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CN107090076A - 一种有机硅改性的水性封闭型聚异氰酸酯交联剂及其制备方法 - Google Patents

一种有机硅改性的水性封闭型聚异氰酸酯交联剂及其制备方法 Download PDF

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CN107090076A
CN107090076A CN201710452064.9A CN201710452064A CN107090076A CN 107090076 A CN107090076 A CN 107090076A CN 201710452064 A CN201710452064 A CN 201710452064A CN 107090076 A CN107090076 A CN 107090076A
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韦军
吕剑伟
孙祥
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Yangcheng Institute of Technology
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Abstract

本发明公开了一种有机硅改性的水性封闭型聚异氰酸酯交联剂及其制备方法。该交联剂通过异氰酸酯三聚体与离子型亲水扩链剂和聚乙二醇反应形成带有支化结构的水性聚氨酯预聚体，随后预聚体与羟烷基封端的聚二甲基硅氧烷反应，在链段上引入Si‑O‑Si结构，接着以封闭剂对残余的活性异氰酸酯基团进行封闭，最后以有机碱来中和骨架结构上的离子基团，得到一种有机硅改性的水性封闭型聚异氰酸酯交联剂。本发明交联剂固化涂层耐水性及耐污性增强，手感滑爽，且机械强度高，在皮革、纸张、纺织、木器等领域有较高的应用价值。

Description

一种有机硅改性的水性封闭型聚异氰酸酯交联剂及其制备 方法
技术领域
本发明属于高分子材料制备技术领域，具体涉及一种有机硅改性的水性封闭型聚异氰酸酯交联剂及其制备方法。
背景技术
异氰酸酯的研究始于20世纪40年代，德国的Bayer和Petersen等(Saunders J.H,et al.Polyurethanes Part 2[M].John Wiley&Sons,Inc.1964)首先成功研究出了异氰酸酯的封闭技术。1943年德国化学家Schlack P第一次成功制备出聚氨酯乳液，从此聚氨酯的发展迈入了新台阶，1944年德国开始步入聚氨酯工业时代，1950年美国、英国相继步入工业化， 1965中国开始生产聚氨酯。经过七十多年的发展，封闭型聚异氰酸酯被广泛应用于如皮革、塑料、纸张、橡胶和纺织等各个行业中。进入21世纪，随着应用的不断拓宽，环保局势的日益严峻，人们对于封闭性异氰酸酯的研究有了更深的认识。水性封闭异氰酸酯交联剂迎来了规模发展的黄金时代。
水性封闭型聚异氰酸酯交联剂具有耐磨性好、强度高等优点，但是其存在耐水性、耐候性差等缺点。有机硅这种特殊结构使其具有柔性好、表面张力低、化学稳定性好等优点(Watermann B T,Daehna B,Sievers S,et al.Bioassays and selected chemicalanalysis of biocide- free antifouling coatings[J].Chemosphere,2005,60:1530-1541)。在交联剂分子链段上引入有机硅可以有效改善固化涂层的性能缺陷。
发明内容
针对现有技术的不足，本发明的目的在于提供一种有机硅改性的水性封闭型聚异氰酸酯交联剂及其制备方法，该交联剂机械强度高，适合用在皮革、纸张、纺织、木器等领域。
为解决现有技术问题，本发明采取的技术方案为：
一种有机硅改性的水性封闭型聚异氰酸酯交联剂，具有如下结构式：式中为或中一种，R1为或R2为R3为B为或
上述有机硅改性的水性封闭型聚异氰酸酯交联剂的制备方法，包括以下步骤：全程在氮气保护下，搅拌进行，且各组分按质量份数计称取加入反应体系，步骤1，将0.1～0.5份的二丁基二月桂酸锡，15.0～30.0份的N-甲基-2-吡咯烷酮和20.0～35.0份的异氰酸酯三聚体加入到四口烧瓶中搅拌均匀，4～8min内升温至50～80℃得组分一；步骤2，在10～25min内向组分一中先后加入1.0～4.0份的离子型亲水扩链剂、0.5～6.5份聚乙二醇和5.0～10.0份N-甲基-2-吡咯烷酮的混合溶液，调节温度至60-70℃，保温1.0-2.5h后得组分二；步骤3，在10～15min内向组分二中加入1.5～13.0份羟烷基封端的聚二甲基硅氧烷和5.0～ 10.0份N-甲基-2-吡咯烷酮的混合溶液，于60-70℃下保温反应0.5～1.5h得组分三；步骤4，向组分三中加入5.0～20.0份的封闭剂，在60～90℃保温反应3.0～4.0h后，降温至30℃时加入1.0～5.0份的三乙胺，搅拌20-60min，即可。
作为改进的是，步骤1中所述异氰酸酯为六亚甲基二异氰酸酯三聚体、甲苯二异氰酸酯三聚体或异佛尔酮二异氰酸酯三聚体。
作为改进的是，步骤2中离子型亲水扩链剂为2,2-二羟甲基丙酸或2,2-二羟甲基丁酸；聚乙二醇为聚乙二醇200、聚乙二醇400、聚乙二醇600、聚乙二醇800或聚乙二醇1000。
作为改进的是，步骤3中羟烷基封端的聚二甲基硅氧烷为羟烷基封端的聚二甲基硅氧烷400、羟烷基封端的聚二甲基硅氧烷600、羟烷基封端的聚二甲基硅氧烷800或羟烷基封端的聚二甲基硅氧烷1000。
作为改进的是，步骤4中封闭剂为3,5-二甲基吡唑、三氮唑、丁酮肟、咪唑或己内酰胺。
本发明反应方程式为：
有益效果
通过异氰酸酯三聚体与离子型亲水扩链剂和聚乙二醇反应形成带有支化结构的水性聚氨酯预聚体，随后预聚体与羟烷基封端的聚二甲基硅氧烷反应，在链段上引入Si-O-Si结构，接着以封闭剂对残余的活性异氰酸酯基团进行封闭，最后以有机碱来中和骨架结构上的离子基团，得到一种有机硅改性的水性封闭型聚异氰酸酯交联剂。在涂层固化过程中，由于硅氧烷的表面张力低，链段柔性强，硅原子自发的向涂层表面富集，有效提高水性涂料固化后的耐水性、耐污性、耐高温性能以及机械性能，因此在皮革、纺织、木器、卷钢等领域有着广泛应用。
附图说明
图1是实施例1制得的一种有机硅改性的水性封闭型聚异氰酸酯交联剂的红外光谱。
图2是实施例2制得的一种有机硅改性的水性封闭型聚异氰酸酯交联剂的红外光谱。
具体实施方式
根据下述实施例，可以更好地理解本发明。然而，本领域的技术人员容易理解，实施例所描述的内容仅用于说明本发明，而不应当也不会限制权利要求书中所详细描述的本发明。
实施例1
上述有机硅改性的水性封闭型聚异氰酸酯交联剂的制备方法，包括以下步骤：全程在氮气保护下，搅拌进行，且各组分按质量份数计称取加入反应体系，步骤1，将0.3份的二丁基二月桂酸锡，40.0份的N-甲基-2-吡咯烷酮和30.0份的六亚甲基二异氰酸酯三聚体加入到四口烧瓶中搅拌均匀，4min内升温至65℃得组分一；步骤2，在15min内向组分一中先后加入 2.8份的2,2-二羟甲基丁酸、6.4份聚乙二醇1000和10.0份N-甲基-2-吡咯烷酮的混合溶液，调节温度至65℃，保温1.5h后得组分二；步骤3，在15min内向组分二中加入6.4份羟烷基封端的聚二甲基硅氧烷1000和10.0份N-甲基-2-吡咯烷酮的混合溶液，于65℃下保温反应1.0h得组分三；步骤4，向组分三中加入15.6份的己内酰胺，在85℃保温反应4.0h后，降温至30℃时加入1.2份的三乙胺，搅拌30min，即可。
本实施例1制备的交联剂，常温贮藏时间超过6个月；固含量49.2％，NCO含量7.87％；FT-IR(KBr,cm-1)：3365(N-H)，2952(-CH3,-CH2-)，1702(C＝O)，1554(C-N)， 1105(Si-O-Si)；图1是实施例1制得的一种有机硅改性的水性封闭型聚异氰酸酯交联剂的红外光谱。
实施例2
上述有机硅改性的水性封闭型聚异氰酸酯交联剂的制备方法，包括以下步骤：全程在氮气保护下，搅拌进行，且各组分按质量份数计称取加入反应体系，步骤1，将0.4份的二丁基二月桂酸锡，30.0份的N-甲基-2-吡咯烷酮和30.0份的异佛尔酮二异氰酸酯三聚体加入到四口烧瓶中搅拌均匀，8min内升温至65℃得组分一；步骤2，在10min内向组分一中先后加入 1.3份的2,2-二羟甲基丙酸、1.0份聚乙二醇200和5.0份N-甲基-2-吡咯烷酮的混合溶液，调节温度至65℃，保温1.0h后得组分二；步骤3，在10min内向组分二中加入3.9份羟烷基封端的聚二甲基硅氧烷400和5.0份N-甲基-2-吡咯烷酮的混合溶液，于65℃下保温反应1.0h得组分三；步骤4，向组分三中加入7.1份的咪唑，在60℃保温反应3.0h后，降温至30℃时加入1.0份的三乙胺，搅拌30min，即可。
本实施例2制备的交联剂，常温贮藏时间超过6个月，固含量为51.4％，NCO含量8.43％；FT-IR(KBr,cm-1)：3336(N-H)，2935(-CH3,-CH2-)，1701(C＝O)，1548(C-N)， 1105(Si-O-Si)；图2是实施例2制得的一种有机硅改性的水性封闭型聚异氰酸酯交联剂的红外光谱。

Claims (6)

1.一种有机硅改性的水性封闭型聚异氰酸酯交联剂，其特征在于，具有如下结构式：式中为中一种，R1为R2为R3为B为
2.基于权利要求1所述的一种有机硅改性的水性封闭型聚异氰酸酯交联剂的制备方法，其特征在于，全程在氮气保护下，搅拌进行，且各组分按质量份数计称取加入反应体系：步骤1，将0.1～0.5份的二丁基二月桂酸锡，15.0～30.0份的N-甲基-2-吡咯烷酮和20.0～35.0份的异氰酸酯三聚体加入到四口烧瓶中搅拌均匀，4～8min内升温至50～80℃得组分一；步骤2，在10～25min内向组分一中先后加入1.0～4.0份的离子型亲水扩链剂、0.5～6.5份聚乙二醇和5.0～10.0份N-甲基-2-吡咯烷酮的混合溶液，调节温度至60-70℃，保温1.0-2.5h后得组分二；步骤3，在10-15min内向组分二中加入1.5～13.0份羟烷基封端的聚二甲基硅氧烷和5.0～10.0份N-甲基-2-吡咯烷酮的混合溶液，于60-70℃下保温反应0.5～1.5h得组分三；步骤4，向组分三中加入5.0～20.0份的封闭剂，在60～90℃保温反应3.0～4.0h后，降温至30℃时加入1.0～5.0份的三乙胺，搅拌20-60min，即可。
3.根据权利要求2所述的一种有机硅改性的水性封闭型聚异氰酸酯交联剂的制备方法，其特征在于，步骤1中所述异氰酸酯为六亚甲基二异氰酸酯三聚体、甲苯二异氰酸酯三聚体或异佛尔酮二异氰酸酯三聚体。
4.根据权利要求2所述的一种有机硅改性的水性封闭型聚异氰酸酯交联剂的制备方法，其特征在于，步骤2中离子型亲水扩链剂为2,2-二羟甲基丙酸或2,2-二羟甲基丁酸；聚乙二醇为聚乙二醇200、聚乙二醇400、聚乙二醇600、聚乙二醇800或聚乙二醇1000。
5.根据权利要求2所述的一种有机硅改性的水性封闭型聚异氰酸酯交联剂的制备方法，其特征在于，步骤3中羟烷基封端的聚二甲基硅氧烷为羟烷基封端的聚二甲基硅氧烷400、羟烷基封端的聚二甲基硅氧烷600、羟烷基封端的聚二甲基硅氧烷800或羟烷基封端的聚二甲基硅氧烷1000。
6.根据权利要求2所述的一种有机硅改性的水性封闭型聚异氰酸酯交联剂的制备方法，其特征在于，步骤4中封闭剂为3,5-二甲基吡唑、三氮唑、丁酮肟、咪唑或己内酰胺。
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