CN117402585A - 一种湿固化热熔胶及其制备方法 - Google Patents
一种湿固化热熔胶及其制备方法 Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
本申请涉及热熔胶的领域,具体涉及一种湿固化热熔胶及其制备方法。该热熔胶包括如下组分:聚酯二元醇、异氰酸酯、聚丙二醇二丙烯酸酯、马来酸酐、增粘树脂、抗氧剂、扩链剂、消泡剂、催化剂;其制备方法包括如下步骤:称取聚酯二元醇、聚丙二醇二丙烯酸酯和增粘树脂加至三口反应器,升温至熔融并搅拌;称取异氰酸酯加至三口反应器中并搅拌;称取马来酸酐加至三口反应器,减压蒸馏后降温;称取抗氧剂、扩链剂、消泡剂、催化剂加至三口反应器,随后充分反应,得到粗品;氮气保护下将粗品熟化。本申请通过聚酯二元醇、聚丙二醇二丙烯酸酯、异氰酸酯和马来酸酐相互交联键合形成类四元穿插网络结构,同时优化了聚氨酯耐候性差和初粘力差的问题。
Description
技术领域
本申请涉及热熔胶的领域,更具体地说,它涉及一种湿固化热熔胶及其制备方法。
背景技术
热熔胶是一种可塑性的胶粘剂,在一定温度范围内其物理状态随温度改变而改变,而化学特性不变,其无毒无味,属环保型化学产品。因其产品本身系固体,便于包装、运输、存储、无溶剂、无污染,以及生产工艺简单,高附加值,黏合强度大、速度快等优点而备受青睐。
聚氨酯热熔胶是以聚氨酯树脂或预聚物为主体材料,配以各种助剂(如催化剂、抗氧剂、增粘剂及填料等)而制得的一类热熔胶。从结构上说,聚氨酯热熔胶主要是以异氰酸酯与多元醇为主要原料合成的预聚物。该预聚物主要以硬段和软段组成,硬段主要指氨基甲酸、脲键等,软段主要指多元醇,此结构决定了聚氨酯热熔胶材料的胶膜坚韧,耐冲击,挠曲性好,且具有剥离强度高、良好的耐低温性能、弹韧性、耐溶剂性、耐疲劳性和耐磨性等优点,可用于粘接聚氨酯海绵、橡胶、橡胶与织物、橡胶与金属、金属与金属、金属与陶瓷、木材与木材和橡胶与塑料等等。目前,聚氨酯胶粘剂发展迅速,其产品种类也日益繁多,应用领域越来越广泛,已成为国内外发展最快的胶粘剂之一。其中,湿固化聚氨酯热熔胶是以-NCO基作为封端基团预聚物,加热熔融施胶于被粘物与基材之间,首先冷却固化,形成一定的初粘力。接着靠基材与被粘物上的水分或者周围环境的湿气进行湿固化交联,即聚氨酯热熔胶中的-NCO基团与水分子中或者其它含活泼氢的化合物进行化学反应,生成氨基甲酸酯基(-NHCOO-),接着氨基甲酸酯继续与(-NCO)基团反应生成脲基甲酸酯(-NHCONH-),脲基继续与(-NCO)基团进行反应生成缩二脲结构。因为独特的遇水固化的机制,湿固化聚氨酯热熔胶逐渐成为炙手可热的聚氨酯热熔胶。
但是,聚氨酯热熔胶依然存在如下缺点:
1.初粘力差;由于聚氨酯热熔胶依赖异氰酸酯和多元醇反应,生成高分子量的聚合物,因此很难一蹴而就地硬化,往往需要一定的时间使得分子完全交联,这就导致了聚氨酯热熔胶的初粘力差,在一些需要胶粘剂快速固化的场合不太适用。
2.耐候性不佳;聚氨酯热熔胶分子中,往往存在大量的羟基、异氰酸酯基等活性基团,在紫外线、水分等作用下,这些活性基团可能键合或者水解,导致胶粘能行下降。但是受制于其施工工艺,若在其固化过程中加入基团抑制剂来增加减小其活性基团的活性,可能又会对其初粘力、粘接牢固程度等性能造成不利影响。
因此,综上所述,若是可以克服现有聚氨酯热熔胶存在的初粘力差、耐候性不佳的缺陷,将会给聚氨酯热熔胶提供更加广阔的市场。
发明内容
为了改善相关技术中聚氨酯热熔胶初粘力差、耐候性不佳的缺陷,本申请提供一种湿固化热熔胶及其制备方法,利用聚酯二元醇、异氰酸酯、聚丙二醇二丙烯酸酯、马来酸酐形成“类四元”的交联网络,增加了该热熔胶的初粘力,同时也使得其耐候性增加。
第一方面,本申请提供一种湿固化热熔胶,采用如下的技术方案:
一种湿固化热熔胶,包括如下重量份的组分:
聚酯二元醇60~100份、异氰酸酯60~100份、聚丙二醇二丙烯酸酯20~30份、马来酸酐10~15份、增粘树脂2~6份、抗氧剂1~3份、扩链剂2~5份、消泡剂0.4~0.8份、催化剂0.1~0.3份。
在一个具体的可实施方式中,所述聚酯二元醇的羟基包括芳香族聚酯二元醇或结晶性聚酯二元醇,羟值为30~50mgKOH/g。
在一个具体的可实施方式中,所述异氰酸酯包括甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、对苯二亚甲基二异氰酸酯、甲基环己基二异氰酸酯、二环己基甲烷二异氰酸酯。
在一个具体的可实施方式中,所述抗氧剂包括PUA102、PUB215、2,6-二叔丁基-4-甲基苯酚中的任意一种。
在一个具体的可实施方式中,所述扩链剂包括1,4-丁二醇、1,6-己二醇、二甘醇、二乙氨基乙醇、N,N-二羟基(二异苯基)苯胺、乙二胺中的任意一种。
在一个具体的可实施方式中,所述增粘树脂包括萜烯树脂、聚醋酸乙烯酯、环氧树脂、松香甘油酯中的任意一种。
在一个具体的可实施方式中,消泡剂包括矿物油、聚醚、聚二甲基硅氧烷、有机硅消泡剂中的任意一种。
在一个具体的可实施方式中,所述催化剂包括辛酸亚锡、叔丁醇锡、DMDEE、甲基丙烯酸甲酯中的任意一种。
第二方面,本申请提供一种湿固化热熔胶的制备方法,采用如下的技术方案:
一种湿固化热熔胶的制备方法,包括如下的步骤:
按重量份称取聚酯二元醇、聚丙二醇二丙烯酸酯和增粘树脂,依次加至三口反应器中,随后升温至各组分熔融,控制转速为40~60r/min,搅拌20~30min;
按重量份称取异氰酸酯,加至三口反应器中,控制转速为40~60r/min,搅拌40~60min;
按重量份称取马来酸酐,加至三口反应器中,控制温度为100~105℃、真空度为-0.1~-0.06MPa压力减压蒸馏至少2h,随后降温至70℃以下;
通入氦气平衡压力,随后按重量份称取抗氧剂、扩链剂、消泡剂、催化剂,加至三口反应器中,随后控制温度为80~90℃、真空度为-0.1~-0.06MPa反应2~3h,得到粗品产物;
氮气保护下将粗品产物置于80~90℃的烘箱中熟化7~8h,得到所述一种湿固化热熔胶。
本申请具有以下有益效果:本申请通过聚酯二元醇、聚丙二醇二丙烯酸酯、异氰酸酯和马来酸酐相互交联键合形成类四元穿插网络结构,同时优化了聚氨酯耐候性差和初粘力差的问题。
具体实施方式
以下结合实施例对本申请作进一步详细说明。
聚氨酯热熔胶领域飞速发展,新技术的更替也日新月异,本申请人通过文献的检索结合自身的研发经验得知,目前广为使用的湿固化聚氨酯热熔胶主要是依靠-NCO基作为端取代基,受热后将胶施加在被粘物和基材之间,首先冷却固化,形成一定的初粘力,随后依靠环境中的水分进行湿固化交联,此处的机理为-NCO基与含有活泼氢的组分(如水分子)反应生成-NHCONH-,随后-NHCONH-再与-NCO基反应生成含有脲基的结构,脲基结构脱水缩合反应生成缩二脲结构,从而完成交联。但是,申请人发现,这种硬化反应需要逐步完成,并且在遇到活泼氢之前,组分并不能发生明显的交联固化,与基材和被粘物之间的作用力很小,即初粘力弱;此外,虽然上述脲基脱水缩合的过程保证了聚氨酯热熔胶固化后具有良好的粘附力和内聚力,但是其与基材、被粘物之间还是主要依靠共价键、氢键和范德华力结合,主要是因为聚氨酯热熔胶分子中在胶粘界面存在众多诸如酯基等活性基团,而这些基团在紫外线、水分、氧气等作用下,可能会自身发生键合或分解,变成活性较低的基团,久而久之,胶粘界面的结合力就会减弱,甚至出现胶粘层完好地从基材/被粘物上脱落的情况,概括而言,湿固化聚氨酯热熔胶固化后,耐候性较差。
针对上述的初粘力弱的技术问题,已有部分本领域技术人员对聚氨酯热熔胶进行改性,包括添加填料(如加入纳米二氧化硅)、偶联剂改性(硅烷/钛酸酯偶联剂改性)、改良配方(如加入丙烯酸酯)等,但是鲜有同时关于初粘力和耐候性的改良出现,因此,本申请人同时针对上述两个问题,提出一种湿固化热熔胶及其制备方法。
首先,基于聚氨酯热熔胶的现有组分:聚酯/聚醚二元醇和异氰酸酯,本申请人在研究中发现,聚酯/聚醚二元醇和异氰酸酯仅能形成一种交联结构,其交联结构较为单一,这可能是初粘力较弱的原因之一。因此,本申请人通过大量实验发现,在聚氨热熔胶的制备过程中,当组分为聚酯二元醇和异氰酸酯时,若加入聚丙二醇二丙烯酸酯,与聚酯二元醇和异氰酸酯相互协同配合,加速交联网络的形成,同时聚丙二醇二丙烯酸酯也是长链结构,在于聚酯二元醇和异氰酸酯的键合之中,会穿插嵌入聚氨酯热熔胶的软段,形成三元互穿网络,从而提高聚氨酯热熔胶的初粘力;但是,仅仅加入聚丙二醇二丙烯酸酯,虽然可以起到上述作用,聚氨酯热熔胶也会因为自身软段的交联结构复杂化,而导致活性集团的数目增多,聚丙二醇二丙烯酸酯引入的活性基团主要是酯基,不同于羧基和羟基,酯基与被粘物/基材的粘接力主要依靠范德华力和氢键等作用力,难以形成键合作用,因此虽对聚氨酯热熔胶的初粘力有积极影响,但是也存在一定的缺陷,可能反而会使得聚氨酯热熔胶具有更差的耐候性。
为此,本申请人提出的方案是:在异氰酸酯、聚酯二元醇和聚丙二醇二丙烯酸酯混合均匀后,升温并于负压下加入马来酸酐,这样可以使得聚丙二醇二丙烯酸酯分子链中的酯基与马来酸酐中的双键进行DA反应,从而将马来酸酐接枝在聚丙二醇二丙烯酸酯分子链上,并达到变酯基为羟基的目的,酯基变成羟基可以增加粘接界面与被粘物和基材之间键合的可能性,也降低了其分解的几率,从而一定程度的改善了该聚氨酯热熔胶的耐候性;同理的,马来酸酐也可以和聚氨酯中原本存在的酯基发生DA反应,降低其降解的可能性。
除此之外,马来酸酐因为自身含有不饱和官能团,也可以在制备条件下穿插在三元互穿网络中,形成类似四元穿插网络结构的结构,从而进一步增加该聚氨酯热熔胶的初粘力和固化。
因此,综上所述,本申请通过聚酯二元醇、聚丙二醇二丙烯酸酯、异氰酸酯和马来酸酐,形成了类四元穿插网络结构,同时优化了聚氨酯耐候性差和初粘力差的问题。
以下结合具体的实施例来对本方案进行进一步解释。
实施例
需要说明的是,本申请旨在提出一种类四元穿插结构的湿固化热熔胶,除特别说明之外,所有上位的添加剂、聚合物均可用本领域内常见的化合物,例如:
聚酯二元醇可以用芳香族聚酯二元醇或结晶性聚酯二元醇,要求羟值需在30~50mgKOH/g;异氰酸酯可以选用常见的甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、对苯二亚甲基二异氰酸酯、甲基环己基二异氰酸酯、二环己基甲烷二异氰酸酯中的任意一种;抗氧剂可以选用市售的PUA102、PUB215、2,6-二叔丁基-4-甲基苯酚中的任意一种;扩链剂可以选用1,4-丁二醇、1,6-己二醇、二甘醇、二乙氨基乙醇、N,N-二羟基(二异苯基)苯胺、乙二胺中的任意一种;增粘树脂可以选用萜烯树脂、聚醋酸乙烯酯、环氧树脂、松香甘油酯中的任意一种;消泡剂可以选用矿物油、聚醚、聚二甲基硅氧烷、有机硅消泡剂中的任意一种;催化剂可以选用辛酸亚锡、叔丁醇锡、DMDEE、甲基丙烯酸甲酯中的任意一种。
实施例1
本实施例提供一种湿固化热熔胶,采用如下的制备方法:
S1、称取聚酯二元醇6kg、聚丙二醇二丙烯酸酯2kg、增粘树脂0.2kg,依次加至三口反应器中,随后升温至各组分熔融,控制转速为60r/min,搅拌20min;
S2、称取异氰酸酯6kg,加至三口反应器中,控制转速为60r/min,搅拌40min;
S3、称取马来酸酐1kg,加至三口反应器中,控制温度为100℃、真空度为-0.1MPa压力减压蒸馏2h,随后降温至65℃;
S4、通入氦气平衡压力,随后称取抗氧剂100g、扩链剂200g、消泡剂40g、催化剂10g,加至三口反应器中,随后控制温度为80℃、真空度为-0.1MPa反应3h,得到粗品产物;
S5、氮气保护下将粗品产物置于80℃的烘箱中熟化8h,得到一种湿固化热熔胶。
本申请实施例中,聚酯二元醇的羟值为30mgKOH/g;异氰酸酯选用甲苯二异氰酸酯;增粘树脂选用聚醋酸乙烯酯;抗氧剂选用PUB215;扩链剂选用乙二胺;消泡剂选用矿物油;催化剂选用DMDEE。
实施例2
本实施例提供一种湿固化热熔胶,采用如下的制备方法:
S1、称取聚酯二元醇8kg、聚丙二醇二丙烯酸酯2.5kg、增粘树脂0.4kg,依次加至三口反应器中,随后升温至各组分熔融,控制转速为50r/min,搅拌25min;
S2、称取异氰酸酯8kg,加至三口反应器中,控制转速为50r/min,搅拌50min;
S3、称取马来酸酐1.3kg,加至三口反应器中,控制温度为102℃、真空度为-0.08MPa压力减压蒸馏3h,随后降温至60℃;
S4、通入氦气平衡压力,随后称取抗氧剂200g、扩链剂350g、消泡剂60g、催化剂20g,加至三口反应器中,随后控制温度为85℃、真空度为-0.08MPa反应2.5h,得到粗品产物;
S5、氮气保护下将粗品产物置于85℃的烘箱中熟化7.5h,得到一种湿固化热熔胶。
本申请实施例中,聚酯二元醇的羟值为41mgKOH/g;异氰酸酯选用二苯基甲烷二异氰酸酯;增粘树脂选用环氧树脂;抗氧剂选用2,6-二叔丁基-4-甲基苯酚;扩链剂选用二甘醇:二乙氨基乙醇=2:1(重量比)组成;消泡剂选用聚二甲基硅氧烷;催化剂选用叔丁醇锡。
实施例3
本实施例提供一种湿固化热熔胶,采用如下的制备方法:
S1、称取聚酯二元醇10kg、聚丙二醇二丙烯酸酯3kg、增粘树脂0.6kg,依次加至三口反应器中,随后升温至各组分熔融,控制转速为40r/min,搅拌30min;
S2、称取异氰酸酯10kg,加至三口反应器中,控制转速为40r/min,搅拌60min;
S3、称取马来酸酐1.5kg,加至三口反应器中,控制温度为105℃、真空度为-0.06MPa压力减压蒸馏4h,随后降温至60℃;
S4、通入氦气平衡压力,随后称取抗氧剂300g、扩链剂500g、消泡剂40~80g、催化剂10~30g,加至三口反应器中,随后控制温度为90℃、真空度为-0.06MPa反应2h,得到粗品产物;
S5、氮气保护下将粗品产物置于90℃的烘箱中熟化8h,得到一种湿固化热熔胶。
本申请实施例中,聚酯二元醇的羟值为50mgKOH/g;异氰酸酯选用甲基环己基二异氰酸酯;增粘树脂选用松香甘油酯;抗氧剂选用2,6-二叔丁基-4-甲基苯酚;扩链剂选用1,6-己二醇;消泡剂选用聚醚;催化剂选用甲基丙烯酸甲酯。
实施例4
本实施例与实施例2的不同之处在于,本实施例中,异氰酸酯选用二苯基甲烷二异氰酸酯和异佛尔酮二异氰酸酯按照重量比3:1复配。
对比例1
本对比例与实施例1的区别在于,组分中缺少马来酸酐。
对比例2
本对比例与实施例1的区别在于,组分中缺少聚丙二醇二丙烯酸酯。
性能检测试验
利用实施例1~4、对比例1~2作为样本进行性能检测试验。部分样本的物理性质如表1所示;(剪切强度和拉伸强度检测时,基材和被粘物均选用AL板)
主要检测指标如下(基材和被粘物均选用PC板):
1.初粘性能:室温条件下,加热涂覆热熔胶后10min,测定其剪切强度。
2.高温高湿耐候性能:85℃@85%RH条件下,测试样品的剪切强度。
3.耐冷热冲击性能:-40℃/1h~85℃/1h,循环20次,测试样品的剪切强度。
初粘性能、高温高湿耐候性能、耐冷热冲击性能的试验结果如表2所示。
表1
表2
结合表1的检测结果可知,实施例1~4具有与市售聚氨酯热熔胶相近或更优异的性能;其中以实施例4最优,这可能是由于实施例4的配方组成以及制备步骤的参数选用更加优异。
结合表2的检测结果和现有的聚氨酯热熔胶的性能可知,实施例1~4的初粘性能、高温高湿下的耐候能力、冷热冲击下的耐受能力均有明显提高,较现有的聚氨酯热熔胶有显著的提升,具有更加优异的初粘力和耐候性,再结合对比例1和对比例2的检测结果可知,由于对比例2中缺少马来酸酐,因此虽然可以借助丙二醇二丙烯酸酯形成三元互穿网络,但是由于引入了更多的酯基,其耐候性明显变差;由于对比例2中缺少丙二醇二丙烯酸酯,因此虽然可以借助马来酸酐消解分子中的酯基,但是互穿网络的形成并不迅速,因此初粘力明显降低。
综上所述,只有同时通过聚酯二元醇、聚丙二醇二丙烯酸酯、异氰酸酯和马来酸酐相互交联键合形成类四元穿插网络结构,才能同时优化聚氨酯耐候性差和初粘力差的问题。
本具体实施例仅仅是对本申请的解释,其并不是对本申请的限制,本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改,但只要在本申请的权利要求范围内都受到专利法的保护。
Claims (9)
1.一种湿固化热熔胶,其特征在于,包括如下重量份的组分:
聚酯二元醇60~100份、异氰酸酯60~100份、聚丙二醇二丙烯酸酯20~30份、马来酸酐10~15份、增粘树脂2~6份、抗氧剂1~3份、扩链剂2~5份、消泡剂0.4~0.8份、催化剂0.1~0.3份。
2.根据权利要求1所述的一种湿固化热熔胶,其特征在于:所述聚酯二元醇的羟基包括芳香族聚酯二元醇或结晶性聚酯二元醇,羟值为30~50mgKOH/g。
3.根据权利要求1所述的一种湿固化热熔胶,其特征在于:所述异氰酸酯包括甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、对苯二亚甲基二异氰酸酯、甲基环己基二异氰酸酯、二环己基甲烷二异氰酸酯。
4.根据权利要求1所述的一种湿固化热熔胶,其特征在于:所述抗氧剂包括PUA102、PUB215、2,6-二叔丁基-4-甲基苯酚中的任意一种。
5.根据权利要求1所述的一种湿固化热熔胶,其特征在于:所述扩链剂包括1,4-丁二醇、1,6-己二醇、二甘醇、二乙氨基乙醇、N,N-二羟基(二异苯基)苯胺、乙二胺中的任意一种。
6.根据权利要求1所述的一种湿固化热熔胶,其特征在于:所述增粘树脂包括萜烯树脂、聚醋酸乙烯酯、环氧树脂、松香甘油酯中的任意一种。
7.根据权利要求1所述的一种湿固化热熔胶,其特征在于:消泡剂包括矿物油、聚醚、聚二甲基硅氧烷、有机硅消泡剂中的任意一种。
8.根据权利要求1所述的一种湿固化热熔胶,其特征在于:所述催化剂包括辛酸亚锡、叔丁醇锡、DMDEE、甲基丙烯酸甲酯中的任意一种。
9.权利要求1~8任一所述的一种湿固化热熔胶的制备方法,其特征在于,包括如下的步骤:
按重量份称取聚酯二元醇、聚丙二醇二丙烯酸酯和增粘树脂,依次加至三口反应器中,随后升温至各组分熔融,控制转速为40~60r/min,搅拌20~30min;
按重量份称取异氰酸酯,加至三口反应器中,控制转速为40~60r/min,搅拌40~60min;
按重量份称取马来酸酐,加至三口反应器中,控制温度为100~105℃、真空度为-0.1~-0.06MPa压力减压蒸馏至少2h,随后降温至70℃以下;
通入氦气平衡压力,随后按重量份称取抗氧剂、扩链剂、消泡剂、催化剂,加至三口反应器中,随后控制温度为80~90℃、真空度为-0.1~-0.06MPa反应2~3h,得到粗品产物;
氮气保护下将粗品产物置于80~90℃的烘箱中熟化7~8h,得到所述一种湿固化热熔胶。
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