CN112724822B - 一种uv固化高光涂料及其制备方法 - Google Patents
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Abstract
一种UV固化高光涂料,其特征在于由下述重量配比的原料制成:异氰酸酯20‑60%,扩链树脂5‑25%,交联树脂5‑20%,活性聚硅氧烷5‑15%,扩链剂0.5‑5%,交联剂0.1‑0.5%,催化剂0.02‑0.2%,羟基丙烯酸酯1‑10%,多官能丙烯酸酯单体10‑30%,光引发剂0.5‑5%,流平剂0.5‑1%,消泡剂0.1-0.2%,抗静电剂0.2‑2%,偶联剂0.5‑2%。本发明还提供上述UV固化高光涂料的一种制备方法。本发明的UV固化高光涂料用于复合转移工艺生产高光纸,纸张表面光泽度高,耐热性好,耐折性好,涂层与纸张附着力好,与模压膜有良好的剥离性,生产成本低,符合节能环保和安全卫生要求。
Description
技术领域
本发明涉及涂料组合物,具体涉及一种UV固化高光涂料及其制备方法。
背景技术
航空玻璃卡纸也叫铸涂纸,传统的加工方法是将涂有涂料的原纸,贴压在加热的,经过高度抛光具有镜面光泽的镀铬烘缸表面上,再经干燥剥离下来的加工纸。由于纸面平滑,光亮如玻璃,故也称玻璃卡纸,俗称高光纸。高光纸作为高端的包装材料广泛应用于化妆品、药品、保健品、高档烟酒等高端产品的外包装,市场需求潜力非常大。
目前国内外生产高光纸有传统的铸涂工艺和复合转移工艺。
传统的铸涂工艺存在工艺比较复杂、设备投资大、控制精度要求很高、涂层厚、生产线速低、生产成本高等缺点,而且生产出来的高光纸的光泽度、耐折性、附着力、印刷和烫金性能还存在一定的不足。
复合转移工艺是国内近几年出现的一种高光纸生产新工艺,它是将高光涂料涂布在纸上,然后与表面光滑的膜(如PET膜、OPP膜等)复合,固化后剥离回收膜,利用膜的光滑表面模压涂层而使纸张表面平滑光亮,形成高光纸。该工艺具有设备简单、容易操作、涂层薄、生产速度快的优点。目前市场上用于复合转移工艺的高光涂料主要是水性丙烯酸类,此类高光涂料生产的高光纸光泽度低、耐折性不足、耐热性差,生产线长且成本高。
发明内容
本发明所要解决的技术问题是提供一种UV固化高光涂料及其制备方法,这种UV固化高光涂料用于复合转移工艺生产高光纸,纸张表面光泽度高,耐热性好,耐折性好,涂层与纸张附着力好,与模压膜有良好的剥离性,生产成本低,符合节能环保和安全卫生要求。采用的技术方案如下:
一种UV固化高光涂料,其特征在于由下述重量配比的原料制成:异氰酸酯20-60%,扩链树脂5-25%,交联树脂5-20%,活性聚硅氧烷5-15%,扩链剂0.5-5%,交联剂0.1-0.5%,催化剂0.02-0.2%,羟基丙烯酸酯1-10%,多官能丙烯酸酯单体10-30%,光引发剂0.5-5%,流平剂0.5-1%,消泡剂0.1-0.2%,抗静电剂0.2-2%,偶联剂0.5-2%。
上述异氰酸酯作为高光涂料的硬段部分,赋予转移胶的强度、耐温性等性能。上述异氰酸酯通常采用不变黄异氰酸酯,这类异氰酸酯在紫外光照射下不变黄,有利于使高光涂料在紫外光照射下不变黄。优选方案中,上述异氰酸酯是异佛尔酮二异氰酸酯(IPDI)、4,4′-二环己基甲烷二异氰酸酯(HMDI)、甲苯二异氰酸酯、六亚甲基二异氰酸酯(HDI)和HDI三聚体中的一种或其中多种的组合。更优选异氰酸酯是4,4′-二环己基甲烷二异氰酸酯(HMDI),HMDI可以降低聚氨酯的反应速度,保证预聚体分子量一致性和规整性。
上述扩链树脂作为高光涂料的软段组分,赋予高光涂料的柔韧性。优选上述扩链树脂可以是聚醚二元胺(如聚氧化乙烯醚二胺、聚氧化丙烯醚二胺,其分子量为200-2000),聚醚二元醇(如聚氧化乙烯醚二醇、聚四氢呋喃醚二醇,其分子量为1000-4000),或聚酯二元醇(如聚碳酸酯二醇、聚己内酯二醇,其分子量为1000-4000),或聚天门冬氨酸酯(如广州齐翔Q440、珠海飞扬F520等)。聚醚如德信联邦的DDL-400、DDL-1000、DDL-220等牌号,聚酯二元醇有华峰基团的PE-3010、PE-3020、PE-3030等。更优选上述扩链树脂为聚醚二元胺,其分子量为2000。
上述交联树脂作为交联型软段组分,能够增加软段含量和交联点,提高高光涂料的强度、硬度和光泽度。优选上述交联树脂是分子量为200-1000的聚醚多元醇,如丙三醇、季戊四醇、山梨醇或蔗糖为起始剂的聚醚多元醇(如一诺威的YNW-6205、YNW-305、YNW-380等牌号)。更优选上述交联树脂是分子量为400,官能度为3.5的山梨醇聚醚多元醇。
上述活性聚硅氧烷赋予高光涂料的膜可剥离性能,并提高耐热性,减少剥离时的静电产生而损伤涂层及模压膜。优选上述活性聚硅氧烷是氨丙基封端聚二甲基硅氧烷或醇羟基封端二甲基硅氧烷,其分子量为500-4000。更优选优选上述活性聚硅氧烷是α,ω-二羟烃基聚硅氧烷,其分子量为1000。
上述扩链剂用于提高聚合物分子量及硬段含量,通常采用低分子二元醇或二元胺。优选上述扩链剂是1,4-丁二醇、新戊二醇、一缩二乙二醇、双酚A、异氟尔酮二胺、乙二胺或苯二胺。更优选上述扩链剂是二元醇或新戊二醇。
上述交联剂用于提高聚合物分子量及硬段含量。交联剂通常采用小分子多元醇。优选上述交联剂是丙三醇、季戊四醇或三羟甲基丙烷。更优选上述交联剂是三羟甲基丙烷。
上述催化剂用于催化异氰酸酯和扩链树脂、交联树脂、活性聚硅氧烷及羟基丙烯酸酯的反应。优选上述催化剂是二月桂酸二丁基锡、辛酸亚锡、异辛酸钾催化剂或铋类催化剂。更优选上述催化剂是辛酸亚锡。
上述羟基丙烯酸酯是聚氨酯和丙烯酸酯的桥接树脂,端羟基和聚氨酯预聚体的NCO反应而接入不饱和树脂。优选上述羟基丙烯酸酯是丙烯酸羟乙酯或甲基丙烯酸羟乙酯。更优选上述羟基丙烯酸酯是甲基丙烯酸羟乙酯。
上述多官能丙烯酸酯单体是活性稀释剂,课降低高光涂料体系的粘度,提高施工性能,赋予UV固化性能;并提供交联双键,赋予产品强度和耐磨性能。上述多官能丙烯酸酯单体可以是二官能团、三官能团或四官能团的丙烯酸酯,优选三官能团的丙烯酸酯。优选上述多官能丙烯酸酯单体是三丙二醇二丙烯酸酯、三羟甲基丙烷三丙烯酸酯或二季戊四醇五丙烯酸酯。
上述光引发剂是UV光引发剂,涂布施工完成后的涂层在引发剂及UV光作用下交联固化,形成良好的产品性能。上述光引发剂可以是自由基光引发剂(如二苯基乙二酮、联苯甲酰、二苯甲酮等)或阳离子光引发剂。优选上述光引发剂是二苯甲酮。
优选上述流平剂是聚醚硅氧烷共聚物,如TEGO Glide 410。
优选上述消泡剂是聚醚型消泡剂,如迪高的TEGO Foamex 805的消泡剂。
上述抗静电剂在产品涂布固化后,用于减少剥离模压膜时产生静电,提高产品质量和生产安全性。上述抗静电剂可以是阳离子抗静电剂、阴离子抗静电剂、非离子抗静电剂或高分子抗静电剂。优选上述抗静电剂是聚氨酯高分子抗静电剂(JL-WT)。
上述偶联剂能够提高涂层与纸张的附着力,提高涂层的印刷适应性。优选上述偶联剂是硅烷偶联剂KH560。
本发明采用多步法合成聚氨酯,再加入多官能丙烯酸酯单体调节粘度。首先是将扩链树脂、交联树脂在一定温度和真空度下除水,然后异氰酸酯分别与扩链树脂、交联树脂、活性聚硅氧烷、羟基丙烯酸酯、小分子扩链剂和交联剂反应,反应完成后冷却,再加入多官能丙烯酸酯单体、光引发剂、抗静电剂、流平剂、消泡剂和偶联剂,混合均匀后即可获得产品并出料,产品应密封避光保存。
本发明还提供上述UV固化高光涂料的一种制备方法,其特征在于包括下述步骤:
(1)按重量计,配备下述原料:异氰酸酯20-60%,扩链树脂5-25%,交联树脂5-20%,活性聚硅氧烷5-15%,扩链剂0.5-5%,交联剂0.1-0.5%,催化剂0.02-0.2%,羟基丙烯酸酯1-10%,多官能丙烯酸酯单体10-30%,光引发剂0.5-5%,流平剂0.5-1%,消泡剂0.1-0.2%,抗静电剂0.2-2%,偶联剂0.5-2%;
(2)将扩链树脂、交联树脂分别加入带有搅拌器及真空除水系统的除水反应釜中,除去其中所含的水分;
(3)将已除水的扩链树脂加入聚合反应釜中,然后在搅拌的情况下滴加入异氰酸酯,并加热至70-85℃,反应0.5-2小时;然后加入已除水的交联树脂,在70-85℃下反应1-4小时;
(4)将聚合反应釜中的温度调节至55-70℃,再加入活性聚硅氧烷,在65-70℃下反应0.5-3小时;
(5)将聚合反应釜中的温度调节至55-70℃,再加入羟基丙烯酸酯和催化剂,加热至70-80℃,反应0.5-3小时;
(6)将聚合反应釜中的温度调节至55-70℃,再加入扩链剂和交联剂,升温至70-80℃,反应1-4小时;
(7)将聚合反应釜中的温度调节至50-70℃,再加入多官能丙烯酸酯单体、光引发剂、抗静电剂、流平剂、消泡剂和偶联剂,搅拌20-60分钟,得到UV固化高光涂料。
优选步骤(2)中,将扩链树脂、交联树脂分别加入带有搅拌器及真空除水系统的除水反应釜中后,在搅拌的情况下加热至100-130℃,在真空度为-0.01MPa至-0.02MPa下进行抽水1-3小时,除去其中所含的水分。
步骤(7)得到UV固化高光涂料后过滤出料,密封遮光保存。
采用本发明合成的高光涂料利用了聚氨酯的柔韧性和丙烯酸酯的耐候性等优点,产品具有高亮度、附着力强、耐折、耐温、耐磨耐擦、单位涂量少、成本低、安全环保、耐老化、无毒无害等优点。
本发明的UV固化高光涂料无毒无害,对环境污染小,符合环保要求;制成高光纸后及后续加工(如印刷、烫金等),具有抗压花、耐溶剂、耐水、耐折耐爆、附着力强,平整度、流平性好等优点,UV照射后没有有机挥发性物析出,同时成本低,无毒、无害、无味,是一种理想的环保型高光包装材料,适用任何固物包装,更符合国家烟草、食品、医药等行业要求。
具体实施方式
实施例1
本实施例中,UV固化高光涂料的制备方法包括下述步骤:
(1)按重量计,配备下述原料:异氰酸酯36%(均为4,4'-二环己基甲烷二异氰酸酯),扩链树脂15%(均为分子量为560的聚天冬氨酸酯(商品名:广州齐翔Q420)),交联树脂10%(均为分子量为595的蔗糖为起始剂的聚醚多元醇(商品名:一诺威YNW-8343)),活性聚硅氧烷10%(均为分子量为1000的α,ω-二羟烃基聚硅氧烷),扩链剂2%(均为新戊二醇),交联剂0.3%(均为三羟甲基丙烷),催化剂0.1%(均为辛酸亚锡),羟基丙烯酸酯3%(均为丙烯酸羟乙酯15kg),多官能丙烯酸酯单体20%(均为三羟甲基丙烷三丙烯酸酯),光引发剂2%(均为二苯甲酮),流平剂0.6%(均为聚醚硅氧烷共聚物,迪高的TEGO Glide 410),消泡剂0.2%(均为聚醚型消泡剂,迪高的TEGO Foamex 805的消泡剂),抗静电剂0.2%(均为聚氨酯高分子抗静电剂),偶联剂0.6%(均为硅烷偶联剂KH560);
(2)将扩链树脂、交联树脂分别加入带有搅拌器及真空除水系统的除水反应釜中,除去其中所含的水分(将扩链树脂、交联树脂分别加入带有搅拌器及真空除水系统的除水反应釜中后,在搅拌的情况下加热至120℃,在真空度为-0.01MPa下进行抽水2小时,除去其中所含的水分);
(3)将已除水的扩链树脂加入聚合反应釜中,然后在搅拌的情况下滴加入异氰酸酯,并加热至70-85℃,反应1小时;然后加入已除水的交联树脂,在70-85℃下反应2小时;
(4)将聚合反应釜中的温度调节至65℃,再加入活性聚硅氧烷,在65-70℃下反应1小时;
(5)将聚合反应釜中的温度调节至65℃,再加入羟基丙烯酸酯和催化剂,加热至70-80℃,反应1小时;
(6)将聚合反应釜中的温度调节至65℃,再加入扩链剂和交联剂,升温至70-80℃,反应2小时;
(7)将聚合反应釜中的温度调节至60℃,再加入多官能丙烯酸酯单体、光引发剂、抗静电剂、流平剂、消泡剂和偶联剂,搅拌30分钟,得到UV固化高光涂料。
步骤(7)得到UV固化高光涂料后过滤出料,密封遮光保存。
实施例2
本实施例中,UV固化高光涂料的制备方法包括下述步骤:
(1)按重量计,配备下述原料:异氰酸酯55%(均为甲苯二异氰酸酯),扩链树脂5%(均为分子量为2000的聚氧化乙烯醚二醇(商品名:一诺威YNW-220)),交联树脂15%(均为分子量为500的聚氧化丙烯醚三醇(商品名:德信联邦DMN-500)),活性聚硅氧烷6%(均为分子量为1000的氨丙基封端聚二甲基硅氧烷),扩链剂3%(均为双酚A),交联剂0.1%(均为三羟甲基丙烷),催化剂0.2%(均为辛酸亚锡),羟基丙烯酸酯2%(均为甲基丙烯酸羟乙酯),多官能丙烯酸酯单体10%(均为三羟甲基丙烷三丙烯酸酯),光引发剂0.6%(均为二苯基乙二酮),流平剂1%(均为聚醚硅氧烷共聚物,迪高的TEGO Glide 410),消泡剂0.1%(均为聚醚型消泡剂,迪高的TEGO Foamex 805的消泡剂),抗静电剂1%(均为聚氨酯高分子抗静电剂),偶联剂1%(均为硅烷偶联剂KH560);
(2)将扩链树脂、交联树脂分别加入带有搅拌器及真空除水系统的除水反应釜中,除去其中所含的水分(将扩链树脂、交联树脂分别加入带有搅拌器及真空除水系统的除水反应釜中后,在搅拌的情况下加热至100℃,在真空度为-0.02MPa下进行抽水1.5小时,除去其中所含的水分);
(3)将已除水的扩链树脂加入聚合反应釜中,然后在搅拌的情况下滴加入异氰酸酯,并加热至70-85℃,反应2小时;然后加入已除水的交联树脂,在70-85℃下反应3小时;
(4)将聚合反应釜中的温度调节至60℃,再加入活性聚硅氧烷,在65-70℃下反应1.5小时;
(5)将聚合反应釜中的温度调节至60℃,再加入羟基丙烯酸酯和催化剂,加热至70-80℃,反应1.5小时;
(6)将聚合反应釜中的温度调节至60℃,再加入扩链剂和交联剂,升温至70-80℃,反应3小时;
(7)将聚合反应釜中的温度调节至55℃,再加入多官能丙烯酸酯单体、光引发剂、抗静电剂、流平剂、消泡剂和偶联剂,搅拌50分钟,得到UV固化高光涂料。
步骤(7)得到UV固化高光涂料后过滤出料,密封遮光保存。
实施例3
本实施例中,UV固化高光涂料的制备方法包括下述步骤:
(1)按重量计,配备下述原料:异氰酸酯21%(均为六亚甲基二异氰酸酯三聚体),扩链树脂20%(均为分子量为430的聚氧化乙烯醚二胺(商品名:德信联邦ZD140)),交联树脂5%(均为分子量为400,官能度为3.5的山梨醇聚醚多元醇),活性聚硅氧烷5%(均为分子量为1000的α,ω-二羟烃基聚硅氧烷),扩链剂4%(均为1,4-丁二醇),交联剂0.5%(均为三羟甲基丙烷),催化剂0.05%(均为二月桂酸二丁基锡),羟基丙烯酸酯10%(均为丙烯酸羟乙酯),多官能丙烯酸酯单体25%(均为三丙二醇二丙烯酸酯),光引发剂5%(均为联苯甲酰),流平剂0.8%(均为聚醚硅氧烷共聚物,迪高的TEGO Glide 410),消泡剂0.15%(均为聚醚型消泡剂,迪高的TEGO Foamex 805的消泡剂),抗静电剂2%(均为聚氨酯高分子抗静电剂),偶联剂1.5%(均为硅烷偶联剂KH560);
(2)将扩链树脂、交联树脂分别加入带有搅拌器及真空除水系统的除水反应釜中,除去其中所含的水分(将扩链树脂、交联树脂分别加入带有搅拌器及真空除水系统的除水反应釜中后,在搅拌的情况下加热至120℃,在真空度为-0.01MPa下进行抽水1.5小时,除去其中所含的水分);
(3)将已除水的扩链树脂加入聚合反应釜中,然后在搅拌的情况下滴加入异氰酸酯,并加热至70-85℃,反应1小时;然后加入已除水的交联树脂,在70-85℃下反应2小时;
(4)将聚合反应釜中的温度调节至65℃,再加入活性聚硅氧烷,在65-70℃下反应1小时;
(5)将聚合反应釜中的温度调节至65℃,再加入羟基丙烯酸酯和催化剂,加热至70-80℃,反应1小时;
(6)将聚合反应釜中的温度调节至65℃,再加入扩链剂和交联剂,升温至70-80℃,反应2小时;
(7)将聚合反应釜中的温度调节至60℃,再加入多官能丙烯酸酯单体、光引发剂、抗静电剂、流平剂、消泡剂和偶联剂,搅拌45分钟,得到UV固化高光涂料。
步骤(7)得到UV固化高光涂料后过滤出料,密封遮光保存。
将实施例1-3的UV固化高光涂料和现有市场高光涂料产品,分别均匀涂布在卡纸上,与OPP膜复合,在功率为1000W的高压UV汞灯下光照10秒,剥离回收OPP膜。实施例1-3和现有市场产品的检测指标见下表。从表中可知,本发明制造的高光涂料表面光泽度、附着力、耐折性、耐热性及印刷适应性都优于市场产品。
Claims (4)
1.一种用于复合转移工艺生产高光纸的UV固化高光涂料,其特征在于由下述重量配比的原料制成:异氰酸酯20-60%,扩链树脂5-25%,交联树脂5-20%,活性聚硅氧烷5-15%,扩链剂0.5-5%,交联剂0.1-0.5%,催化剂0.02-0.2%,羟基丙烯酸酯1-10%,多官能丙烯酸酯单体10-30%,光引发剂0.5-5%,流平剂0.5-1%,消泡剂0.1-0.2%,抗静电剂0.2-2%,偶联剂0.5-2%;
所述扩链树脂是聚醚二元胺、聚醚二元醇、聚酯二元醇或聚天门冬氨酸酯;
所述活性聚硅氧烷是氨丙基封端聚二甲基硅氧烷或醇羟基封端二甲基硅氧烷,其分子量为500-4000;
所述异氰酸酯是异佛尔酮二异氰酸酯、4,4′-二环己基甲烷二异氰酸酯、甲苯二异氰酸酯、六亚甲基二异氰酸酯和HDI三聚体中的一种或其中多种的组合;
所述交联树脂是分子量为200-1000的聚醚多元醇;
所述扩链剂是1,4-丁二醇、新戊二醇、一缩二乙二醇、双酚A、异氟尔酮二胺、乙二胺或苯二胺;
所述交联剂是丙三醇、季戊四醇或三羟甲基丙烷;
所述催化剂是二月桂酸二丁基锡、辛酸亚锡、异辛酸钾催化剂或铋类催化剂;
所述羟基丙烯酸酯是丙烯酸羟乙酯或甲基丙烯酸羟乙酯;
所述多官能丙烯酸酯单体是三丙二醇二丙烯酸酯、三羟甲基丙烷三丙烯酸酯或二季戊四醇五丙烯酸酯;
所述光引发剂是自由基光引发剂或阳离子光引发剂;所述自由基光引发剂是二苯基乙二酮、联苯甲酰或二苯甲酮。
2.根据权利要求1所述的用于复合转移工艺生产高光纸的UV固化高光涂料,其特征是:
所述流平剂是聚醚硅氧烷共聚物;
所述消泡剂是聚醚型消泡剂;
所述抗静电剂是阳离子抗静电剂、阴离子抗静电剂或非离子抗静电剂;
所述偶联剂是硅烷偶联剂KH560。
3.权利要求1所述的用于复合转移工艺生产高光纸UV固化高光涂料的制备方法,其特征在于包括下述步骤:
(1)按重量计,配备下述原料:异氰酸酯20-60%,扩链树脂5-25%,交联树脂5-20%,活性聚硅氧烷5-15%,扩链剂0.5-5%,交联剂0.1-0.5%,催化剂0.02-0.2%,羟基丙烯酸酯1-10%,多官能丙烯酸酯单体10-30%,光引发剂0.5-5%,流平剂0.5-1%,消泡剂0.1-0.2%,抗静电剂0.2-2%,偶联剂0.5-2%;
(2)将扩链树脂、交联树脂分别加入带有搅拌器及真空除水系统的除水反应釜中,除去其中所含的水分;
(3)将已除水的扩链树脂加入聚合反应釜中,然后在搅拌的情况下滴加入异氰酸酯,并加热至70-85℃,反应0.5-2小时;然后加入已除水的交联树脂,在70-85℃下反应1-4小时;
(4)将聚合反应釜中的温度调节至55-70℃,再加入活性聚硅氧烷,在65-70℃下反应0.5-3小时;
(5)将聚合反应釜中的温度调节至55-70℃,再加入羟基丙烯酸酯和催化剂,加热至70-80℃,反应0.5-3小时;
(6)将聚合反应釜中的温度调节至55-70℃,再加入扩链剂和交联剂,升温至70-80℃,反应1-4小时;
(7)将聚合反应釜中的温度调节至50-70℃,再加入多官能丙烯酸酯单体、光引发剂、抗静电剂、流平剂、消泡剂和偶联剂,搅拌20-60分钟,得到UV固化高光涂料。
4.根据权利要求3所述的用于复合转移工艺生产高光纸的UV固化高光涂料的制备方法,其特征在于:步骤(2)中,将扩链树脂、交联树脂分别加入带有搅拌器及真空除水系统的除水反应釜中后,在搅拌的情况下加热至100-130℃,在真空度为-0.01MPa至-0.02MPa下进行抽水1-3小时,除去其中所含的水分。
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