CN114045108A - 一种sis衍生物改性聚氨酯-环氧树脂水性涂料 - Google Patents
一种sis衍生物改性聚氨酯-环氧树脂水性涂料 Download PDFInfo
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Abstract
本发明涉及一种SIS衍生物改性聚氨酯‑环氧树脂水性涂料,按重量份计,其组成为:SIS衍生物改性水性聚氨酯‑环氧树脂100.0~200.0份、甲基硅酸钾2.0~4.0份、羧基纤维素钠1.0~3.0份、成膜助剂6.0~15.0份、流平剂0.4~1.0份、分散剂0.6~1.5份、消泡剂0.4~1.0份、填料15.0~60.0份、润湿剂0.5~1.3份、AMP‑95 0.5~1.5份、去离子水20.0~60.0份;本发明制备的一种SIS衍生物改性聚氨酯‑环氧树脂水性涂料,成膜后涂层表面张力低,难以被污染物覆盖;制得的SIS衍生物改性聚氨酯‑环氧树脂水性涂料无需外抗流挂剂,其具有良好的抗流挂性能,且其具有交联密度高、耐磨性好、硬度高、良好的贮存稳定性、柔韧性好以及抗冲击性好等特点。
Description
技术领域
本发明涉及一种改性聚氨酯-环氧树脂水性涂料,尤其涉一种SIS衍生物改性聚氨酯-环氧树脂水性涂料,属于水性特种涂料技术领域。
背景技术
目前,大部分涂料主要以人工合成树脂为基础的合成涂料,大部分合成涂料都含有大量有机溶剂和一定毒性的颜料以及助剂等,造成对环境的污染,危害人身体健康,因此,水性涂料以其使用安全、方便、节能、环保等优势成为环保型涂料的研发重点。
水性聚氨酯涂料是以水性聚氨酯树脂为基料并以水为分散介质的一类涂料,不仅具有无毒无臭味、无污染、不易燃烧、不易损伤被涂饰表面、施工容易、易于清理等优点,其还具有良好耐磨性,但由于其防腐蚀性能、力学性能弱、抗流挂性能等不足之处,限制了水性聚氨酯的应用范围及进一步发展。所以通过对其改性,来增强水性聚氨酯的综合性能就非常关键。环氧树脂涂料具有力学性能好,耐热性能强、耐溶剂、耐腐蚀性能优良等性能。通过环氧树脂改性的水性聚氨酯兼具环氧树脂和聚氨酯的优异性能,具有广泛的应用前景,但只用环氧树脂改性的水性聚氨酯,虽然能提高其综合性能,但其抗流挂性以及柔韧性难以满足要求。
中国专利CN112745756A公开了一种环氧树脂改性聚氨酯防水涂料的制备方法,包括基团定量、环氧改性、粘度调节和减压提取;本发明通过设置在滴定器中的电位仪对制备原料中的异氰酸酯基浓度进行测量,监测取样液在测量试剂作用下离子浓度数量级变化产生的电位跃迁,替代对测量试剂的滴定计算过程,获取异氰酸酯基的浓度数据,从而提升了环氧树脂改性聚氨酯防水涂料的制备效果。
中国专利CN108707414A公开一种环氧树脂改性聚氨酯防水涂料及其制备方法,包括以下重量份组分:聚醚二元醇80~100份、异佛尔酮二异氰酸酯20~40份、环氧树脂30~50份、端羟基聚二甲基硅氧烷2~6份、氯铂酸0.04~0.2份、硅烷偶联剂0.6~1份、二羟甲基丙酸2~6份、丙酮15~25份、三乙胺4~10份、二月桂酸二丁基锡0.02~0.5份、水5~10份、无机填料30~60份。其制备方法如下:S1:改性环氧树脂;S2:在65-75℃氮气保护下,进行聚醚二元醇的亲核加成反应;S3:70℃下,将S1、S2的反应产物和二羟甲基丙酸共聚;S4:中和、匀质。本发明利用聚二甲基硅氧烷、环氧树脂、聚氨酯相互交联改性,综合三者优势,提高涂膜的结构稳定性和力学性能,生产出的聚氨酯防水涂料能紧密依附于非极性基面上,防水抗渗性能优异。
上述发明均具有好的性能,但其抗流挂性以及柔韧性难以满足要求,因此开发一种聚氨酯-环氧树脂具有良好抗流挂性和柔韧性符合社会发展的需求。
发明内容
本发明采用具有良好抗流挂性以及柔韧性等性能的SIS衍生物改性水性聚氨酯-环氧树脂为成膜物质,SIS衍生物改性水性聚氨酯-环氧树脂首先合成以双键封端的聚氨酯-环氧树脂,然后加入SIS衍生物,SIS衍生物中含有双键,SIS衍生物与聚氨酯-环氧树脂通过化学键相连,从而得到SIS衍生物改性水性聚氨酯-环氧树脂,由于SIS衍生物与聚氨酯-环氧树脂通过化学键相连,结构稳定,性能优良。
在制备本发明水性涂料时,无需外抗流挂剂,其具有良好的抗流挂性能。
本发明的目的提供一种SIS衍生物改性聚氨酯-环氧树脂水性涂料。
为了解决上面所述的技术问题,本发明采取以下技术方案:本发明涉及一种SIS衍生物改性聚氨酯-环氧树脂水性涂料,按重量份计,其组成为:SIS衍生物改性水性聚氨酯-环氧树脂100.0~200.0份、甲基硅酸钾2.0~4.0份、羧基纤维素钠1.0~3.0份、成膜助剂6.0~15.0份、流平剂0.4~1.0份、分散剂0.6~1.5份、消泡剂0.4~1.0份、填料15.0~60.0份、润湿剂0.5~1.3份、AMP-950.5~1.5份、去离子水20.0~60.0份。
所述的填料为云母粉、滑石粉、透明粉、高岭土、碳酸钙、膨润土、钛白粉、纳米二氧化硅中的一种或几种的组合。
所述的成膜助剂为醇酯十二、十六碳醇酯、二丙二醇丁醚中的一种或几种的组合。
所述的一种SIS衍生物改性水性聚氨酯-环氧树脂,按重量份计,其组成为:二异氰酸酯50.0~80.0份、环氧树脂10.0~30.0份、SIS衍生物6.0~12.0份、过氧化苯甲酰0.2~0.8份、低聚物多元醇30.0~70.0份、多元醇2.0~8.0份、二羟甲基丙酸4.5~10.0份、丙烯酸羟乙酯1.5~4.0份、二月桂酸二丁基锡0.01~0.1份、丙酮15.0~60.0份、乙酸乙酯12.0~30.0份、中和剂3.0~15.0份、聚乙烯醇2.0~6.0份、去离子水180.0~350.0份;所述的SIS衍生物为甲基丙烯酸丁酯接枝SIS弹性体,其采用溶液法接枝制得。
所述的二异氰酸酯为甲苯二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、苯二亚甲基二异氰酸酯中的一种或几种的组合。
所述的低聚物多元醇为聚四氢呋喃二元醇、聚碳酸酯二元醇、聚己内酯二元醇、聚环氧乙烷多元醇、聚乙二醇中的一种或几种的组合;所述的低聚物多元醇分子量为1000~3000。
所述的多元醇为丁二醇、1,4-环己二甲醇、新戊二醇、2-丁基-2-乙基-1,3-丙二醇、2,4-二乙基-1,5-戊二醇、三羟甲基丙烷中的一种或几种的组合。
所述的中和剂为三乙胺、氨水、二甲基乙醇胺中的一种或几种的组合。
所述的环氧树脂为脱水双酚A环氧树脂。
所述的SIS衍生物改性水性聚氨酯-环氧树脂,其制备工艺如下:
a)、在滴定罐中按配方重量份,将SIS衍生物和过氧化苯甲酰溶于乙酸乙酯中,得到混合液Ⅰ;
b)、在四口反应器中,按配方重量份,依次加入低聚物多元醇、多元醇、二羟甲基丙酸,升温至110~120℃,真空下脱水2.0h;
c)、降温,缓慢加入二异氰酸酯,然后加入环氧树脂,搅拌反应0.5h,滴加配方量的二月桂酸二丁基锡,升温到80~82℃搅拌反应,然后加入丙烯酸羟乙酯,视体系粘度补充丙酮,检测,当NCO值达到规定的设计值时为止;
d)、缓慢滴加滴加上述混合液Ⅰ,滴加完毕后,保温反应1.5h,并加入适量的聚乙烯醇;
e)、继续搅拌,除去部分溶剂,降温缓慢滴加中和剂,高速搅拌分散条件下,加入计算量去离子水,再一次除溶剂,过滤,得到SIS衍生物改性水性聚氨酯-环氧树脂。
本发明所述的一种SIS衍生物改性水性聚氨酯-环氧树脂,基于申请的发明专利“一种SIS衍生物改性水性聚氨酯-环氧树脂及其制备方法”,并作了详细描述。
本发明制备的一种SIS衍生物改性聚氨酯-环氧树脂水性涂料,成膜后涂层表面张力低,难以被污染物覆盖;制得的SIS衍生物改性聚氨酯-环氧树脂水性涂料无需外抗流挂剂,其具有良好的抗流挂性能,且其具有交联密度高、耐磨性好、硬度高、良好的贮存稳定性、柔韧性好、抗冲击性好等特点。
具体实施方式
下面结合实施例对本发明的一种SIS衍生物改性聚氨酯-环氧树脂水性涂料做进一步的描述。可以理解的是,此处所描述的具体实施例仅仅用于解释相关发明,而非对该发明的限定。
实施例1
一种SIS衍生物改性水性聚氨酯-环氧树脂A,按重量份计,其组成为:甲苯二异氰酸酯50.0份、环氧树脂15.0份、SIS衍生物8.0份、过氧化苯甲酰0.5份、聚碳酸酯二元醇45.0份、丁二醇2.5份、二羟甲基丙酸6.0份、丙烯酸羟乙酯2.5份、二月桂酸二丁基锡0.06份、丙酮40.0份、乙酸乙酯16.0份、三乙胺6.5份、聚乙烯醇4.0份、去离子水250.0份。
本实施例中一种SIS衍生物改性水性聚氨酯-环氧树脂A的制备方法,包括以下步骤:
a)、在滴定罐中按配方重量份,将SIS衍生物和过氧化苯甲酰溶于乙酸乙酯中,得到混合液Ⅰ;
b)、在四口反应器中,按配方重量份,依次加入聚碳酸酯二元醇、丁二醇、二羟甲基丙酸,升温至110~120℃,真空下脱水2.0h;
c)、降温,缓慢加入甲苯二异氰酸酯,然后加入环氧树脂,搅拌反应0.5h,滴加配方量的二月桂酸二丁基锡,升温到80~82℃搅拌反应,然后加入丙烯酸羟乙酯,视体系粘度补充丙酮,检测,当NCO值达到规定的设计值时为止;
d)、缓慢滴加滴加上述混合液Ⅰ,滴加完毕后,保温反应1.5h,并加入适量的聚乙烯醇;
e)、继续搅拌,除去部分溶剂,降温缓慢滴加三乙胺,高速搅拌分散条件下,加入计算量去离子水,再一次除溶剂,过滤,得到SIS衍生物改性水性聚氨酯-环氧树脂A。
实施例2
一种SIS衍生物改性水性聚氨酯-环氧树脂B,按重量份计,其组成为:异佛尔酮二异氰酸酯70.0份、环氧树脂20.0份、SIS衍生物10.0份、过氧化苯甲酰0.7份、聚四氢呋喃二元醇60.0份、1,4-环己二甲醇4.0份、二羟甲基丙酸7.5份、丙烯酸羟乙酯3.0份、二月桂酸二丁基锡0.07份、丙酮50.0份、乙酸乙酯20.0份、氨水5.5份、聚乙烯醇5.0份、去离子水350.0份。
本实施例中一种SIS衍生物改性水性聚氨酯-环氧树脂B的制备方法,包括以下步骤:
a)、在滴定罐中按配方重量份,将SIS衍生物和过氧化苯甲酰溶于乙酸乙酯中,得到混合液Ⅰ;
b)、在四口反应器中,按配方重量份,依次加入聚四氢呋喃二元醇、1,4-环己二甲醇、二羟甲基丙酸,升温至110~120℃,真空下脱水2.0h;
c)、降温,缓慢加入异佛尔酮二异氰酸酯,然后加入环氧树脂,搅拌反应0.5h,滴加配方量的二月桂酸二丁基锡,升温到80~82℃搅拌反应,然后加入丙烯酸羟乙酯,视体系粘度补充丙酮,检测,当NCO值达到规定的设计值时为止;
d)、缓慢滴加滴加上述混合液Ⅰ,滴加完毕后,保温反应1.5h,并加入适量的聚乙烯醇;
e)、继续搅拌,除去部分溶剂,降温缓慢滴加氨水,高速搅拌分散条件下,加入计算量去离子水,再一次除溶剂,过滤,得到SIS衍生物改性水性聚氨酯-环氧树脂B。
实施例3
一种SIS衍生物改性水性聚氨酯-环氧树脂C,按重量份计,其组成为:六亚甲基二异氰酸酯60.0份、环氧树脂10.0份、SIS衍生物7.5份、过氧化苯甲酰0.5份、聚己内酯二元醇60.0份、新戊二醇6.0份、二羟甲基丙酸6.0份、丙烯酸羟乙酯3.0份、二月桂酸二丁基锡0.05份、丙酮40.0份、乙酸乙酯15.0份、二甲基乙醇胺9.5份、聚乙烯醇5.0份、去离子水300.0份。
本实施例中一种SIS衍生物改性水性聚氨酯-环氧树脂C的制备方法,包括以下步骤:
a)、在滴定罐中按配方重量份,将SIS衍生物和过氧化苯甲酰溶于乙酸乙酯中,得到混合液Ⅰ;
b)、在四口反应器中,按配方重量份,依次加入聚己内酯二元醇、新戊二醇、二羟甲基丙酸,升温至110~120℃,真空下脱水2.0h;
c)、降温,缓慢加入六亚甲基二异氰酸酯,然后加入环氧树脂,搅拌反应0.5h,滴加配方量的二月桂酸二丁基锡,升温到80~82℃搅拌反应,然后加入丙烯酸羟乙酯,视体系粘度补充丙酮,检测,当NCO值达到规定的设计值时为止;
d)、缓慢滴加滴加上述混合液Ⅰ,滴加完毕后,保温反应1.5h,并加入适量的聚乙烯醇;
e)、继续搅拌,除去部分溶剂,降温缓慢滴加二甲基乙醇胺,高速搅拌分散条件下,加入计算量去离子水,再一次除溶剂,过滤,得到SIS衍生物改性水性聚氨酯-环氧树脂C。
对比例1
一种常规改性水性聚氨酯-环氧树脂X,按重量份计,其组成为:甲苯二异氰酸酯50.0份、环氧树脂15.0份、聚碳酸酯二元醇45.0份、丁二醇2.5份、二羟甲基丙酸6.0份、丙烯酸羟乙酯2.5份、二月桂酸二丁基锡0.06份、丙酮40.0份、三乙胺6.5份、聚乙烯醇4.0份、去离子水250.0份。
本实施例中一种常规改性水性聚氨酯-环氧树脂X的制备方法,包括以下步骤:
a)、在四口反应器中,按配方重量份,依次加入聚碳酸酯二元醇、丁二醇、二羟甲基丙酸,升温至110~120℃,真空下脱水2.0h;
b)、降温,缓慢加入甲苯二异氰酸酯,然后加入环氧树脂,搅拌反应0.5h,滴加配方量的二月桂酸二丁基锡,升温到80~82℃搅拌反应,然后加入丙烯酸羟乙酯,视体系粘度补充丙酮,检测,当NCO值达到规定的设计值时为止,加入适量的聚乙烯醇;
d)、继续搅拌,除去部分溶剂,降温缓慢滴加三乙胺,高速搅拌分散条件下,加入计算量去离子水,再一次除溶剂,过滤,得到常规改性水性聚氨酯-环氧树脂X。
实施例4
一种SIS衍生物改性聚氨酯-环氧树脂水性涂料,按重量份计,其组成为:SIS衍生物改性水性聚氨酯-环氧树脂A180.0份、甲基硅酸钾3.0份、羧基纤维素钠2.0份、醇酯十二12.0份、流平剂0.7份、分散剂1.2份、消泡剂0.7份、云母粉15.0份、滑石粉15.0份、透明粉15.0份、润湿剂1.0份、AMP-95 1.0份、去离子水50.0份。
实施例5
一种SIS衍生物改性聚氨酯-环氧树脂水性涂料,按重量份计,其组成为:SIS衍生物改性水性聚氨酯-环氧树脂B 160.0份、甲基硅酸钾2.0份、羧基纤维素钠2.5份、十六碳醇酯10.0份、流平剂0.6份、分散剂1.2份、消泡剂0.8份、高岭土20.0份、碳酸钙20.0份、润湿剂0.8份、AMP-95 0.9份、去离子水48.0份。
实施例6
一种SIS衍生物改性聚氨酯-环氧树脂水性涂料,按重量份计,其组成为:SIS衍生物改性水性聚氨酯-环氧树脂C 150.0份、甲基硅酸钾4.0份、羧基纤维素钠1.5份、二丙二醇丁醚9.0份、流平剂0.8份、分散剂0.9份、消泡剂0.6份、膨润土10.0份、钛白粉20.0份、润湿剂0.7份、AMP-95 0.8份、去离子水35.0份。
对比例2
一种常规改性聚氨酯-环氧树脂水性涂料,按重量份计,其组成为:常规改性水性聚氨酯-环氧树脂X 160.0份、甲基硅酸钾3.0份、羧基纤维素钠2.0份、醇酯十二10.0份、流平剂0.7份、分散剂1.2份、消泡剂0.8份、透明粉20.0份、高岭土20.0份、润湿剂0.8份、AMP-95 1.1份、去离子水40.0份。
按照相关标准,对本发明的实施例4、实施例5、实施例6与对比例2进行检测,其检测的性能指标如表1所示。
其中,附着力:按照GB/T1720-1988的规定进行测试;
硬度:按照GB/T6739-2006色漆和清铅笔法测定漆膜硬度;
耐水性:按照GB/T1733-93的规定进行检测;
耐冲击性:按照GB/T1732-2020的规定进行检测;
抗流挂性:按照GB/T9264-2012的规定进行检测;
柔韧性:按照GB/T1731-1993的规定进行检测;
丝状腐蚀:按照丝状腐蚀(GB/T13452.4-92)的规定进行检测。
表1:涂层的性能技术指标
由表1可以看出本发明的实施例4、实施例5、实施例6的附着力、抗流挂性、耐冲击性、丝状腐蚀、贮存稳定性以及柔韧性等性能要好于对比例2的相应性能;这表明本发明制备的SIS衍生物改性聚氨酯-环氧树脂水性涂料的附着力、抗流挂性、耐冲击性、丝状腐蚀、贮存稳定性以及柔韧性等性能等性能要好于常规改性水性聚氨酯-环氧树脂的相应性能。
以上描述仅为本申请的较佳实施例以及对所运用技术原理的说明;本领域技术人员应当理解,本申请中所涉及的发明范围,并不限于上述技术特征的特定组合而成的技术方案,同时也应涵盖在不脱离所述发明构思的情况下,由上述技术特征或其等同特征进行任意组合而形成的其它技术方案。例如上述特征与本申请中公开的(但不限于)具有类似功能的技术特征进行互相替换而形成的技术方案。
Claims (4)
1.一种SIS衍生物改性聚氨酯-环氧树脂水性涂料,其特征在于:所述的SIS衍生物改性聚氨酯-环氧树脂水性涂料,按重量份计,其组成为:SIS衍生物改性水性聚氨酯-环氧树脂100.0~200.0份、甲基硅酸钾2.0~4.0份、羧基纤维素钠1.0~3.0份、成膜助剂6.0~15.0份、流平剂0.4~1.0份、分散剂0.6~1.5份、消泡剂0.4~1.0份、填料15.0~60.0份、润湿剂0.5~1.3份、AMP-95 0.5~1.5份、去离子水20.0~60.0份;
其中,所述的一种SIS衍生物改性水性聚氨酯-环氧树脂,按重量份计,其组成为:二异氰酸酯50.0~80.0份、环氧树脂10.0~30.0份、SIS衍生物6.0~12.0份、过氧化苯甲酰0.2~0.8份、低聚物多元醇30.0~70.0份、多元醇2.0~8.0份、二羟甲基丙酸4.5~10.0份、丙烯酸羟乙酯1.5~4.0份、二月桂酸二丁基锡0.01~0.1份、丙酮15.0~60.0份、乙酸乙酯12.0~30.0份、中和剂3.0~15.0份、聚乙烯醇2.0~6.0份、去离子水180.0~350.0份;所述的SIS衍生物为甲基丙烯酸丁酯接枝SIS弹性体,其采用溶液法接枝制得。
2.如权利要求1所述的一种SIS衍生物改性聚氨酯-环氧树脂水性涂料,其特征在于:所述的填料为云母粉、滑石粉、透明粉、高岭土、碳酸钙、膨润土、钛白粉、纳米二氧化硅中的一种或几种的组合。
3.如权利要求1所述的一种SIS衍生物改性聚氨酯-环氧树脂水性涂料,其特征在于:所述的成膜助剂为醇酯十二、十六碳醇酯、二丙二醇丁醚中的一种或几种的组合。
4.如权利要求1所述的一种SIS衍生物改性聚氨酯-环氧树脂水性涂料,其特征在于:所述的SIS衍生物改性水性聚氨酯-环氧树脂,其制备工艺如下:
a)、在滴定罐中按配方重量份,将SIS衍生物和过氧化苯甲酰溶于乙酸乙酯中,得到混合液Ⅰ;
b)、在四口反应器中,按配方重量份,依次加入低聚物多元醇、多元醇、二羟甲基丙酸,升温至110~120℃,真空下脱水2.0h;
c)、降温,缓慢加入二异氰酸酯,然后加入环氧树脂,搅拌反应0.5h,滴加配方量的二月桂酸二丁基锡,升温到80~82℃搅拌反应,然后加入丙烯酸羟乙酯,视体系粘度补充丙酮,检测,当NCO值达到规定的设计值时为止;
d)、缓慢滴加滴加上述混合液Ⅰ,滴加完毕后,保温反应1.5h,并加入适量的聚乙烯醇;
e)、继续搅拌,除去部分溶剂,降温缓慢滴加中和剂,高速搅拌分散条件下,加入计算量去离子水,再一次除溶剂,过滤,得到SIS衍生物改性水性聚氨酯-环氧树脂。
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