CN108949088A - 一种高性能双组份聚氨酯压敏胶、其制备方法及应用 - Google Patents

一种高性能双组份聚氨酯压敏胶、其制备方法及应用 Download PDF

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CN108949088A
CN108949088A CN201810530026.5A CN201810530026A CN108949088A CN 108949088 A CN108949088 A CN 108949088A CN 201810530026 A CN201810530026 A CN 201810530026A CN 108949088 A CN108949088 A CN 108949088A
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李卫东
薛伟
白永平
李晶波
殷晓芬
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Wuxi Haite New Material Research Institute Co Ltd
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Abstract

本发明公开了一种高性能双组份聚氨酯压敏胶、其制备方法及应用。本发明的高性能双组份聚氨酯压敏胶其包括(A)组分及(B)组分,所述(A)组分是由下述重量百分比的各成分制得的胶液,硬单体10~12%、软单体24~30%、扩链剂2.5~4%、有机锡催化剂0.08~0.12%、溶剂54~60%、所述(B)组分为环氧固化剂,所述(B)组分为(A)组分胶液重量的0.1%。本发明的高性能双组份聚氨酯压敏胶具备低持粘低剥离力等力学性能,且耐湿性能好。

Description

一种高性能双组份聚氨酯压敏胶、其制备方法及应用
技术领域
本发明涉及压敏胶技术领域,具体涉及一种高性能双组份聚氨酯压敏胶、其制备方法及应用。
背景技术
聚氨酯胶粘剂是分子链中含有氨基甲酸酯(-NHCOO-)或异氰酸酯基(-NCO)类的胶粘剂。由于聚氨酯胶粘剂含有化学活泼性极强的基团,因而不仅与含有活泼氢的材料如泡沫、塑料、木材、皮革、织物、纸张、陶瓷等多孔材料有极强的粘接能力,而且与金属、玻璃、橡胶等表面光洁材料也有良好的化学粘接力。此外,聚氨酯胶粘剂还具有韧性可调节、粘接工艺简便、极佳的耐低温性能等特点,成为国内外胶粘剂同仁们研究的热点,并且在国民经济中迅速得到广泛应用,是八大合成胶粘剂中的重要品种之一。
1940年德国法本公司(拜耳公司的前身)的研究人员发现异氰酸酯具有特殊的粘合性能,并将三苯基甲烷一4,4’,4”一异氰酸酯成功地用于金属与橡胶的粘接,在第二次世界大战中使用到坦克履带上。50年代以后,Bayer公司开发了Desmodur系列(二异氰酸酯和多异氰酸酯)和Desmophen系列(低分子量端轻基聚酯多元醇)商品原料,使用一定量的Desmophen和Desmophen配制成Polystal系列双组分的溶剂型聚氨酯胶粘剂Polystal系列双组分聚氨酯胶粘剂具有可低温固化,粘合强度好以及耐水、耐溶剂、耐低温等优点,是当时最好的胶粘剂,为日后聚氨酯胶粘剂工业的发展奠定了基础。
美国于第二次世界大战后开始学习德国的聚氨酯工艺,1953年引进聚氨酯胶粘剂技术,同时开发了以蓖麻油和聚醚多元醇为原料的聚氨酯胶粘剂,美国B.F.Goodrich公司也开发成功了聚酯型热塑性聚氨酯胶粘剂。1968年G00dyear公司开发了无溶剂型聚氨酯结构胶粘剂“PliogriP”,成功地用于汽车玻璃纤维增强塑料(FRP)部件的粘接。1978年又开发了单组分湿固化型聚氨酯胶粘剂,并开始在汽车工业和建筑部门应用。1984年美国市场上又出现了反应型热熔聚氨酯胶粘剂,解决了传统热熔胶粘剂耐热、耐溶剂等问题,在汽车、家用电器、书籍装订等行业得到广泛应用。日本于1954年引进德国和美国聚氨酯技术,1960年开始生产聚氨酯材料,1966年开始生产聚氨酯胶粘剂。1975年日本光洋公司开发成功“乙烯基类聚氨酯”水性胶粘剂,并于1981年投入工业化生产。目前日本聚氨酯胶粘剂的研究与生产十分活跃,并与美国、西欧一起成为聚氨酯生产、出口大国。
聚氨酯压敏胶跟丙烯酸的相比主要有三点优势1无残胶2反复揭帖3遇潮不脱落。橡胶体系压敏胶非极性,自身疏水性强,透水透气性能不好;橡胶易老化,在成型过程中添加增粘剂、抗老化剂等助剂,这些助剂容易迁移出来。丙烯酸树脂的聚合会残存部分丙烯酸酯单体,这类单体有刺激气味,而且容易造成皮肤过敏。丙烯酸压敏胶粘结力太大,拆绷带麻烦,聚氨酯压敏胶的粘合原理是靠分子间的静电力,其粘度根据要求的不同,能灵活调控。
发明内容
为解决现有技术中存在的问题,本发明提供一种高性能双组份聚氨酯压敏胶及其制备方法和应用。
本发明的高性能双组份聚氨酯压敏胶具备低持粘低剥离力等力学性能,且耐湿性能好。
具体地,本发明的高性能双组份聚氨酯压敏胶,包括(A)组分及(B)组分,所述(A)组分是由下述重量百分比的各成分制得的胶液:
硬单体10~12%、
软单体24~30%、
扩链剂2.5~4%、
有机锡催化剂0.08~0.12%、
溶剂54~60%、
所述(B)组分为环氧固化剂,所述(B)组分为(A)组分胶液重量的0.1%。
其中,所述硬单体为异佛尔酮二异氰酸酯、甲苯二异氰酸酯、六亚甲基二异氰酸酯中的一种或几种;所述软单体为聚四氢呋喃醇酯二醇、聚氧化丙烯二醇、聚碳酸酯二元醇中的一种或几种;所述扩链剂为1,4丁二醇、1,6己二醇、三羟甲基丙烷、甘油中的一种或几种;所述有机锡催化剂为二月桂酸二丁基锡、辛酸亚锡中的一种或几种;所述溶剂为乙酸乙酯、甲苯、丁酮中的一种或几种。
本发明优选提供一种压敏胶,其包括(A)组分及(B)组分,所述(A)组分是由下述重量百分比的各成分制得的胶液:
异佛尔酮二异氰酸酯7~8.5%、甲苯二异氰酸酯2.8~3%、聚四氢呋喃醇酯二醇24~26%、1,4丁二醇2.5~4%、二月桂酸二丁基锡0.08~0.12%、乙酸乙酯26~30%、甲苯26~30%;
所述(B)组分为环氧固化剂,所述(B)组分为(A)组分胶液重量的0.1%。
本发明进一步提供一种优选压敏胶,其包括(A)组分及(B)组分,所述(A)组分是由下述重量百分比的各成分制得的胶液:
异佛尔酮二异氰酸酯8.5%、甲苯二异氰酸酯3%、聚四氢呋喃醇酯二醇27%、1,4丁二醇3.4%、二月桂酸二丁基锡0.1%、乙酸乙酯29%、甲苯29%;
所述(B)组分为环氧固化剂,所述(B)组分为(A)组分胶液重量的0.1%。
本发明还提供一种如上所述的压敏胶的制备方法,其由下述步骤制得作为(A)组分的胶液:
(1)将软单体、硬单体及70~90%溶剂混匀后,加入反应瓶中,加热至60~65℃;
(2)步骤(1)得到的混合物加入有机锡催化剂,自然升温至79~80℃,水浴同步升温至79~80℃;
(3)步骤(2)得到的混合物进行保温反应,再加入扩链剂进行扩链反应;
(4)步骤(3)得到的混合物进行保温反应,再加入剩余的溶剂,降温出料。
其中,在所述步骤(2)中,升温至60℃后再加入有机锡催化剂;在所述步骤(3)中,保温反应4h后再加入扩链剂进行扩链,保温反应的反应体系温度为79~80℃;在所述步骤(4)中,保温反应4h后再加入再加入剩余的溶剂,而后开始降温。
此外本发明还提供一种如上所述的压敏胶的应用方法,其在使用时,向作为(A)组分的胶液中加入作为(B)组分的环氧固化剂后搅拌,将混合液涂布在PET膜上,厚度10um,110℃固化5min。
有益效果
与现有技术相比,本发明提供的高性能双组份聚氨酯压敏胶具有以下优点:二元醇的羟基用环氧交联剂固化,所制得的溶剂型聚氨酯压敏胶经交联剂固化后具有低剥离力等较好的力学特性,剥离力最高可达到1g/25mm,同时具有较好的耐湿性,高湿持粘可达48h无残胶满足了汽车车辆、节能建筑、电子电器、医疗卫生、高档家具等高性能、高品质产品对特种胶黏剂的较高需求,解决了许多胶黏剂粘接力过大或粘接力虽低但不耐湿的问题
具体实施方式
以下对本发明的优选实施例进行说明,应当理解,此处所描述的优选实施例仅用于说明和解释本发明,并不用于限定本发明。
本发明实施例中的原料均为市场可得品,其中环氧固化剂使用深圳市佳迪达新材料科技有限公司生产的产品,型号:L-75。
实施例1
一种压敏胶,由如下原料制成:异佛尔酮二异氰酸酯8.5g、甲苯二异氰酸酯3g、聚四氢呋喃醇酯二醇27g、1,4丁二醇3.4g、二月桂酸二丁基锡0.1g、乙酸乙酯29g、甲苯29g,环氧固化剂L-75。
制备方法包括如下步骤:
(1)将聚四氢呋喃醇酯二醇、异佛尔酮二异氰酸酯、甲苯二异氰酸酯及乙酸乙酯的70%和甲苯质量70%称好混匀后,倒入装有搅拌装置、温度计和冷凝管的烧瓶中,加热至65℃;
(2)将所有的催化剂二月桂酸二丁基锡加入反应瓶中,升温至80℃。
(3)注意观察反应现象,反应升温至80℃后,保温反应4h,后加入1,4丁二醇进行扩链反应,继续保温4h;
(4)加入溶剂剩余的甲苯、乙酸乙酯稀释,降温出料,制得胶液。
将制得胶液取一部分称重并加胶液质量的0.1%的L-75环氧固化剂后充分搅拌,然后将其用直径1.5cm的玻璃棒涂布在PET膜上,将其厚度控制在10μm,在120℃固化5min,取出后制样测试。
实施例2
一种压敏胶,由如下原料制成:异佛尔酮二异氰酸酯6.5g、六亚甲基二异氰酸酯3.5g、聚氧化丙烯二醇30g、三羟甲基丙烷2.5g、二月桂酸二丁基锡0.08g、乙酸乙酯30g、甲苯27.42g,和环氧固化剂。
制备方法包括如下步骤:
(1)将聚氧化丙烯二醇、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯及总乙酸乙酯的90%和总甲苯质量的90%称好混匀后,倒入装有搅拌装置、温度计和冷凝管的烧瓶中,加热至65℃;
(2)将催化剂二月桂酸二丁基锡加入反应瓶中,升温至80℃。
(3)注意观察反应现象,反应升温至80℃后,保温反应4h,后加入三羟甲基丙烷进行扩链反应,继续保温4h。
(4)加入剩余的甲苯、乙酸乙酯稀释,降温出料,制得胶液。
将制得胶液取一部分称重并加胶液质量的0.1%的L-75环氧固化剂后充分搅拌,然后将其用直径1.5cm的玻璃棒涂布在PET膜上,将其厚度控制在10μm,在120℃固化5min,取出后制样测试。
实施例3
一种压敏胶,由如下原料制成:异佛尔酮二异氰酸酯8g、甲苯二异氰酸酯4g、聚碳酸酯二元醇24g、1,6己二醇4g、二月桂酸二丁基锡0.12g、乙酸乙酯29.88g、甲苯30g,和环氧固化剂。
制备方法包括如下步骤:
(1)将聚碳酸酯二元醇、异佛尔酮二异氰酸酯、甲苯二异氰酸酯及总乙酸乙酯的80%和总甲苯质量80%称好混匀后,倒入装有搅拌装置、温度计和冷凝管的烧瓶中,加热至60℃;
(2)将催化剂二月桂酸二丁基锡加入反应瓶中,升温至80℃。
(3)注意观察反应现象,反应升温至80℃后,保温反应4h,后加入1,6己二醇进行扩链反应,继续保温4h。
(4)加入溶剂剩余的甲苯、乙酸乙酯稀释,降温出料,制得胶液。
将制得胶液取一部分称重并加胶液量的0.1%的L-75环氧固化剂后充分搅拌,然后将其用直径1.5cm的玻璃棒涂布在PET膜上,将其厚度控制在10μm,在120℃固化5min,取出后制样测试。
实施例4
一种压敏胶,由如下原料制成:异佛尔酮二异氰酸酯8.5g、甲苯二异氰酸酯2.8g、聚四氢呋喃醇酯二醇26g、1,4丁二醇2.58g、二月桂酸二丁基锡0.12g、乙酸乙酯30g、甲苯30g,和环氧固化剂。
制备方法包括如下步骤:
(1)将聚四氢呋喃醇酯二醇,异佛尔酮二异氰酸酯、甲苯二异氰酸酯及总乙酸乙酯的质量的70%和总甲苯质量的70%称好混匀后,倒入装有搅拌装置、温度计和冷凝管的烧瓶中,加热至65℃;
(2)将所有的催化剂二月桂酸二丁基锡加入反应瓶中,升温至80℃。
(3)注意观察反应现象,反应升温至80℃后,保温反应4h,后加入1,4丁二醇进行扩链反应,继续保温4h。
(4)加入溶剂剩余的甲苯、乙酸乙酯稀释,降温出料,制得胶液。
将制得胶液取一部分称重并加胶液质量的0.1%的L-75环氧固化剂后充分搅拌,然后将其用直径1.5cm的玻璃棒涂布在PET膜上,将其厚度控制在10μm,在120℃固化5min,取出后制样测试。
实施例5
一种压敏胶,由如下原料制成:异佛尔酮二异氰酸酯7g、甲苯二异氰酸酯3g、聚四氢呋喃醇酯二醇26g、1,4丁二醇3.92g、二月桂酸二丁基锡0.08g、乙酸乙酯30g、甲苯30g,和环氧固化剂。
制备方法包括如下步骤:
(1)将聚四氢呋喃醇酯二醇,异佛尔酮二异氰酸酯、甲苯二异氰酸酯及总乙酸乙酯的质量的80%和总甲苯质量80%甲苯称好混匀后,倒入装有搅拌装置、温度计和冷凝管的烧瓶中,加热至65℃;
(2)将所有的催化剂二月桂酸二丁基锡加入反应瓶中,升温至80℃。
(3)注意观察反应现象,反应升温至80℃后,保温反应4h,后加入1,4丁二醇进行扩链反应,继续保温4h。
(4)加入溶剂剩余的甲苯、乙酸乙酯稀释,降温出料,制得胶液。
将制得胶液取一部分称重并加胶液质量的0.1%的L-75环氧固化剂后充分搅拌,然后将其用直径1.5cm的玻璃棒涂布在PET膜上,将其厚度控制在10μm,在120℃固化5min,取出后制样测试。
对本发明实施例1-5涂布胶的PE膜进行测试,持粘力测试按照《压敏胶粘带持粘性试验方法》GBT 4851-1998;剥离力测试按照《压敏胶粘带180°剥离强度试验方法》GBT2792-1998。结果见下表。
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。

Claims (7)

1.一种高性能双组份聚氨酯压敏胶,其特征在于,包括(A)组分及(B)组分,所述(A)组分是由下述重量百分比的各成分制得的胶液:
硬单体10~12%、
软单体24~30%、
扩链剂2.5~4%、
有机锡催化剂0.08~0.12%、
溶剂54~60%、
所述(B)组分为环氧固化剂,所述(B)组分为(A)组分胶液重量的0.1%。
2.根据权利要求1所述的压敏胶,其特征在于,
所述硬单体为异佛尔酮二异氰酸酯、甲苯二异氰酸酯、六亚甲基二异氰酸酯中的一种或几种;
所述软单体为聚四氢呋喃醇酯二醇、聚氧化丙烯二醇、聚碳酸酯二元醇中的一种或几种;
所述扩链剂为1,4丁二醇、1,6己二醇、三羟甲基丙烷、甘油中的一种或几种;
所述有机锡催化剂为二月桂酸二丁基锡、辛酸亚锡中的一种或几种;
所述溶剂为乙酸乙酯、甲苯、丁酮中的一种或几种。
3.根据权利要求1或2所述的压敏胶,其特征在于,
包括(A)组分及(B)组分,所述(A)组分是由下述重量百分比的各成分制得的胶液:
异佛尔酮二异氰酸酯7~8.5%、甲苯二异氰酸酯2.8~3%、聚四氢呋喃醇酯二醇24~26%、1,4丁二醇2.5~4%、二月桂酸二丁基锡0.08~0.12%、乙酸乙酯26~30%、甲苯26~30%;
所述(B)组分为环氧固化剂,所述(B)组分为(A)组分胶液重量的0.1%。
4.根据权利要求3所述的压敏胶,其特征在于,包括(A)组分及(B)组分,所述(A)组分是由下述重量百分比的各成分制得的胶液:
异佛尔酮二异氰酸酯8.5%、甲苯二异氰酸酯3%、聚四氢呋喃醇酯二醇27%、1,4丁二醇3.4%、二月桂酸二丁基锡0.1%、乙酸乙酯29%、甲苯29%;
所述(B)组分为环氧固化剂,所述(B)组分为(A)组分胶液重量的0.1%。
5.一种如权利要求1-4中任意一项所述的压敏胶的制备方法,其特征在于,由下述步骤制得作为(A)组分的胶液:
(1)将软单体、硬单体及70~90%溶剂混匀后,加入反应瓶中,加热至60~65℃;
(2)步骤(1)得到的混合物加入有机锡催化剂,自然升温至79~80℃,水浴同步升温至79~80℃;
(3)步骤(2)得到的混合物进行保温反应,再加入扩链剂进行扩链反应;
(4)步骤(3)得到的混合物进行保温反应,再加入剩余的溶剂,降温出料。
6.根据权利要求5所述的制备方法,其特征在于,
在所述步骤(2)中,升温至60℃后再加入有机锡催化剂;
在所述步骤(3)中,保温反应4h后再加入扩链剂进行扩链,保温反应的反应体系温度为79~80℃;
在所述步骤(4)中,保温反应4h后再加入再加入剩余的溶剂,而后开始降温。
7.一种如如权利要求1-4中任意一项所述的压敏胶的应用,其特征在于,使用时,向作为(A)组分的胶液中加入作为(B)组分的环氧固化剂后搅拌,将混合液涂布在PET膜上,厚度10um,110℃固化5min。
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Application publication date: 20181207