CN110684177A - 一种水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂及其制备方法 - Google Patents
一种水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂及其制备方法 Download PDFInfo
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Abstract
本发明属于紫外光固化涂料树脂技术领域,公开了一种水性紫外光固化涂料专用树脂及其制备方法。该方法包括以下步骤:先将环氧树脂、阻聚剂对羟基苯甲醚、还原剂次磷酸(其作用防止产品颜色黄变)混合均匀,加热至90℃;再将丙烯酸和催化剂三苯基膦混合均匀,将其滴加入热溶液中,再升温至115℃,保温1h,当酸值小于5mgKOH/g,可以结束反应,降温至50‑60℃,加入酸酐和阻聚剂对羟基苯甲醚,然后缓慢加热至70‑80℃,保温1h后,停止反应,得到环氧丙烯酸酯低聚物;最后加入中和剂三乙醇胺,反应1h后,再在剧烈搅拌下加水进行稀释,得到水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂稠状液体。
Description
技术领域:
本发明涉及属于水性紫外光固化涂料树脂技术领域,特别是涉及一种水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂及其制备方法。
背景技术:
近几年来,水性涂料的需求不断增加。与有机溶剂型涂料相比,水性涂料中有机挥发物较少,因此水性涂料更具环保性、安全性,应用范围更广。水性涂料按成膜物质类型主要分为水性丙烯酸涂料、水性聚氨酯涂料、水性环氧涂料等。在涂料成膜过程中,需要运用涂料的固化技术,自然固化、加热固化和辐射固化(紫外光、电子束等)是涂料固化的常用方法。紫外光固化技术具有固化速度快、不需使用溶剂、对设备要求不高。能够作为紫外光固化的树脂结构中应含有不饱和键。水性紫外光固化涂料主要分为四种类型,分别是水性不饱聚酯、水性聚氨酯丙烯酸酯、水性聚酯丙烯酸酯、水性环氧丙烯酸酯,其中水性环氧丙烯酸酯因性价比高,得到消费者的青睐,成为用量最大的水性紫外光固化涂料。
目前国内外水性紫外光固化环氧丙烯酸酯树脂,主要是以环氧树脂为原料,在其环氧基团开环引入碳碳双键,实现光固化性能之后,将环氧丙烯酸树脂侧链上的羟基与含有亲水性基团的物质进行反应,提高亲水性。含有亲水性基团的物质进主要有马来酸酐、丁二酸酐和偏苯三甲酸酐等。
目前水性紫外光固化环氧丙烯酸酯树脂技术尚未成熟,除了树脂本身水溶性存在的问题,树脂水性化还可能带来涂膜张力大、耐水性差、稳定性差等问题。通常需要进行引入有机硅、有机氟、聚氨酯、纳米材料等对树脂改性以改善水性紫外光固化环氧丙烯酸酯树脂的性能,从而提高紫外光固化涂料的固含量、降低其黏度、提高对光敏感活性。
本专利围绕如何提高环氧丙烯酸树脂水溶性开展研究工作,以环氧树脂、丙烯酸为原料,以三苯基膦为催化剂,制备环氧丙烯酸酯树脂,为提高其水溶性,选用酒石酸酐为改性剂,利用其结构中含有较多亲水基团,对环氧丙烯酸酯树脂进行改性,获得水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂产品,专利的申请对水性紫外光固化涂料的开发具有积极意义。
发明内容:
本发明的目的在于提高紫外光固化环氧丙烯酸酸酯树脂的水溶性,选用酒石酸酐为改性剂,利用酒石酸酐结构中含有较多亲水基团,对环氧丙烯酸酯树脂进行改性,获得水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂产品。
本发明所述的水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂的制备方法,其特征在于,包括以下步骤:
(1)在装有搅拌桨、恒压漏斗、球形冷凝管和温度计的250mL四口烧瓶中投入120g环氧树脂、0.389g阻聚剂对羟基苯甲醚、0.06g还原剂次磷酸(其作用防止产品颜色黄变);
(2)称取46.2g取丙烯酸,1.15g催化剂三苯基膦,将丙烯酸和催化剂三苯基膦混合溶解,搅拌均匀,将此混合溶液转入滴液漏斗;
(3)用油浴加热步骤(1)四口烧瓶中反应物至90℃时,通过步骤(2)的滴液漏斗滴加混合溶液,30min滴完,然后匀速升温至95-105℃,维持45min,再在30min内匀速升温至115℃,保温1h后,用邻苯二甲酸氢钾标定过的0.1mol/L标准KOH-乙醇溶液进行滴定,测定酸值,是否≤5mgKOH/g,当酸值小于5mgKOH/g,可以结束反应;
(4)将步骤(3)结束反应后的溶液,降温至50-60℃,加入40g酸酐和0.36g阻聚剂对羟基苯甲醚,然后缓慢加热至70-80℃,保温1h后,停止反应,得到环氧丙烯酸酯低聚物;
(5)在常温搅拌下,向步骤(4)得到的环氧丙烯酸酯低聚物中,加入7.8g中和剂三乙醇胺,反应1h后,再在剧烈搅拌下加42.2g水进行稀释,得到水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂稠状液体。
与现有水溶性紫外光固化涂料制备方法相比,本发明具有如下特点:
以丙烯酸和环氧树脂为原料,生成环氧丙烯酸酯树脂,然后用酒石酸酐对其改性,以增加环氧丙烯酸酯树脂的水溶性,最后用有机碱三乙醇胺进行中和,使产品水溶性进一步增强和稳定性进一步提高。水性紫外光固化环氧丙烯酸酯树脂的合成线见图1。
本发明方法提出的水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂制备方法简单可行,绿色环保。
涂料在材料保护领域占有重要的地位,但涂料中常常含有大量的挥发性有机物(VOC),对人们的身体健康产生较大的影响。水性环氧丙烯酸酯树脂涂料以水为溶剂成膜,具有安全、环保等优势。
紫外光固化技术与其它涂料固化技术相比,具有固化速度快,不需要特殊设备的优点。环氧丙烯酸酯树脂是一种重要紫外光固化树脂。环氧丙烯酸酯树脂虽然有生产成本低、漆膜性能优异等优点,但同时也有粘度大,涂装不易等缺陷。因此水性环氧丙烯酸酯树脂的研究与生产显得极其重要。
附图说明
图1为本发明流程图。
具体实施方式:
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。
实施例:
(1)在装有搅拌桨、恒压漏斗、球形冷凝管和温度计的250mL四口烧瓶中投入120g环氧树脂、0.389g阻聚剂对羟基苯甲醚、0.06g还原剂次磷酸(其作用防止产品颜色黄变);
(2)称取46.2g取丙烯酸,1.15g催化剂三苯基膦,将丙烯酸和催化剂三苯基膦混合溶解,搅拌均匀,将此混合溶液转入滴液漏斗;
(3)用油浴加热步骤(1)四口烧瓶中反应物至90℃时,通过步骤(2)的滴液漏斗滴加混合溶液,30min滴完,然后匀速升温至95-105℃,维持45min,再在30min内匀速升温至115℃,保温1h后,用邻苯二甲酸氢钾标定过的0.1mol/L标准KOH-乙醇溶液进行滴定,测定酸值,是否≤5mgKOH/g,当酸值小于5mgKOH/g,可以结束反应;
(4)将步骤(3)结束反应后的溶液,降温至50-60℃,加入40g酸酐和0.36g阻聚剂对羟基苯甲醚,然后缓慢加热至70-80℃,保温1h后,停止反应,得到环氧丙烯酸酯低聚物;
(5)在常温搅拌下,向步骤(4)得到的环氧丙烯酸酯低聚物中,加入7.8g中和剂三乙醇胺,反应1h后,再在剧烈搅拌下加42.2g水进行稀释,得到水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂稠状液体。
Claims (2)
1.一种水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂,其特征在于,所述水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂是在以环氧树脂、丙烯酸为原料,以三苯基膦为催化剂,制备环氧丙烯酸酯树脂,再通过酒石酸酐对环氧丙烯酸酯树脂进行改性,最后获得紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂。
2.一种权利要求1所述的紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂的制备方法,其特征在于,包括以下步骤:
(1)在装有搅拌桨、恒压漏斗、球形冷凝管和温度计的250mL四口烧瓶中投入120g环氧树脂、0.389g阻聚剂对羟基苯甲醚、0.06g还原剂次磷酸(其作用防止产品颜色黄变);
(2)称取46.2g取丙烯酸,1.15g催化剂三苯基膦,将丙烯酸和催化剂三苯基膦混合溶解,搅拌均匀,将此混合溶液转入滴液漏斗;
(3)用油浴加热步骤(1)四口烧瓶中反应物至90℃时,通过步骤(2)的滴液漏斗滴加混合溶液,30min滴完,然后匀速升温至95-105℃,维持45min,再在30min内匀速升温至115℃,保温1h后,用邻苯二甲酸氢钾标定过的0.1mol/L标准KOH-乙醇溶液进行滴定,测定酸值,是否≤5mgKOH/g,当酸值小于5mgKOH/g,可以结束反应;
(4)将步骤(3)结束反应后的溶液,降温至50-60℃,加入40g酸酐和0.36g阻聚剂对羟基苯甲醚,然后缓慢加热至70-80℃,保温1h后,停止反应,得到环氧丙烯酸酯低聚物;
(5)在常温搅拌下,向步骤(4)得到的环氧丙烯酸酯低聚物中,加入7.8g中和剂三乙醇胺,反应1h后,再在剧烈搅拌下加42.2g水进行稀释,得到水性紫外光固化涂料专用酒石酸酐改性环氧丙烯酸酸酯树脂稠状液体。
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