CN106753162A - 一种可剥离型聚氨酯压敏胶粘剂的制备方法 - Google Patents
一种可剥离型聚氨酯压敏胶粘剂的制备方法 Download PDFInfo
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- CN106753162A CN106753162A CN201611156516.0A CN201611156516A CN106753162A CN 106753162 A CN106753162 A CN 106753162A CN 201611156516 A CN201611156516 A CN 201611156516A CN 106753162 A CN106753162 A CN 106753162A
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Abstract
本发明涉及一种可剥离型聚氨酯压敏胶粘剂的制备方法，首先采用缩聚法合成一种以异氰酸酯封端的聚氨酯预聚物；采用化学改性制备一种表面带胺基活性基团的白炭黑；再将上述以异氰酸酯封端的聚氨酯预聚物、表面带胺基活性基团的白炭黑、有机溶剂混合并搅拌均匀后，加入一定量的填料、催化剂和固化剂，搅拌均匀，加热回流反应一定时间，即得一种可剥离型聚氨酯压敏胶粘剂。该方法较好地解决了现有的一些可剥离型聚氨酯压敏胶粘剂产品存在的涂层脆性大、可剥离性差、耐久性和耐候性不足、成本较高等难题。可剥离型聚氨酯压敏胶粘剂的初粘力、持粘力、成膜性、拉伸强度和可剥离性能优异，从基材上剥离后能够不留任何痕迹并可重复使用而不损失其粘合性。
Description
技术领域
本发明属于胶粘剂技术领域，具体涉及一种可剥离型聚氨酯压敏胶粘剂的制备方法。
背景技术
压敏胶粘剂是一类无需借助于溶剂或热，只需施加轻度指压，即能与被粘物牢固粘合的胶粘剂。它具有应用灵活方便，经济效益高和应用范围广等特点。随着经济和科技的发展，压敏胶正越来越广泛地应用在包装、服装、建筑、汽车、机械、电子电器、航空航天、通讯、日常生活等领域，已成为一个极其发展前景的精细化工行业。
随着经济社会的发展，对压敏胶的研究变得越来越活跃，目前，压敏胶粘剂的研究主要为以下三个方面。(1) 高性能化：随着其它高科技领域的发展，对压敏胶现有品种及应用提出了更多更新更高的性能要求，如耐高温，耐溶剂性等，高性能化已经成为压敏胶不断发展的关注热点。(2)环保化：随着世界各国对环保要求的呼声越来越高，环保法规越来越严格和完善，如何降低压敏胶溶液VOC（挥发性有机化合物）含量也就成为一个非常重要的研究课题。(3)功能化：所谓压敏胶的功能化就是指压敏胶除具有普通压敏胶的物理力学性能，如初粘性，持粘性和180º剥离强度等，还具有特殊的热、光、电、磁功能，如导热性，导电性等，这些压敏胶均属于特殊压敏胶，应用在特别场合。
近几年压敏胶的需求量一直保持较快的增长速度，高性能特种压敏胶（如聚酰亚胺类、聚氨酯类、环氧树脂类、酚醛树脂类）的发展尤其迅速，生产和销售持续大幅上升，在全球范围内成为销售额最高的压敏胶品种。但在我国，受技术上的制约，其应用远低于国际水平。随着性能的不断提高，预计该类压敏胶的增长仍将是最快的；而传统的包装带用压敏胶由于市场业已成熟和趋近饱和，增长缓慢，利润渐低。
目前我国可剥离型聚氨酯压敏胶主要还依靠进口，国内的研发还处于初期阶段。现有的一些可剥离型聚氨酯压敏胶，在成膜性、可剥离性等方面都存在明显的问题，主要表现在涂层脆性大、不耐水、可剥离性和耐候性差，还有成本较高等问题，其应用受到了很大的限制。因此，寻找一种性能优越且又成本低廉的可剥离型聚氨酯压敏胶粘剂及相关生产技术是非常重要的。
目前已公开的发明专利和公开文献仍然存在许多不足，例如可剥离型压敏胶中一般含有较大量的增塑剂和/或液态增粘树脂，这是组分虽然带来了压敏胶具有良好的可剥离性能，但是产品的耐水性、耐久性和耐候性能一般，因此寻找含较少量或无增塑剂和液态增粘树脂的可剥离压敏胶，显著提高其耐水性、耐久性、耐候性和可剥离性，成为可剥离型有机硅压敏胶的制备方法中一个技术难题；其次，现有的可剥离型压敏胶产品，其可剥离性和粘合性难以同时兼顾，很少有能多次重复使用后仍具有优良的可剥离性及足够的粘接性能，最理想的可剥离压敏胶应该是可以从基材上剥离后而不留任何痕迹并可重复使用而不损失其粘合性，甚至在重复使用后仍具有优良的可剥离性及足够的粘接性；另外，上述方法的工艺复杂、成本较高，可剥离型压敏胶的可剥离性、粘接性、耐久性和耐候性要求也不达标，难以工业化应用，为此仍需继续寻找一种综合性能优越且又成本低廉的可剥离型压敏胶粘剂及相关生产技术。
发明内容
本发明的目的在于克服现有技术存在的不足，提出一种可剥离型聚氨酯压敏胶粘剂的制备方法。
本发明的一种可剥离型聚氨酯压敏胶粘剂的制备方法，具体步骤如下：
(1) 将二异氰酸酯、聚酯多元醇、催化剂以及有机溶剂以100：（300～400）：（0.05～5）：（300～500）的重量比混合均匀，升温至50～80℃，反应2～8小时，使反应趋于完成，即得到以异氰酸酯封端的聚氨酯预聚物；
(2) 将100重量份的白碳黑和60～150重量份的γ-氨丙基三乙氧基硅烷在110～140℃下搅拌反应12～72小时，即得到表面带胺基活性基团的白炭黑；
(3) 将30～60重量份的步骤(1)得到的以异氰酸酯封端的聚氨酯预聚物、40～80重量份的羟基官能化丙烯酸酯、30～80重量份的有机溶剂和0.05～0.5重量份的催化剂，搅拌均匀，控制反应瓶内温度为70～90℃，加热回流l～5 h，降低温度至50～60℃并抽真空10～60min，停止加热和搅拌，即获得所需的压敏胶粘剂成膜物质；
(4) 称取50重量份的步骤(3)中得到的压敏胶粘剂成膜物质，5～10重量份的步骤(2)得到的表面带胺基活性基团的白炭黑，5～10重量份的填料，充分搅拌均匀后升温至110～140℃，抽真空10～30 min，经三辊研磨过滤，即可得到压敏胶粘剂；
(5) 称取100重量份的步骤（４）得到的压敏胶粘剂，加入1～5重量份的固化剂，充分搅拌均匀后涂布在聚酰亚胺膜基材上，在140～160℃温度下烘干10～60 min，即获得可剥离型聚氨酯压敏胶粘剂。
本发明中，步骤(1)中，所述的二异氰酸酯，可以是芳香族二异氰酸酯，如甲苯-2,4-二异氰酸酯、甲苯-2,6-二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、1,5-萘二异氰酸酯、乙苯二异氰酸酯、4,6-二甲苯二异氰酸酯、3,3’-二甲基联苯-4,4’-二异氰酸酯或3,3’-二甲基-4,4’-二苯基甲烷二异氰酸酯，或者脂肪族二异氰酸酯，如己二异氰酸酯、六亚甲基二异氰酸酯、环己基二异氰酸酯、4,4’-二环己基甲烷二异氰酸酯或异佛儿酮二异氰酸酯等。所述的聚酯多元醇，可以是己二酸聚酯多元醇、苯酐聚酯多元醇、聚己内酯多元醇、高分子量聚酯多元醇、带侧基的特种聚酯多元醇或聚碳酸酯二元醇等中任一种；所述的催化剂，可以是二丁基锡二月桂酸酯、辛酸亚锡、N－甲基吗啉或三亚乙基二胺中任一种；所述的有机溶剂，可以是丙酮、丁酮、二氧六环、甲苯、二甲苯、乙酸乙酯、N-甲基吡咯烷酮、N,N-二甲基甲酰胺或N,N-二甲基乙酰胺等中任一种。
本发明中，所述步骤(3)中有机溶剂选自汽油、甲苯、二甲苯、二氧六环、醋酸乙酯、醋酸丁酯或甲乙酮等中的一种或两种以上的混合物。所述步骤(3)中催化剂选自二丁基锡二月桂酸酯、辛酸亚锡、N－甲基吗啉或三亚乙基二胺中的一种或两种以上的混合物。
本发明中，所述步骤(4)中填料选自硅微粉、微粉氢氧化铝、活性碳酸钙或超细硅酸铝中的一种或两种以上的混合物。
本发明中，所述步骤(5)中固化剂选自过氧化苯甲酰、2,4-二氯过氧化苯甲酰、叔丁基过氧化氢、偶氮二异丁腈中的一种或两种以上的混合物。
本发明提出的可剥离型聚氨酯压敏胶的制备方法，该制备方法：(1)采用缩聚法合成一种以异氰酸酯封端的聚氨酯预聚物；(2)采用化学改性制备一种表面带胺基活性基团的白炭黑；(3)将上述以异氰酸酯封端的聚氨酯预聚物、表面带胺基活性基团的白炭黑、有机溶剂混合并搅拌均匀后，加入一定量的填料、催化剂和固化剂，搅拌均匀，加热回流反应一定时间，即得一种可剥离型聚氨酯压敏胶粘剂。该方法较好地解决了现有的一些可剥离型聚氨酯压敏胶粘剂产品存在的涂层脆性大、可剥离性差、耐久性和耐候性不足、成本较高等难题。
本发明的优点是：①本发明的制备方法具有简单工艺方便、产品质量高、投入产出比高、成本低廉和应用前景广泛等优点。②利用本发明制备的可剥离型聚氨酯压敏胶粘剂，不含增塑剂和液态增粘树脂，该压敏胶产品储存稳定性、成膜性、耐水性和可剥离性能优异，工业化应用前景广阔，是新一代绿色环保高性能胶粘剂产品。③与普通可剥离型聚氨酯压敏胶相比，利用本发明制备的可剥离型聚氨酯压敏胶可从基材上剥离后而不留任何痕迹并可重复使用而不损失其粘合性，甚至在重复使用后仍具有优良的可剥离性及足够的粘接性，在可剥离性、耐高温、耐久性及耐候性方面有明显的优势，可应用于医疗、汽车、包装、电器电子、建筑材料、航空航天、LCD液晶板等多个领域。
附图说明
图1是可剥离型聚氨酯压敏胶粘剂的工艺流程示意图。
具体实施方式
以下结合具体实施例对上述方案做进一步说明。应理解，这些实施例是用于说明本发明而不限于限制本发明的范围。实施例中采用的实施条件可以根据具体厂家的条件做进一步调整，未注明的实施条件通常为常规实验中的条件。
下面结合实施例详细说明本发明，应当理解，此处所描述的举例仅仅用以解释本发明，并不用于限定本发明。
实施例1
将二异氰酸酯、聚酯多元醇、催化剂以及有机溶剂以100：350：0.25：400(重量)的比例混合均匀，升高温度60℃，反应5小时，使反应趋于完成，即得以异氰酸酯封端的聚氨酯预聚物；
将100重量份的白碳黑和90重量份的γ-氨丙基三乙氧基硅烷，120℃下搅拌反应24小时，即得到表面带胺基活性基团的白炭黑；
将50重量份的上述以异氰酸酯封端的聚氨酯预聚物、50重量份的2,2’-二羟甲基丙酸、60重量份的二氧六环和0.25重量份的二丁基锡二月桂酸酯，搅拌均匀，控制反应瓶内温度为80℃，加热回流4 h，降低温度至55℃并抽真空30 min，停止加热和搅拌，即获得所需的压敏胶粘剂成膜物质；
称取50重量份的上述压敏胶粘剂成膜物质，8重量份的上述表面处理的白炭黑，8重量份的硅微粉，充分搅拌均匀后升温至130℃，抽真空15 min，经三辊研磨过滤即可得聚氨酯压敏胶粘剂。
称取100重量份的上述聚氨酯压敏胶粘剂，加入3.5重量份的过氧化苯甲酰，充分搅拌均匀后涂布在聚酰亚胺膜基材上，在150℃温度下烘干45 min，即获得一种可剥离型聚氨酯压敏胶粘剂。
实施例2
与实施例1相同，但是步骤(3) 以异氰酸酯封端的聚氨酯预聚物的用量由50变为60，步骤(3) 2,2’-二羟甲基丙酸的用量由50变为70，其他不变。
实施例3
与实施例1相同，但是步骤(3) 以异氰酸酯封端的聚氨酯预聚物的用量由50变为40，步骤(3) 2,2’-二羟甲基丙酸的用量由50变为40，其他不变。
实施例4
与实施例1相同，但是步骤(4)表面处理的白炭黑的用量由8份变为5份，其他不变。
实施例5
与实施例1相同，但是步骤(4)表面处理的白炭黑的用量由8份变为10份，其他不变。
表1为本发明的可剥离型聚氨酯压敏胶粘剂的主要性能。
表1 可剥离型聚氨酯压敏胶的主要性能
| 实施例 | 1 | 2 | 3 | 4 | 5 |
| 初粘性/(球号) | 14 | 14 | 14 | 13 | 13 |
| 持粘力（1h位移/mm） | 无明显位移 | 无明显位移 | 无明显位移 | 无明显位移 | 无明显位移 |
| 持粘力（6h位移/mm） | 无明显位移 | 无明显位移 | 无明显位移 | 0.1 | 0.2 |
| 持粘力（24h位移/mm） | 无明显位移 | 无明显位移 | 0.8 | 1.0 | 2.0 |
| 剥离强度/(N/25mm) | 5.6 | 5.1 | 4.5 | 4.4 | 4.1 |
| 拉伸强度/ MPa | 4.5 | 4.2 | 4.0 | 3.9 | 3.6 |
| 伸长率/ % | 405 | 401 | 392 | 378 | 363 |
| 粘贴15d后剥离的残胶情况 | 无残胶 | 无残胶 | 无残胶 | 无残胶 | 少量残胶 |
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人是能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所做的等效变换或修饰，都应涵盖在本发明的保护范围之内。
Claims (5)
1.一种可剥离型聚氨酯压敏胶粘剂的制备方法，其特征在于具体步骤如下：
（１）将二异氰酸酯、聚酯多元醇、催化剂以及有机溶剂以100：300～400：0.05～5：300～500的重量比混合均匀，升温至50～80℃，反应2～8小时，使反应趋于完成，即得以异氰酸酯封端的聚氨酯预聚物；
（２）将100重量份的白碳黑和60～150重量份的γ-氨丙基三乙氧基硅烷在110～140℃下搅拌反应12～72小时，即得到表面带胺基活性基团的白炭黑；
（３）将30～60重量份的步骤(1)得到的以异氰酸酯封端的聚氨酯预聚物、40～80重量份的羟基官能化丙烯酸酯、30～80重量份的有机溶剂和0.05～0.5重量份的催化剂，搅拌均匀，控制反应瓶内温度为70～90℃，加热回流l～5 h，降低温度至50～60℃并抽真空10～60min，停止加热和搅拌，即获得所需的压敏胶粘剂成膜物质；
（４）称取50重量份的步骤(3)中得到的压敏胶粘剂成膜物质，5～10重量份的步骤(2)中得到的表面表面带胺基活性基团的白炭黑，5～10重量份的填料，充分搅拌均匀后升温至110～140℃，抽真空10～30 min，经三辊研磨过滤，即可得到压敏胶粘剂；
（５）称取100重量份的步骤（４）得到的压敏胶粘剂，加入1～5重量份的固化剂，充分搅拌均匀后涂布在聚酰亚胺膜基材上，在140～160℃温度下烘干10～60 min，即获得可剥离型聚氨酯压敏胶粘剂。
2.根据权利要求1所述的一种可剥离型聚氨酯压敏胶粘剂的制备方法，其特征在于步骤(1)中所述的二异氰酸酯是芳香族二异氰酸酯或脂肪族二异氰酸酯中任一种，所述的聚酯多元醇是己二酸聚酯多元醇、苯酐聚酯多元醇、聚己内酯多元醇、高分子量聚酯多元醇、带侧基的特种聚酯多元醇或聚碳酸酯二元醇中任一种；所述的催化剂是二丁基锡二月桂酸酯、辛酸亚锡、N－甲基吗啉和三亚乙基二胺中一种；所述的有机溶剂是丙酮、丁酮、二氧六环、甲苯、二甲苯、乙酸乙酯、N-甲基吡咯烷酮、N,N-二甲基甲酰胺或N,N-二甲基乙酰胺中一种或者两种以上的混合物。
3.根据权利要求1所述的一种可剥离型聚氨酯压敏胶粘剂的制备方法，其特征在于所述步骤(3)中有机溶剂是汽油、甲苯、二甲苯、二氧六环、醋酸乙酯、醋酸丁酯或甲乙酮中的一种或两种以上的混合物，所述催化剂是二丁基锡二月桂酸酯、辛酸亚锡、N－甲基吗啉或三亚乙基二胺中的任一种。
4.根据权利要求1所述的一种可剥离型聚氨酯压敏胶粘剂的制备方法，其特征在于所述步骤(4)中填料是硅微粉、微粉氢氧化铝、活性碳酸钙或超细硅酸铝中的一种或两种以上的混合物。
5.根据权利要求1所述的一种可剥离型聚氨酯压敏胶粘剂的制备方法，其特征在于所述步骤(5)中固化剂是过氧化苯甲酰、2,4-二氯过氧化苯甲酰、叔丁基过氧化氢或偶氮二异丁腈中的一种或两种以上的混合物。
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| CN113278123B (zh) * | 2021-05-19 | 2022-08-19 | 核工业华南花都建设工程公司 | 一种用于基坑止水的聚氨酯灌浆材料及其制备方法 |
| CN116421770A (zh) * | 2023-04-14 | 2023-07-14 | 中国乐凯集团有限公司 | 医用胶黏剂组合物及医用胶贴 |
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