CN115558457B - 一种双组分聚氨酯结构胶及其制备方法和应用 - Google Patents
一种双组分聚氨酯结构胶及其制备方法和应用 Download PDFInfo
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Abstract
本发明属于高分子材料技术领域,具体涉及一种双组分聚氨酯结构胶及其制备方法和应用。本发明的双组分聚氨酯结构胶,包括A组分和B组分,所述A组分包括如下重量份的组分:NCO封端的聚氨酯预聚体10~40份;多亚甲基多苯基多异氰酸酯0~30份;导热填料A 50~80份;除水剂A 1~4份;所述B组分包括如下重量份的组分:蓖麻油多元醇5~30份;芳香族聚醚多元醇2~20份;非卤化磷多元醇1~10份;醛酮树脂1~8份;导热填料B 50~80份;除水剂B 1~3份。本发明的结构胶选用恰当的原料以及科学的配比,得到的结构胶具有高粘结强度、高导热性能、以及低密度的特点,可应用于电池的组装。
Description
技术领域
本发明属于高分子材料技术领域,具体涉及一种双组分聚氨酯结构胶及其制备方法和应用。
背景技术
随着CTP(Cell to Pack)与刀片电池技术的应用,对胶粘剂要求和用量的提高,单个PACK包胶黏剂用量会从目前的1-2公斤呈现较高倍数的增长,单pack价值量也会从200-300元增长至400-900元。目前,用于PACK组装的胶粘剂有两大类:第一类以结构粘接为主,粘结强度及本体强度>10MPa,兼顾阻燃及一定的导热作用;第二类以导热粘接为主,目的是将电芯工作时产生的热量传导到外部的散热部件,实现热管理的部分功能作用,且兼顾结构粘接,避免发生电芯之间相对位移或机械疲劳而导致电芯的串、并联焊接线断路,或与某些部件接触造成短路。
电池包在CTP发展趋势下,由于电池厂商对导热胶需求量大,同时追求低成本,促使在粘结强度、经济成本上占优的聚氨酯导热结构胶成为主流导热用胶。目前主流聚氨酯导热结构胶采用的导热填料主要为氢氧化铝和氧化铝,莫氏硬度较高,加之填料形貌多为角形或多边形,对打胶设备的关键部件造成较严重的磨损,导致频繁的停机和检修。且导热填料的密度大,达到一定导热系数需要添加大量的导热填料,不利于车辆轻量化。因此,如何实现导电胶高粘结强度、高导热率的同时满足轻量化的要求仍是本领域亟需解决的问题。
发明内容
本发明旨在至少解决上述现有技术中存在的技术问题之一。为此,本发明提出一种双组分聚氨酯结构胶,具有低密度、高导热率、高强度的优势。
本发明还提出上述双组分聚氨酯结构胶的制备方法和应用。
本发明的第一方面,提出一种双组分聚氨酯结构胶,包括A组分和B组分,所述A组分包括如下重量份的组分:
所述B组分包括如下重量份的组分:
根据本发明的第一方面,至少具有如下的有益效果:
本发明采用的蓖麻油多元醇燃点高、稳定性好,能够改善结构胶的阻燃性能;芳香族聚醚多元醇中苯环具有耐湿热型,改善结构胶的耐老化性能;非卤化磷多元醇是含磷多元醇阻燃剂,具有阻燃效果,可以减少阻燃填料以及小分子阻燃剂的加入量,实现轻量化,且不含卤族元素,燃烧过程中无大量烟放出,环保无毒,而且非卤化磷多元醇参与固化反应,避免小分子阻燃剂在使用过程中析出。同时,醛酮树脂的加入可以增强结构胶对金属基材的粘结,提高粘结强度。本发明的结构胶选用恰当的原料和科学的配比,得到的结构胶具有高粘结强度、高导热性能、以及低密度的特点。
优选地,所述组分A包括如下重量份的组分:
优选地,所述组分A包括如下重量份的组分:
优选地,所述B组分包括如下重量份的组分:
优选地,所述B组分包括如下重量份的组分:
优选地,所述导热填料A、导热填料B独立地包括球形氧化铝、片层氧化铝中的至少一种。
优选地,所述球形氧化铝包括大粒径球形氧化铝、小粒径球形氧化铝;所述大粒径球形氧化铝的粒径为10~50μm,更优选15~40μm;所述小粒径球形氧化铝的粒径为1~10μm,更优选1~6μm。
优选地,所述片层氧化铝的当量粒径为1~50μm,更优选2~50μm。
优选地,所述导热填料A、导热填料B独立地为大粒径球形氧化铝、小粒径球形氧化铝、片层氧化铝的组合;所述大粒径球形氧化铝、小粒径球形氧化铝、片层氧化铝的质量比为5~10:1~4:1,更优选7~8:2~4:1,进一步优选7.1~8:2.3~2.7:1。在本发明中,大粒径球形氧化铝、小粒径球形氧化铝分散在导热胶中,形成初步的导热网络;片层氧化铝的加入起到桥梁的作用,搭建在不同球形颗粒之间,得到三维立体的导热网络结构,能够有效改善聚氨酯导热胶的导热性能;其中以球形氧化铝为主体,能减少对打胶设备的磨损;同时球形氧化铝和片层氧化铝成本低廉,工艺简单。
优选地,所述除水剂A、除水剂B独立地包括3A分子筛活化粉、乙烯基三甲氧基硅烷、噁唑烷除水剂中的至少一种。
优选地,所述除水剂A为3A分子筛活化粉。
优选地,所述除水剂B选自3A分子筛活化粉、乙烯基三甲氧基硅烷中的至少一种。
优选地,所述3A分子筛活化粉的pH(1%水溶液)为8~10,更优选9~10,进一步优选9.8左右。
优选地,所述3A分子筛活化粉的静态水吸附量[75% RH,(25±1)℃,24h]为25~28%,更优选26~27%,进一步优选26.65%左右。
优选地,所述3A分子筛活化粉为洛阳建龙维纳新材料股份有限公司的JLH-PU分子筛活化粉。在本发明中,3A分子筛活化粉中含有Na+、K+,通过调节Na+、K+的量,使得3A分子筛活化粉的pH为9.8。碱性条件下会促进聚氨酯的反应,本发明选用pH为9.8的3A分子筛活化粉相较于常用的分子筛活化粉(pH一般在11左右),能够有效延长施工时间。
优选地,所述NCO封端的聚氨酯预聚体的NCO质量百分比含量为15~20%,更优选17%。
优选地,所述NCO封端的聚氨酯预聚体由聚碳酸亚丙酯二元醇和二异氰酸酯聚合得到,所述二异氰酸酯中的NCO基团与聚碳酸亚丙酯二元醇中的OH基团的摩尔比为2~6:1,更优选2~5:1,进一步优选4:1左右。
优选地,制备NCO封端的聚氨酯预聚体的二异氰酸酯包括二苯基甲烷二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯中的至少一种。
优选地,所述多亚甲基多苯基多异氰酸酯包括二甲苯甲烷二异氰酸酯。
优选地,蓖麻油多元醇的羟值为100~200mgKOH/g,更优选150~170mgKOH/g,进一步优选165mgKOH/g。
优选地,所述蓖麻油多元醇的分子量700~1200,更优选1000。
优选地,所述非卤化磷多元醇的羟值为100~200mgKOH/g,更优选150~200mgKOH/g,进一步优选170mgKOH/g左右。
优选地,所述非卤化磷多元醇的分子量为400~700,更优选500~700,进一步优选600。
优选地,所述非卤化磷多元醇的磷质量百分比含量为15~20%,更优选16~18%。
优选地,所述非卤化磷多元醇的酸值≤5mgKOH/g,更优选酸值≤2mgKOH/g。
优选地,所述非卤化磷多元醇为科莱恩化工公司的OP 550。
优选地,所述芳香族聚醚多元醇的分子量为200~600,更优选300~400。芳香族聚醚多元醇具有良好的耐湿热、阻燃和力学性能。
优选地,所述芳香族聚醚多元醇的羟值为400~800mgKOH/g,更有选400~600mgKOH/g,进一步优选560mgKOH/g左右。
优选地,所述醛酮树脂的羟值为70~90mgKOH/g,更优选75~85mgKOH/g;所述醛酮树脂的分子量为300~500,更优选350~450。醛酮树脂对钢、铜、铝、锌等金属均有极强的附着力。
优选地,所述B组分还包括粘接促进剂、催化剂中的至少一种。
优选地,以重量份计,所述B组分还包括0~1份粘接促进剂、0.01~0.05份催化剂;更优选,所述B组分还包括0.5~0.8份粘接促进剂、0.01~0.02份催化剂。
优选地,所述粘接促进剂包括甲基三乙氧基硅烷、γ-氨丙基三乙氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷中的至少一种。
优选地,所述催化剂包括二月桂酸二正丁基锡、有机铋、有机锌中的至少一种。
优选地,所述催化剂选自有机锌、铋锌复配催化剂中的至少一种,更优选铋锌复配催化剂。相较于有机锌催化剂,铋锌复合催化剂的催化作用更温和,使用铋锌复合催化剂能够有效延长加工过程中的操作时间。
优选地,所述有机锌催化剂为广州优润合成材料有限公司的AUCAT-T62;所述铋锌复配催化剂为美国领先化学品公司的BiCAT 8。
本发明的第二方面,提出所述双组分聚氨酯结构胶的制备方法,包括如下步骤:
将A组分的各组分混合得到A组分;将B组分的各组分混合得到B组分。
优选地,所述将A组分的各组分混合得到A组分,具体为:将所述NCO封端的聚氨酯预聚体、多亚甲基多苯基多异氰酸酯、导热填料A、除水剂A,真空状态下搅拌,得到所述A组分。
优选地,所述NCO封端的聚氨酯预聚物由包括如下步骤的制备方法制备得到:
将聚碳酸亚丙酯二元醇、二异氰酸酯混合反应,得到所述NCO封端的聚氨酯预聚体。
优选地,所述NCO封端的聚氨酯预聚体为NCO双封端的聚氨酯预聚体。
优选地,所述聚碳酸亚丙酯二元醇、二异氰酸酯混合反应的温度为70~90℃,更优选75~85℃,进一步优选80℃左右;所述反应的时间为2~5h,更优选3~5h,进一步优选4h左右。
优选地,所述NCO封端的聚氨酯预聚物的制备方法还包括聚碳酸亚丙酯二元醇的预加热,所述预加热的温度为50~70℃,更优选55~65℃,进一步优选60℃左右。
优选地,所述将B组分的各组分混合得到B组分,具体为:将所述蓖麻油多元醇、芳香族聚醚多元醇、醛酮树脂、导热填料A、混合加热至110~130℃,真空状态下搅拌脱水,降温至40~60℃,加入除水剂B、粘接促进剂、催化剂,真空状态下搅拌,得到B组分。
本发明的第三方面,所述双组分聚氨酯结构胶在电池组装中的应用。
与现有技术相比,本发明至少具有如下的有益效果:
1)本发明的导热填料由两种粒径范围的球形氧化铝,以及片层氧化铝复配得到。大粒径球形氧化铝、小粒径球形氧化铝分散在导热胶中,形成初步的导热网络;片层氧化铝的加入起到桥梁的作用,搭建在不同球形颗粒之间,得到三维立体的导热网络结构,能够有效改善聚氨酯导热胶的导热性能。其中球形氧化铝为主体,能减少对打胶设备的磨损。同时球形氧化铝和片层氧化铝成本低廉,工艺简单。
2)本发明采用蓖麻油多元醇、芳香族聚醚多元醇、非卤化磷多元醇复配使用,非卤化膦多元醇是含磷阻燃剂,具有阻燃效果,能够有效减少阻燃填料的加入量,实现轻量化,且不含卤族元素,燃烧时无大量烟放出,环保无毒;蓖麻油多元醇燃点高、稳定性好,能够改善胶粘剂的阻燃性能;而且蓖麻油多元醇、非卤化磷多元醇都参与固化反应,提高交联密度,增强导热胶的强度。
3)本发明采用了醛酮树脂参与反应,大大增加了导热胶对金属的粘接性,提高粘结强度,能广泛应用于各种新能源汽车铝材上。
4)本发明采用的3A分子筛活化粉中含有Na+、K+,通过调节Na+、K+的量,使得3A分子筛活化粉的pH为8~10(如JLH-PU分子筛活化粉)。碱性条件下会促进聚氨酯的反应,本发明选用pH为8~10的3A分子筛活化粉相较于常用的分子筛活化粉(pH一般在11左右),能够有效延长施工时间。
具体实施方式
以下将结合实施例对本发明的构思及产生的技术效果进行清楚、完整地描述,以充分地理解本发明的目的、特征和效果。显然,所描述的实施例只是本发明的一部分实施例,而不是全部实施例,基于本发明的实施例,本领域的技术人员在不付出创造性劳动的前提下所获得的其他实施例,均属于本发明保护的范围。
如无特殊说明,本发明具体实施方式使用的原料为本领域常规的原料;试验/测试方法为本领域常用的方法。
实施例1~6
本实施例1~6制备了系列双组分聚氨酯结构胶,各组分的用量详见表1,具体过程为:
(1)NCO封端的聚氨酯预聚物的制备过程:
称取1000g聚碳酸亚丙酯二元醇(分子量2000)加入干燥的搅拌釜中边搅拌边升温至60℃,缓慢加入500g的二苯基甲烷二异氰酸酯(MDI),真空下以10℃为一梯度逐步升温至80℃,恒温反应4h,取样检测NCO含量,当-NCO含量达到理论值后,得到NCO封端的聚氨酯预聚体。
(2)导热胶的制备过程:
按照表1的用量,将导热填料大粒径球形氧化铝、小粒径球形氧化铝和片层氧化铝放入150℃烘箱中6小时烘干水分,然后将烘干好的导热填料、NCO封端的聚氨酯预聚体、二苯基甲烷二异氰酸酯和除水剂A加入到行星釜中,在真空状态下搅拌,得到A组分;
将蓖麻油多元醇、芳香族聚醚多元醇、非卤化磷多元醇、醛酮树脂、大粒径球形氧化铝、小粒径球形氧化铝和片层氧化铝加入到行星釜中,加热至110~130℃,并在真空状态下搅拌脱水,然后降温至40~60℃,再加入除水剂B、粘接促进剂、催化剂,在真空状态下搅拌,得到B组分。
表1实施例1~6和对比例1~4双组分聚氨酯结构胶的各组分用量(重量百分比)
大粒径球形氧化铝:粒径为15~40μm;
小粒径球形氧化铝:粒径为1~6μm;
片层氧化铝:当量粒径为3~50μm;
蓖麻油多元醇:羟值为165mgKOH/g;
芳香族聚醚多元醇:分子量为300,羟值为560mgKOH/g;
非卤化磷多元醇:分子量600,羟值为170mgKOH/g,科莱恩化工公司的OP550;
醛酮树脂:分子量350~450,羟值为75~85mgKOH/g;
3A分子筛活化粉:洛阳建龙维纳新材料股份有限公司的JLH-PU分子筛活化粉,格蕾斯贸易(上海)有限公司的SYLOSIV A3;
有机锌催化剂:广州优润合成材料有限公司的AUCAT-T62;
铋锌复配催化剂:美国领先化学品公司的BiCAT 8。
对比例1
本对比例制备了一种双组分聚氨酯结构胶,与实施例1的主要区别在于A组分、B组分中的3A分子筛活化粉JLH-PU均替换成SA-03,具体制备过程与实施例1相似。
对比例2
本对比例制备了一种双组分聚氨酯结构胶,与实施例3的主要区别在于A组分中导热填料仅使用大粒径球形氧化铝、B组分中的导热填料仅使用小粒径球形氧化铝,具体制备过程与实施例3相似。
对比例3
本对比例制备了一种双组分聚氨酯结构胶,与实施例的主要区别在于B组分不含非卤化磷多元醇,具体制备过程与实施例1相似。
对比例4
本对比例制备了一种双组分聚氨酯结构胶,与实施例的区别在于B组分中不含醛酮树脂,具体制备过程与实施例1相似。
试验例
将实施例和对比例制备的双组分聚氨酯结构胶的A组分、B组分混合固化后,测试各项性能,具体性能如表2。
表2本发明实施例1~6和对比例1~4制得的双组分聚氨酯结构胶的性能
本发明实施例1~6同时采用大粒径球形氧化铝、小粒径球形氧化铝、片层氧化铝,搭建立体的导热网络,在相同导热填料用量下,取得更优的导热效果,导热系数为1.39~1.66W/(m·K);采用蓖麻油多元醇、芳香族聚醚多元醇、非卤化磷多元醇复配,配合醛酮树脂,能够有效改善结构胶阻燃性能和粘结强度,阻燃等级均能达到V0级,剪切强度在15.3MPa;采用特定的3A分子筛活化粉JLH-PU能够有效地延长可操作时间,改善结构胶的加工性能。本发明通过科学搭配导热填料,以及特定选择的多元醇,结构胶具有高粘结强度、高阻燃性能的同时实现轻量化,结构胶的密度为1.3~1.52g/cm3。相较于实施例1,对比例1采用3A分子筛活化粉SA-03替换JLH-PU,可操作时间明显缩短,加工性能变差。相较于实施例3,对比例2改变导热填料的种类组合,结构胶的导热系数大幅下降,同时密度也有所增大。对比例3省去非卤化磷多元醇,阻燃等级仅为V1级;对比例4省去醛酮树脂,结构胶的剪切强度下降,粘结强度变差。
上面对本发明实施例作了详细说明,但是本发明不限于上述实施例,在所属技术领域普通技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下作出各种变化。此外,在不冲突的情况下,本发明的实施例及实施例中的特征可以相互组合。
Claims (7)
1.一种双组分聚氨酯结构胶,其特征在于,由A组分和B组分组成,所述A组分由如下重量份的组分组成:
所述B组分由如下重量份的组分组成:
所述导热填料A、导热填料B独立地为大粒径球形氧化铝、小粒径球形氧化铝、片层氧化铝的组合;所述大粒径球形氧化铝、小粒径球形氧化铝、片层氧化铝的质量比为5~10:1~4:1;
所述大粒径球形氧化铝的粒径为10~50μm;所述小粒径球形氧化铝的粒径为1~10μm。
2.根据权利要求1所述的双组分聚氨酯结构胶,其特征在于,所述除水剂A、除水剂B独立地包括3A分子筛活化粉、乙烯基三甲氧基硅烷、噁唑烷除水剂中的至少一种。
3.根据权利要求2所述的双组分聚氨酯结构胶,其特征在于,所述3A分子筛活化粉的pH为8~10。
4.根据权利要求1所述的双组分聚氨酯结构胶,其特征在于,所述B组分还包括粘接促进剂、催化剂中的至少一种。
5.根据权利要求4所述的双组分聚氨酯结构胶,其特征在于,所述粘接促进剂包括甲基三乙氧基硅烷、γ-氨丙基三乙氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷中的至少一种。
6.权利要求1-5任一项所述的双组分聚氨酯结构胶的制备方法,其特征在于,包括如下步骤:
将A组分的各组分混合得到A组分;将B组分的各组分混合得到B组分。
7.权利要求1-5任一项所述的双组分聚氨酯结构胶在电池组装中的应用。
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