CN104629612B - 一种高折光防雾薄膜涂层的制备方法 - Google Patents

一种高折光防雾薄膜涂层的制备方法 Download PDF

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CN104629612B
CN104629612B CN201310565802.2A CN201310565802A CN104629612B CN 104629612 B CN104629612 B CN 104629612B CN 201310565802 A CN201310565802 A CN 201310565802A CN 104629612 B CN104629612 B CN 104629612B
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姚伯龙
李根龙
韩兵
张国标
齐家鹏
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Abstract

一种高折光防雾薄膜涂层的制备方法，以2,5‑双[(2‑羟基)丙硫基]‑1,3,4‑噻二唑(自制)、间苯二甲酸二缩三乙二醇酯‑5‑磺酸钠(自制)、异佛尔酮二异氰酸酯及季戊四醇三丙烯酸酯为主要原料，以N‑甲基吡咯烷酮作溶剂，二月桂酸二丁基锡为催化剂，对苯二甲醇为扩链剂制备了可UV固化的高折光亲水预聚物；以钛酸丁酯为前驱体，以乙烯基三乙氧基硅烷为改性剂，采用溶胶‑凝胶法制得均一、稳定的TiO2溶胶；采用UV固化的方式将高折光亲水预聚物与TiO2溶胶进行杂化制得薄膜涂层。本发明所制备的薄膜涂层硬度、附着力及耐水性好，折射率高，防雾效果佳，可用于镜片表面的防雾，实现眼镜片的薄型化；该薄膜涂层制备工艺符合绿色环保理念，固化成膜快，具有较好的市场前景。

Description

一种高折光防雾薄膜涂层的制备方法
技术领域
一种高折光防雾薄膜涂层的制备方法属于紫外光固化领域
背景技术
近年来，随着光学应用领域的不断拓展，传统的光学材料已经不能满足人们对材料和器件微型化、多功能和集成化等方面的要求，研究制备多功能新型光学材料备受人们的广泛关注。目前综合UV固化技术和有机无机杂化技术制备高折光防雾薄膜薄膜涂层的研究鲜有报道，作为新型的多功能光学材料，高折光防雾薄膜涂层不仅能满足人们对材料和器件微型化、多功能化、集成化等方面的要求，而且被广泛应用于树脂镜片、汽车玻璃、光学元件、功能材料和信息存储器件等多个不同领域。因此制备高折光防雾薄膜涂层是未来光学材料的主流研究方向。
发明内容
本发明的目的是设计出制备硬度及附着力较好，耐水，折射率高且防雾效果佳的薄膜涂层的工艺。该技术的创新点在于综合UV固化技术与有机无机杂化技术的优点，以2,5-双[(2’-羟基)丙硫基]-1,3,4-噻二唑(自制)、间苯二甲酸二缩三乙二醇酯-5-磺酸钠(自制)、异佛尔酮二异氰酸酯(IPDI)及季戊四醇三丙烯酸酯(PETA)为主要原料，以1-甲基-2-吡咯烷酮(NMP)作为溶剂，二月桂酸二丁基锡(DBTDL)为催化剂，对苯二甲醇为扩链剂制备可UV固化的高折光亲水预聚物，再以钛酸丁酯(TBT)为前驱体，以乙烯基三乙氧基硅烷(A-151)为改性剂，采用溶胶-凝胶法制得均一、稳定的TiO2溶胶；最后通过UV固化的方式将高折光亲水预聚物与TiO2溶胶进行杂化制得薄膜涂层。所得产品硬度及附着力较好，耐水，折射率高且防雾效果佳。
(1)高折光亲水UV预聚物的合成，各组分的质量份如下：
称取IPDI，置于三口烧瓶中，边搅拌边滴加2,5-双[(2’-羟基)丙硫基]-1，3，4-噻二唑与间苯二甲酸二缩三乙二醇酯-5-磺酸钠的混合液，约30min，期间滴3-4d二月桂酸二丁基锡(DBTDL)，温度控制为50℃。滴加完毕后，继续反应1h，以二正丁胺法监测体系中NCO值的变化，当达到理论值时，加入对苯二甲醇，同时升温至70℃；反应6-7h后，以二正丁胺法监测体系中NCO值的变化，当达到理论值时，加入季戊四醇三丙烯酸酯(PETA)继续反应，整个反应过程都以1-甲基-2-吡咯烷酮(NMP)控制体系粘度。当NCO达到理论值时，反应结束，保存产物，以待后用。
(2)TiO2溶胶的合成，各组分的体积份如下：
将钛酸丁酯(TBT)，乙烯基三乙氧基硅烷(A-151)和无水乙醇按一定的体积比混合，置于磁力搅拌水浴中(70℃)，滴加0.1ml乙酰丙酮(AcAc)，用浓盐酸调pH在4-5内，搅拌15min后向烧杯中逐滴加入去离子水。经过磁力搅拌2h和陈化48h后得到A-151改性的TiO2溶胶。
(3)高折光防雾薄膜涂层的合成，各组分的质量份如下：
称取高折光亲水UV预聚物、TMPTA、光引发剂819、TiO2溶胶和NMP，避光混合搅拌均匀，再将其涂覆在干净玻璃板上成膜，待溶剂挥发后，置于紫外灯下光固化，即得高折光防雾薄膜涂层。
具体实施方式
实施例1
(1)高折光亲水UV预聚物的合成，各组分的质量如下：
称取15.6g IPDI，置于三口烧瓶中，边搅拌边滴加15g2,5-双[(2’-羟基)丙硫基]-1，3，4-噻二唑与24g间苯二甲酸二缩三乙二醇酯-5-磺酸钠的混合液，约30min，期间滴3-4d二月桂酸二丁基锡(DBTDL)，温度控制为50℃。滴加完毕后，继续反应1h，以二正丁胺法监测体系中NCO值的变化，当达到理论值时，加入1.8g对苯二甲醇，同时升温至70℃；反应6-7h后，以二正丁胺法监测体系中NCO值的变化，当达到理论值时，加入3.6g季戊四醇三丙烯酸酯(PETA)继续反应，整个反应过程都以1-甲基-2-吡咯烷酮(NMP)控制体系粘度。当NCO达到理论值时，反应结束，保存产物，以待后用。
(2)TiO2溶胶的合成，各组分的体积如下：
将20ml钛酸丁酯(TBT)，8ml乙烯基三乙氧基硅烷(A-151)和60ml无水乙醇按一定的体积比混合，置于磁力搅拌水浴中(70℃)，滴加0.1ml乙酰丙酮(AcAc)，用浓盐酸调pH在4-5内，搅拌15min后向烧杯中逐滴加入25ml去离子水。经过磁力搅拌2h和陈化48h后得到A-151改性的TiO2溶胶。
(3)高折光防雾薄膜涂层的合成，各组分的质量如下：
定量称取高折光亲水UV预聚物、TMPTA、光引发剂819、TiO2溶胶和NMP，避光混合搅拌均匀，再将其涂覆在干净玻璃板上成膜，待溶剂挥发后，置于紫外灯下光固化，即得高折光防雾薄膜涂层。
实施例2
(1)高折光亲水UV预聚物的合成，各组分的质量如下：
季戊四醇三丙烯酸酯(PETA) 3.6g
称取15.6g IPDI，置于三口烧瓶中，边搅拌边滴加15g2,5-双[(2’-羟基)丙硫基]-1，3，4-噻二唑与24g间苯二甲酸二缩三乙二醇酯-5-磺酸钠的混合液，约30min，期间滴3-4d二月桂酸二丁基锡(DBTDL)，温度控制为50℃。滴加完毕后，继续反应1h，以二正丁胺法监测体系中NCO值的变化，当达到理论值时，加入1.8g对苯二甲醇，同时升温至70℃；反应6-7h后，以二正丁胺法监测体系中NCO值的变化，当达到理论值时，加入3.6g季戊四醇三丙烯酸酯(PETA)继续反应，整个反应过程都以1-甲基-2-吡咯烷酮(NMP)控制体系粘度。当NCO达到理论值时，反应结束，保存产物，以待后用。
(2)TiO2溶胶的合成，各组分的质量如下：
将20ml钛酸丁酯(TBT)，10ml乙烯基三乙氧基硅烷(A-151)和60ml无水乙醇按一定的体积比混合，置于磁力搅拌水浴中(70℃)，滴加0.1ml乙酰丙酮(AcAc)，用浓盐酸调pH在4-5内，搅拌15min后向烧杯中逐滴加入35ml去离子水。经过磁力搅拌2h和陈化48h后得到A-151改性的TiO2溶胶。
(3)高折光防雾薄膜涂层的合成，各组分的质量如下：
定量称取高折光亲水UV预聚物、TMPTA、光引发剂819、TiO2溶胶和NMP，避光混合搅拌均匀，再将其涂覆在干净玻璃板上成膜，待溶剂挥发后，置于紫外灯下光固化，即得高折光防雾薄膜涂层。

Claims (1)

1.一种高折光防雾薄膜涂层的制备方法，其特征步骤为：
(1)高折光亲水UV预聚物的合成，各组分的质量份如下：
称取IPDI，置于三口烧瓶中，边搅拌边滴加2，5-双[(2′-羟基)丙硫基]-1，3，4-噻二唑与间苯二甲酸二缩三乙二醇酯-5-磺酸钠的混合液，30min，期间滴3-4d二月桂酸二丁基锡，温度控制为50℃；滴加完毕后，继续反应1h，以二正丁胺法监测体系中NCO值的变化，当达到理论值时，加入对苯二甲醇，同时升温至70℃；反应6-7h后，以二正丁胺法监测体系中NCO值的变化，当达到理论值时，加入季戊四醇三丙烯酸酯继续反应；整个反应过程都以1-甲基-2-吡咯烷酮控制体系粘度，当NCO达到理论值时，反应结束，保存产物以待后用；
(2)TiO2溶胶的合成，各组分的体积份如下：
将钛酸丁酯，乙烯基三乙氧基硅烷A-151和无水乙醇按一定的体积比混合，置于70℃的磁力搅拌水浴中，滴加0.1ml乙酰丙酮，用浓盐酸调pH在4-5内，搅拌15min后向烧杯中逐滴加入去离子水；经过磁力搅拌2h和陈化48h后得到A-151改性的TiO2溶胶；
(3)高折光防雾薄膜涂层的合成，各组分的质量份如下：
称取高折光亲水UV预聚物、TMPTA、光引发剂819、TiO2溶胶和1-甲基-2-吡咯烷酮，避光混合搅拌均匀，再将其涂覆在干净玻璃板上成膜，待溶剂挥发后，置于紫外灯下光固化，即得高折光防雾薄膜涂层。
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