC
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Abstract

本公开提供一种包含多元醇组分和异氰酸酯组分的聚氨酯热熔粘合剂组合物，其中所述多元醇组分包含具有两个或更多个OH基团和氢桥接基团的多元醇。

Description

可湿固化的聚氨酯热熔树脂组合物
技术领域
本公开涉及具有改善的粘合强度和用于纸/箔层压的热封强度的可湿固化的聚氨酯热熔树脂组合物。本公开还涉及其中使用这种组合物的粘合剂和制品。
背景技术
常规的反应性聚氨酯热熔粘合剂用于包装、纸张转化、纸张构造、装订、纸箱、封箱、建筑、汽车等中。反应性聚氨酯热熔粘合剂可产生非常耐用的产品，并在包装和教科书的制造中特别有用。
常规的反应性聚氨酯热熔粘合剂是在室温下为固体的湿气固化或湿气交联粘合剂，但它们以熔体的形式施加。粘合剂的聚合物成分含有氨基甲酸酯基团和反应性异氰酸酯基团。熔体的冷却首先导致热熔粘合剂的快速物理固化，然后仍然存在异氰酸酯基团与环境中的湿气发生化学反应以形成交联的不溶性粘合剂。
然而，当将常规的反应性聚氨酯热熔粘合剂应用于纸/箔层压时，对于这种应用存在两个限制。第一，常规的反应性聚氨酯的高粘度导致差的润湿能力和较低的层压速度。同时，较高的应用温度(例如，高于100℃)不适用于纸/薄膜层压。此外，常规的反应性聚氨酯对于箔结构显示出较差的粘合强度。确切地说，在热封之后，完全固化的常规反应性聚氨酯粘合剂将易于从箔上剥离。
因此，在本领域中需要一种特别适合于粘合箔和纸的新颖的聚氨酯热熔粘合剂，其具有改善的性能，包括粘合强度和热封强度。
发明内容
本公开提供一种包含多元醇组分和异氰酸酯组分的聚氨酯热熔粘合剂组合物，其中所述多元醇组分包含具有两个或更多个OH基团和氢桥接基团的多元醇。
具体实施方式
根据本公开的聚氨酯热熔粘合剂组合物包含多元醇组分和异氰酸酯组分。
多元醇组分
聚氨酯热熔粘合剂组合物包含多元醇组分，所述多元醇组分包含具有两个或更多个OH基团和氢桥接基团的多元醇，以及任选的选自以下组成的组的多元醇：聚酯多元醇、聚醚多元醇和其组合。多元醇组分可任选地包括增粘剂，以及二醇或三醇单体。
具有两个或更多个OH基团和氢桥接基团的多元醇是具有两个或更多个末端OH基团(即在多元醇分子链的末端)和至少一个在侧分子链中的氢桥接基团(即，一个分支基团)的多元醇。合适的氢桥接基团的实例包括(但不限于)O＝C-Oˉ、O＝C-C-Oˉ和O＝C-C＝C-Oˉ以及其旋前形式。所公开的具有两个或更多个OH基团和氢桥接基团的多元醇还具有至少50mgKOH/g且不超过200mg KOH/g的酸值。此外，所公开的多元醇具有至少400g/mol且不超过5,000g/mol的分子量。又另外，所公开的多元醇具有至少1.8且不超过3的羟基官能度(即，1.8≤f≤3)。在一些实施例中，具有两个或更多个OH基团和氢桥接基团的多元醇是聚酯多元醇。
以粘合剂组合物的重量计，粘合剂组合物中具有两个或更多个OH基团和氢桥接基团的多元醇的量按重量计为至少3wt％、或至少3.5wt％、或至少4wt％。以粘合剂组合物的重量计，粘合剂组合物中具有两个或更多个OH基团和氢桥接基团的多元醇的量按重量计不超过40wt％、或50wt％、或80wt％。
具有两个或更多个羟基的化合物为“多元醇”。具有恰好两个羟基的多元醇为“二醇”。具有恰好三个羟基的多元醇为“三醇”。同一直链原子链中含有两个或更多个酯键的化合物在本文中称为“聚酯”。作为聚酯和多元醇的化合物在本文中称为“聚酯多元醇”。所公开的聚酯多元醇具有不超过4,000g/mol的分子量。此外，所公开的聚酯多元醇具有至少1.5且不超过3的羟基官能度(即，1.5≤f≤3)。
适合根据本公开使用的聚酯多元醇是二醇并且任选地也是多元醇(例如，三醇、四醇)与二羧酸并且任选地也是与聚羧酸(例如，三羧酸、四羧酸)或羟基羧酸或内酯的已知缩聚物。聚酯多元醇也可以衍生自相应的聚羧酸酐或相应的低级醇的聚羧酸酯，而不是游离的聚羧酸。
合适的二醇包括(但不限于)乙二醇、丁二醇、二乙二醇、三乙二醇、聚亚烷基二醇(例如聚乙二醇)以及1,2-丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,6-己二醇和新戊二醇。为了获得大于2的聚酯多元醇官能度，官能度为3的多元醇可任选地包括在粘合剂组合物中(例如，三羟甲基丙烷、丙三醇、赤藻糖醇、季戊四醇、三羟甲基苯或异氰脲酸三羟乙酯)。
合适的二羧酸包括(但不限于)脂肪族酸、芳香族酸和其组合。合适的芳香族酸的实例包括邻苯二甲酸、间苯二甲酸、对苯二甲酸和四氢邻苯二甲酸。合适的脂肪族酸的实例包括六氢邻苯二甲酸、环己烷二羧酸、己二酸、壬二酸、癸二酸、戊二酸、四氯邻苯二甲酸、马来酸、富马酸、衣康酸、丙二酸、辛二酸、2-甲基琥珀酸、3,3-二乙基戊二酸、2,2-二甲基琥珀酸和偏苯三酸。如本文所使用，术语“酸”还包括所述酸的任何酸酐。此外，应当从所公开的组合物中最小化或排除一元羧酸，例如苯甲酸和己烷羧酸。优选饱和脂肪族或芳香族酸，例如己二酸或间苯二甲酸。
在同一直链原子链中含有两个或更多个醚键的化合物在本文中称为“聚醚”。作为聚醚和多元醇的化合物为“聚醚多元醇”。所公开的聚醚多元醇具有不超过5,000g/mol的分子量。此外，所公开的聚醚多元醇具有至少1.5且不超过4的羟基官能度(即，1.5≤f≤4)。
适合根据本公开使用的聚醚多元醇是环氧乙烷、环氧丙烷、四氢呋喃、环氧丁烷的加聚产物，及其共加成和接枝产物，以及通过多元醇缩合得到的聚醚多元醇或其混合物。适用的聚醚多元醇的实例包括(但不限于)聚丙二醇(“PPG”)、聚乙二醇(“PEG”)、聚丁二醇和聚四亚甲基醚二醇(“PTMEG”)。
所公开的多元醇组分可任选地进一步包含生物基多元醇，例如蓖麻油或其它已知的生物基多元醇。所公开的生物基多元醇具有至少1.5且不超过4的羟基官能度(即，1.5≤f≤4)。
所公开的多元醇组分可任选地进一步包含一些小分子量扩链剂，其包括(但不限于)二醇和三醇，例如乙二醇、丁二醇、二乙二醇、三乙二醇、聚亚烷基二醇(例如聚乙二醇)，以及1,2-丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,6-己二醇、新戊二醇、三羟甲基丙烷、丙三醇、赤藻糖醇、季戊四醇、三羟甲基苯和异氰脲酸三羟乙酯。
异氰酸酯组分
异氰酸酯组分包含至少一种异氰酸酯。
如本文中所使用，“聚异氰酸酯”是含有两个或更多个异氰酸酯基的任何化合物。“芳香族聚异氰酸酯”是含有一个或多个芳香族环的聚异氰酸酯。“脂肪族聚异氰酸酯”不含芳香族环。
适合根据本公开使用的聚异氰酸酯可选自由芳香族聚异氰酸酯、脂肪族聚异氰酸酯和其组合组成的组。适合根据本公开使用的芳香族聚异氰酸酯的实例包括(但不限于)亚甲基二苯基二聚异氰酸酯(“MDI”)的异构体，例如4,4-MDI、2,4-MDI和2,2'-MDI；甲苯-二聚异氰酸酯(“TDI”)的异构体，例如2,4-TDI、2,6-TDI；萘-二聚异氰酸酯(“NDI”)的异构体，如1,5-NDI；和其组合。适合根据本公开使用的脂肪族聚异氰酸酯的实例包括(但不限于)六亚甲基二聚异氰酸酯(“HDI”)的异构体、异佛尔酮二聚异氰酸酯(“IPDI”)的异构体、二甲苯二聚异氰酸酯(“XDI”)的异构体、氢化苯基甲烷二异氰酸酯(“HMDI”)的异构体和其组合。在一些实施例中，芳香族聚异氰酸酯包含MDI的异构体。
聚异氰酸酯化合物可以用参数“％NCO”表征，所述参数是按重量计的聚异氰酸酯的量(按化合物重量计)。参数％NCO通过ASTM D 2572-97(2010)方法来测量。所公开的异氰酸酯组分具有至少2wt％、或至少5wt％、或至少7wt％的％NCO。在一些实施例中，异氰酸酯组分具有不超过30wt％、或25wt％、或22wt％、或19wt％的％NCO。
在一些实施例中，异氰酸酯组分在25℃下具有300mPa-s到100,000mPa-s的粘度，如根据ASTM D2196方法所测量。
异氰酸酯组分可任选地包含一种或多种催化剂。适合根据本公开使用的至少一种催化剂的实例包括(但不限于)二月桂酸二丁基锡、乙酸锌、2,2-二吗啉基二乙醚和其组合。
在一些实施例中，异氰酸酯组分与多元醇组分的重量比为4:1或更高，或4.5:1或更高；或5:1或更高。在一些实施例中，异氰酸酯组分与多元醇组分的重量比为1:1或更低，或1:2或更低，或1:4或更低。
在一些实施例中，粘合剂组合物任选地包含增粘剂，例如氨基硅烷。
聚氨酯热熔粘合剂组合物的制备是用所属领域的一般技术人员所熟知的任何方式，包括缩合聚合。聚氨酯粘合剂组合物配方公开的化学计量使得二异氰酸酯过量存在，且所述聚氨酯粘合剂组合物为NCO基团封端的。在一些实施例中，聚氨酯粘合剂组合物具有3％到10％、或4％到9％或5％到8％的异氰酸酯含量(也称为％NCO，如通过ASTM D2572所测量)。
还公开一种使用聚氨酯粘合剂组合物形成层压材料的方法。在一些实施例中，聚氨酯粘合剂组合物为液态。在一些实施例中，所述组合物在25℃下是液体。即使所述组合物在25℃下是固体，但仍可接受视需要加热所述组合物以使其处于液态。可以通过涂布辊将聚氨酯粘合剂组合物的层施加到箔的表面或纸的表面上，然后将水添加到聚氨酯粘合剂组合物层上。“箔”是在一个维度上为6μm到20μm且在另外两个维度上均为1cm或更大的结构。优选地，箔片由铝制成。“纸”是在一个维度上为10μm到200μm且在另外两个维度上均为1cm或更大的结构。“纸”由植物纤维或聚合物树脂制成，并且合适的实例包括牛皮纸、白卡纸、胶版纸、铜版纸等。通过压力辊将纸的表面(或箔的表面)进一步与箔/粘合剂(或纸/粘合剂)复合材料层压，以形成箔/粘合剂/纸(或纸/粘合剂/箔)层压材料。
实例
现在将通过说明性实例和比较实例(统称为“实例”)进一步详细解释本公开。然而，本公开的范围当然不限于实例中所阐述的调配物。实际上，实例仅为本公开的说明。
聚氨酯粘合剂组合物制备
用于制备实例的原材料在下表1中通过商业名称和供应商确定。
表1：原材料
按照以下步骤合成聚氨酯粘合剂组合物实例(说明性实例1到7(IE1-7)和比较实例1到3(CE1-3))：步骤1)将一种或多种异氰酸酯组分装入反应器中并保持在60℃下用氮气保护，步骤2)在约80℃的增大温度下将一种或多种多元醇组分缓慢地装入同一反应器中并保持直到“％NCO”到达所计算的范围内。然后将制备的聚氨酯粘合剂组合物用于与纸和铝箔形成层压材料以进行性能测试。
表2：聚氨酯粘合剂组合物实例CE1-3和IE1-7
层压材料性能测试
将粘合剂组合物以3.5gsm涂层重量涂覆到纸上，与铝膜结合在一起，然后在50℃下固化24小时以形成层压材料。一旦形成层压材料，就进行测试以分析粘合强度和热封强度，
1.基材撕裂测试
在固化后，将层压膜切成15mm宽的带材，以用于在具有250mm/min的十字头速度的Instron 5943机器中进行T-剥离测试。测试三条带材以取得平均值。在测试期间，用手指轻轻拉动带材的尾部以确保尾部与剥离方向保持90度。撕裂测试后纸表面的损坏率记录为层压牢度。
2.热封强度测试
将层压材料在220℃密封温度和300N压力下在可从布鲁格公司(BruggerCompany)获得的HSG-C热封机器中热封1秒，然后冷却并切割成15mm宽的带材以用于在250mm/min十字头速度下使用可从英斯特朗公司(Instron Corporation)获得的5940系列单柱桌面系统(5940Series Single Column Table Top System)进行热封强度测试。测试每个样品的三条带材并计算平均值。结果以N/15mm为单位。
3.粘度测试
在进行测试之前，将层压材料放置在100℃的热烤箱中几个小时。粘度在100℃下在布鲁克菲尔德(Brookfield)DV-II粘度计中使用27号转轴来测量。旋转速度为12RM，并且测试层压材料20分钟以达到稳定旋转测试。
表3：性能测试结果
与比较实例相比，说明性实施例对于纸/箔层压表现出良好的粘合强度和热封强度。随着DMPATM Polyol HA-0135聚酯多元醇的含量增加，在撕裂测试后检测到更高的纸张断裂率。当DMPATM Polyol HA-0135聚酯多元醇的含量达到6.3％时，撕裂测试后的纸张断裂率将变得稳定并达到90％断裂率。然而，当DMPATM Polyol HA-0135聚酯多元醇的含量小于6.3％时，纸张断裂率很低，这对于此应用是不可接受的。此外，对于比较实例，在热封之后检测到隧道和分层。

Claims (10)

1.一种聚氨酯热熔粘合剂组合物，其包含多元醇组分和异氰酸酯组分，其中所述多元醇组分包含具有两个或更多个OH基团和氢桥接基团的多元醇。
2.根据权利要求1所述的聚氨酯热熔粘合剂组合物，其中所述氢桥接基团选自O＝C-Oˉ、O＝C-C-Oˉ和O＝C-C＝C-Oˉ，以及其旋前形式。
3.根据权利要求1所述的聚氨酯热熔粘合剂组合物，其中具有两个或更多个OH基团和氢桥接基团的所述多元醇具有至少50mg KOH/g且不超过200mg KOH/g的酸值。
4.根据权利要求1所述的聚氨酯热熔粘合剂组合物，其中具有两个或更多个OH基团和氢桥接基团的所述多元醇具有至少400g/mol且不超过5,000g/mol的分子量。
5.根据权利要求1所述的聚氨酯热熔粘合剂组合物，其中具有两个或更多个OH基团和氢桥接基团的所述多元醇具有至少1.8且不超过3的羟基官能度。
6.根据权利要求1所述的聚氨酯热熔粘合剂组合物，其中基于粘合剂组合物的重量，具有两个或更多个OH基团和氢桥接基团的所述多元醇为至少3wt％且不超过80wt％。
7.根据权利要求1所述的聚氨酯热熔粘合剂组合物，其中所述异氰酸酯组分包含至少一种选自以下的聚异氰酸酯：芳香族聚异氰酸酯、脂肪族聚异氰酸酯及其组合。
8.根据权利要求1所述的聚氨酯热熔粘合剂组合物，其中所述异氰酸酯组分具有至少2wt％且不超过30wt％的％NCO。
9.根据权利要求1所述的聚氨酯热熔粘合剂组合物，其中具有两个或更多个OH基团和氢桥接基团的所述多元醇为聚酯多元醇。
10.一种层压材料，其用根据权利要求1所述的聚氨酯热熔粘合剂组合物将箔和纸粘合。
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