CN115141596B - 一种高强高韧聚氨酯导热结构胶及其制备方法 - Google Patents
一种高强高韧聚氨酯导热结构胶及其制备方法 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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- Adhesives Or Adhesive Processes (AREA)
Abstract
本发明公开一种高强高韧聚氨酯导热结构胶及其制备方法。通过利用多官能团聚酯多元醇、聚醚多元醇改性端异氰酸酯聚氨酯预聚物、低分子量异氰酸酯这三者共同作用,可同时提高材料的强度和韧性。其中,多官能团聚酯多元醇的引入可以提高材料的化学交联密度和分子间氢键密度,有助于提高材料的强度和韧性;聚醚多元醇改性端异氰酸酯聚氨酯预聚体和低分子量异氰酸酯复配,既可以提高材料的拉伸强度和韧性,又可以保持异氰酸酯基团与基体材料的浸润性和结合速度,提高与基体界面的粘接强度。本发明的聚氨酯导热结构胶不仅具有优异的拉伸强度、韧性和粘接强度,而且具有良好的导热性能和阻燃性能,具有广阔的应用前景。
Description
技术领域
本发明属于聚氨酯结构胶散热技术领域,具体涉及一种高强高韧聚氨酯导热结构胶及其制备方法。
背景技术
聚氨酯结构胶因具有优良的强度和弹性,耐磨、耐寒、耐油等特性,在建筑、电子、交通等领域应用广泛。然而,聚氨酯本身热导率不高,仅仅只有0.1-0.3W/m·K,因此,导致其散热性能差,难以满足电气电子设备的散热需求,从而影响设备的可靠性和使用寿命。虽然填充导热填料会有效提升材料的导热性能,但通常以牺牲材料的力学强度、韧性等为代价,严重限制了其应用和发展。
由于汽车在运行过程中会发生长期震动,这不仅仅需要胶黏剂具有高的粘接强度,更重要的是具备良好的韧性,从而起到缓冲、保护电池的作用。因此对于汽车动力电池的粘接应用来说,胶黏剂不仅需要具备较高的导热性能,还需要具备高强度、高粘接、高韧性等特点。然而,目前导热结构胶研究大多集中于提高强度,而忽略了韧性(材料在塑性变形过程中吸收能量的能力)这一指标。如果材料只追求高强度,而没有适当的韧性的情况下,几乎没有实际用处。因此,提高胶黏剂的强度和韧性是至关重要的。但是,这两个属性是相互矛盾的。
中国专利CN110982485 B公开了一种高性能导热阻燃结构胶及其制备方法。虽然通过硅烷改性聚醚树脂的方法制备得到的聚氨酯灌装胶具有良好的柔韧性,但其拉伸强度低于7MPa,粘接性能低于6MPa,无法满足高强度的使用要求。因此,制备一种高强、高韧的聚氨酯导热结构胶仍具有很大的挑战。
发明内容
为了解决现有技术问题,本发明提供了一种高强高韧聚氨酯导热结构胶及其制备方法,所得聚氨酯导热结构胶不仅能够导热、阻燃,而且具备高强度、高粘接与高韧性,力学性能优异。
一种高强高韧聚氨酯导热结构胶,由A组分、B组分组成,按照重量份数计,A组分包括以下成分:
生物基多元醇10-70份;
聚酯二元醇5-50份;
多官能度聚酯多元醇2-20份;
扩链剂2-30份;
导热填料50-400份;
阻燃填料5-100份;
抗氧剂1-10份;
硅烷偶联剂3-15份;
分子筛5-20份;
B组分包括以下成分:
低分子量异氰酸酯3-50份,
端异氰酸酯预聚物10-70份,
导热填料50-400份,
阻燃填料5-100份。
作为改进的是,所述生物基多元醇的羟值为100-300,官能度为2.5-3;所述聚酯多元醇的数均分子量为1000-3000;所述多元醇的官能度为3-4,数均分子量为500-3000。
进一步改进的是,所述生物基多元醇为蓖麻油多元醇、橄榄油多元醇、大豆油改性多元醇、菜籽油基多元醇或棕榈油多元醇的一种或多种混合而成。
进一步改进的是,所述聚酯二元醇为聚碳酸酯二醇、聚己内酯二元醇、聚己二酸乙二醇酯二醇、聚己二酸缩二乙二醇酯二醇、聚己二酸新戊醇酯二醇、或聚己二酸1,4-丁二醇中的一种或多种混合而成。
进一步改进的是,所述多官能度聚酯多元醇为聚碳酸酯三元醇、聚己内酯三元醇、聚己内酯四元醇的一种或多种混合而成。
进一步改进的是,所述扩链剂为乙二醇、丙二醇、丙三醇、丁二醇、一缩二乙二醇、二甘醇、新戊二醇、二亚甲基苯基二醇的一种或多种混合而成;所述导热填料为氧化铝、氧化镁、氧化锌、氮化硼、氮化铝中的一种或多种混合而成;所述阻燃填料为氢氧化铝、氢氧化镁、三氧化二锑、聚磷酸铵、红磷、三聚氮氨的一种或多种混合而成;所述硅烷偶联剂为3-氨丙基三羟基硅烷(KH-553)、γ-甲基丙烯酰氧基丙基三甲氧基硅烷(KH570)、γ-(2,3-环氧丙氧)丙基三甲氧基硅烷(KH560)、3-缩水甘油醚氧丙基三乙氧基硅烷(KH-561)、N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷(KH-792)、γ-巯丙基三乙氧基硅烷(KH-580)、γ-巯丙基三甲氧基硅烷(KH-590)、N-β-(氨乙基)-γ-氨丙基甲基二甲氧基硅烷(DL-602)、γ-异氰酸丙基三乙氧基硅烷(KH-907)、1,3,5-三(三甲氧基硅丙基)异氰脲酸酯(KH-597)或γ-氨乙基氨丙基三甲氧基硅烷(KH-792)的一种或多种混合而成。
作为改进的是,所述低分子量异氰酸酯为甲苯二异氰酸酯(TDI)、异佛尔酮二异氰酸酯(IPDI)、二苯基甲烷二异氰酸酯(MDI)、二环己基甲烷二异氰酸酯(HMDI)、六亚甲基二异氰酸酯(HDI)、赖氨酸二异氰酸酯(LDI)、液化MDI或多亚甲基多苯基多异氰酸酯的一种或多种混合而成。
作为改进的是,所述端异氰酸酯预聚物由聚醚二元醇或多元醇与异氰酸酯反应生成,异氰酸酯基(NCO)含量为10-25%。预聚物改性过程中,异氰酸酯基团与聚醚多元醇的羟基发生反应,可以引入柔性链段和提高分子量,有利于增强其韧性。若是不进行预聚改性处理,由于各类多元醇的活性不同,其羟基与异氰酸酯的反应速度存在差异,会导致最终聚氨酯的微观结构有所不同。
上述高强高韧聚氨酯导热结构胶制备方法,包括以下步骤:
步骤1,A组分的制备
(1)将生物基多元醇、聚酯二元醇、多官能度聚酯多元醇和扩链剂投于三口烧瓶中,置于油浴锅中110-120℃真空状态下,搅拌除水2-3h;
(2)将温度降至30-60℃,加入导热填料、阻燃填料、抗氧剂、硅烷偶联剂、分子筛;搅拌均匀后,真空脱泡后密封待用;
步骤2,B组分的制备,
(1)将聚醚多元醇投于三口烧瓶中,置于油浴锅中110-120℃真空状态下,搅拌脱水2-3h;
(2)将温度降至40-60℃,加入低分子量异氰酸酯,升温至70-90℃,在氮气氛围下搅拌反应2-3h,得到端异氰酸酯的聚氨酯预聚物,降温至25-50℃,加入异氰酸酯、导热填料、阻燃填料,搅拌均匀,真空脱泡后密封待用;
步骤3,将A组分、B组分按照体积比1:1,搅拌均匀固化得到聚氨酯结构胶。
有益效果:
与现有技术相比,本发明一种高强高韧聚氨酯导热结构胶及其制备方法,所得聚氨酯导热结构胶具有高强度、高韧性,以及良好的导热和阻燃性能。具有如下优势:
(1)通过添加多官能度聚酯多元醇,一方面可以提高基体的化学交联密度,有利于增强基体的内聚力,从而提高材料的力学性能。另一方面可以提高分子间氢键密度,增大能量耗散,有利于提高材料的韧性;
(2)利用聚醚多元醇优异的柔韧性,制备聚醚多元醇改性的端异氰酸酯预聚物,有助于提高材料的断裂伸长率和韧性;
(3)将端异氰酸酯预聚物与低分子量异氰酸酯复配,扩大异氰酸酯的分子量分布范围。其中,较高分子量的端异氰酸酯预聚物有利于提高材料的强度和韧性;而低分子量异氰酸酯活动能力强,易于在基体材料表面扩散浸润,有助于提高与被粘接材料的结合力,从而提高粘接强度。
附图说明
图1为材料韧性的计算方法,韧性数值为应力-应变曲线下的面积;
图2为本发明实施例1的工程应力-应变曲线;
图3为本发明实施例2的工程应力-应变曲线;
图4为本发明对比例1的工程应力-应变曲线;
图5为本发明对比例2的工程应力-应变曲线;
图6为本发明对比例3的工程应力-应变曲线;
图7为本发明实施1-2和对比例1-3的粘接强度-位移曲线。
具体实施方式
为了便于理解本发明,下面将结合具体实施例对本发明进行更全面的描述。但是,本发明可以通过不同的形式来实现,并不限于本文所描述的实施方式。相反地,提供这些实施方式的目的是使对本发明公开内容理解得更加透彻。
一种高强高韧聚氨酯导热结构胶,由A组分、B组分组成,按照重量份数计,A组分包括以下成分:
生物基多元醇10-70份;
聚酯二元醇5-50份;
多官能度聚酯多元醇2-20份;
扩链剂2-30份;
导热填料50-400份;
阻燃填料5-100份;
抗氧剂1-10份;
硅烷偶联剂3-15份;
分子筛5-20份;
B组分包括以下成分:
低分子量异氰酸酯3-50份,
端异氰酸酯预聚物10-70份,
导热填料50-400份,
阻燃填料5-100份。
作为改进的是,所述生物基多元醇的羟值为100-300,官能度为2.5-3;所述聚酯多元醇的数均分子量为1000-3000;所述多元醇的官能度为3-4,数均分子量为500-3000;
进一步改进的是,所述生物基多元醇为蓖麻油多元醇、橄榄油多元醇、大豆油改性多元醇、菜籽油基多元醇或棕榈油多元醇的一种或多种混合而成。
进一步改进的是,所述聚酯二元醇为聚碳酸酯二醇、聚己内酯二元醇、聚己二酸乙二醇酯二醇、聚己二酸缩二乙二醇酯二醇、聚己二酸新戊醇酯二醇、或聚己二酸1,4-丁二醇中的一种或多种混合而成。
进一步改进的是,所述多官能度聚酯多元醇为聚碳酸酯三元醇、聚己内酯三元醇、聚己内酯四元醇的一种或多种混合而成。
进一步改进的是,所述扩链剂为乙二醇、丙二醇、丙三醇、丁二醇、一缩二乙二醇、二甘醇、新戊二醇、二亚甲基苯基二醇的一种或多种混合而成;所述导热填料为氧化铝、氧化镁、氧化锌、氮化硼、氮化铝中的一种或多种混合而成;所述阻燃填料为氢氧化铝、氢氧化镁、三氧化二锑、聚磷酸铵、红磷、三聚氮氨的一种或多种混合而成;所述硅烷偶联剂为3-氨丙基三羟基硅烷(KH-553)、γ-甲基丙烯酰氧基丙基三甲氧基硅烷(KH570)、γ-(2,3-环氧丙氧)丙基三甲氧基硅烷(KH560)、3-缩水甘油醚氧丙基三乙氧基硅烷(KH-561)、N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷(KH-792)、γ-巯丙基三乙氧基硅烷(KH-580)、γ-巯丙基三甲氧基硅烷(KH-590)、N-β-(氨乙基)-γ-氨丙基甲基二甲氧基硅烷(DL-602)、γ-异氰酸丙基三乙氧基硅烷(KH-907)、1,3,5-三(三甲氧基硅丙基)异氰脲酸酯(KH-597)或γ-氨乙基氨丙基三甲氧基硅烷(KH-792)的一种或多种混合而成。
作为改进的是,所述低分子量异氰酸酯为甲苯二异氰酸酯(TDI)、异佛尔酮二异氰酸酯(IPDI)、二苯基甲烷二异氰酸酯(MDI)、二环己基甲烷二异氰酸酯(HMDI)、六亚甲基二异氰酸酯(HDI)、赖氨酸二异氰酸酯(LDI)、液化MDI或多亚甲基多苯基多异氰酸酯的一种或多种混合而成。
作为改进的是,所述端异氰酸酯预聚物由聚醚二元醇或多元醇与异氰酸酯反应生成,异氰酸酯基(NCO)含量为10-25%。
上述高强高韧聚氨酯导热结构胶制备方法,包括以下步骤:
步骤1,A组分的制备,
(1)将生物基多元醇、聚酯二元醇、多官能度聚酯多元醇和扩链剂投于三口烧瓶中,置于油浴锅中110-120℃真空状态下,搅拌除水2-3h;
(2)将温度降至30-60℃,加入导热填料、阻燃填料、抗氧剂、硅烷偶联剂、分子筛;搅拌均匀后,真空脱泡后密封待用;
步骤2,B组分的制备,
(1)将聚醚多元醇投于三口烧瓶中,置于油浴锅中110-120℃真空状态下,搅拌脱水2-3h;
(2)将温度降至40-60℃,加入低分子量异氰酸酯,升温至70-90℃,在氮气氛围下搅拌反应2-3h,得到端异氰酸酯的聚氨酯预聚物,降温至25-50℃,加入异氰酸酯、导热填料、阻燃填料,搅拌均匀,真空脱泡后密封待用;
步骤3,将A组分、B组分按照体积比1:1,搅拌均匀固化得到聚氨酯结构胶。
实施例1
A组分的制备步骤:
将20g蓖麻油多元醇、16g聚碳酸酯二醇、3g聚己内酯三元醇、4g丁二醇于120℃反应釜中,真空除水3h;温度降至30℃,加入150g导热填料氧化铝、15g阻燃填料氢氧化铝、5g硅烷偶联剂KH560、5g抗氧剂1010、10g 3A分子筛,搅拌均匀,得到A组分;将A组分于真空脱泡机脱泡后密封备用。
B组分的制备步骤:
称20g聚丙二醇于反应釜中,120℃真空搅拌除水3h;温度降至50℃,加入30g多亚甲基多苯基异氰酸pm200。升温至80℃,搅拌反应2h,得到端异氰酸酯预聚物。降温至30℃,加入10g液化MDI,200g导热填料氧化铝,15g阻燃填料氢氧化铝,搅拌均匀,得到B组分;将B组分于真空脱泡机脱泡后密封备用。
将A组分、B组分按照体积比1:1固化得到聚氨酯胶黏剂。
图2是实施例1的工程应力-应变曲线,实施例1的拉伸强度是10.9MPa,断裂伸长率是51.1%。根据图1所示方法,计算得出实施例1的韧性值为4.8MJ/m3。
实施例2
A组分的制备步骤:
将20g蓖麻油多元醇、16g聚己内酯二醇、3g聚己内酯三元醇、4g丙二醇于120℃反应釜中,真空除水3h;温度降至30℃,加入150g导热填料氧化铝、15g阻燃填料氢氧化铝、5g硅烷偶联剂KH560、5g抗氧剂1010、10g 3A分子筛,搅拌均匀,得到A组分;将A组分于真空脱泡机脱泡后密封备用。
B组分的制备步骤:
称20g聚丙二醇于反应釜中,120℃真空搅拌除水3h;温度降至50℃,加入30g多亚甲基多苯基异氰酸pm200。升温至80℃,搅拌反应2h,得到端异氰酸酯预聚物。降温至30℃,加入10g液化MDI,200g导热填料氧化铝,15g阻燃填料氢氧化铝,搅拌均匀,得到B组分;将B组分于真空脱泡机脱泡后密封备用。
将A组分、B组分按照体积比1:1固化得到聚氨酯胶黏剂。
图3是实施例2的工程应力-应变曲线,实施例1的拉伸强度是10.2MPa,断裂伸长率是78.8%。根据图1所示方法,计算得出实施例2的韧性值为6.5MJ/m3。
对比例1
A组分的制备步骤:
将20g蓖麻油多元醇、16g聚己内酯二醇、4g丁二醇于120℃反应釜中,真空除水3h;温度降至30℃,加入150g导热填料氧化铝、15g阻燃填料氢氧化铝、5g硅烷偶联剂KH560、5g抗氧剂1010、10g 3A分子筛,搅拌均匀,得到A组分;将A组分于真空脱泡机脱泡后密封备用。
对比例2的B组分的制备方法和实施例1相同。
将A组分、B组分按照体积比1:1固化得到聚氨酯胶黏剂。
图4是对比例1的工程应力-应变曲线,实施例1的拉伸强度是6.8MPa,断裂伸长率是90.4%。根据图1所示方法,计算对比例1的韧性为4.6MJ/m3。
对比例2
A组分的制备步骤:
将20g蓖麻油多元醇、16g聚己内酯二醇、4g丁二醇于120℃反应釜中,真空除水3h;温度降至30℃,加入150g导热填料氧化铝、15g阻燃填料氢氧化铝、5g硅烷偶联剂KH560、5g抗氧剂1010、10g 3A分子筛,搅拌均匀,得到A组分;将A组分于真空脱泡机脱泡后密封备用。
B组分的制备步骤:
将30g多亚甲基多苯基异氰酸酯pm200,10g液化MDI,140g导热填料氧化铝,10g阻燃填料氢氧化铝,搅拌均匀,得到B组分。将B组分于真空脱泡机脱泡后密封备用。
将A组分、B组分按照体积比1:1固化得到聚氨酯胶黏剂。
图5是对比例2的工程应力-应变曲线,实施例1的拉伸强度是4.3MPa,断裂伸长率是95.1%。根据图1所示方法,计算对比例2的韧性为1.5MJ/m3。
对比例3
对比例3的A组分的制备方法和对比例1相同。
B组分的制备步骤:
称20g聚丙二醇于反应釜中,120℃真空搅拌除水3h;温度降至50℃,加入30g多亚甲基多苯基异氰酸pm200。升温至80℃,搅拌反应2h,得到端异氰酸酯预聚物。降温至30℃,加入160g导热填料氧化铝,12g阻燃填料氢氧化铝,搅拌均匀,得到B组分。将B组分于真空脱泡机脱泡后密封备用。
将A组分、B组分按照体积比1:1固化得到聚氨酯胶黏剂。
图6是对比例3的工程应力-应变曲线,实施例1的拉伸强度是6.8MPa,断裂伸长率是90.4%。根据图1所示方法,计算对比例3的韧性为3.1MJ/m3。
性能测试:
将实施例1-2和对比例1-3进行各项性能测试,测试结果见表1。
体积电阻率测试:按照GB/T10064标准测试体积电阻率。
拉伸强度和断裂伸长率测试:按照ASTM D412标准测试拉伸强度和断裂伸长率。
粘接强度测试:按照ASTM D638标准测试拉伸剪切强度。
导热系数测试:按照ASTM D5470标准测试导热系数。
阻燃性能测试:按照UL-94标准测试阻燃性能。
表1实施例1-2和对比例1-3的各项性能测试结果统计表
由表1可知,制备出的实施例1和2不仅具有高导热、高粘接性能,而且具有高强度高韧性的特点。
与实施例2相比,对比例1未添加多官能度聚酯多元醇,拉伸强度和粘接强度明显降低,说明多官能度聚酯多元醇的引入可以提高材料的强度和韧性,这是由于添加多官能度聚酯多元醇不仅可以提高分子间氢键密度,增大能量耗散,有利于提高材料的韧性,而且可以提高基体的化学交联密度,有利于增强基体的内聚力。
与实施例2相比,对比例2未添加多官能度聚酯多元醇和端异氰酸酯预聚物,拉伸强度和韧性明显降低;
与实施例2相比,对比例3同时未添加多官能度聚酯多元醇和低分子量异氰酸酯,拉伸强度和粘接强度明显降低。
与对比例1相比,对比例3未添加低分子量异氰酸酯,拉伸强度和粘接强度明显降低。
因此,本发明通过添加多官能度聚酯多元醇、聚醚改性的端异氰酸酯预聚物和低分子量异氰酸酯,三者协同调控基体分子结构和作用力,能够全面提高聚氨酯结构胶的拉伸强度、韧性和粘接强度。
以上所述仅是本发明的优选实施方式,需要指出的是,这些实施例仅用于说明本发明而不用于限制本发明的范围,而且,在阅读了本发明的内容之后,本领域相关技术人员可以对本发明做出各种改动或修改,这些等价形式同样落入本申请所附权利要求书所限定的范围。
Claims (1)
1.一种高强高韧聚氨酯导热结构胶,其特征在于,包括A组分和B组分,具体制备方法,包括以下步骤:
步骤1,A组分的制备
将20g蓖麻油多元醇、16g聚己内酯二醇、3g聚己内酯三元醇、4g丙二醇于120℃反应釜中,真空除水3h;温度降至30℃,加入150g导热填料氧化铝、15g阻燃填料氢氧化铝、5g硅烷偶联剂KH560、5g抗氧剂1010、
10g 3A分子筛,搅拌均匀,得到A组分;将A组分于真空脱泡机脱泡后密封备用;
步骤2,B组分的制备,
称20g聚丙二醇于反应釜中,120℃真空搅拌除水3h;温度降至50℃,加入30g多亚甲基多苯基异氰酸酯pm200,升温至80℃,搅拌反应2h,得到端异氰酸酯预聚物;降温至30℃,加入10g液化二苯基甲烷二异氰酸酯,200g导热填料氧化铝,15g阻燃填料氢氧化铝,搅拌均匀,得到B组分;将B组分于真空脱泡机脱泡后密封备用;
步骤3,将A组分、B组分按照体积比1:1固化得到聚氨酯胶黏剂。
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