CN114853955A - 一种高透氧超柔软的硅水凝胶日抛透片的制备方法 - Google Patents
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Abstract
本发明公开了一种高透氧超柔软的硅水凝胶日抛透片的制备方法,包括以下步骤:S1:准备材料;S2:盐酸标准溶液的配置;S3:氢氧化钾标准溶液的配制;S4:紫外光固化有机硅改性聚氨酯预聚物;S5:紫外光固化羟基改性有机硅预聚物的制备;S6:硅水凝胶日抛透片材料的准备;S7:硅水凝胶日抛透片的制备。本发明所述的一种高透氧超柔软的硅水凝胶日抛透片的制备方法,制备的硅水凝胶日抛透片具有优异的光学性能,在吸水平衡状态下,在可见光区的透光率大于95%,通过加入的氢氧化钾标准溶液和盐酸标准溶液能降低材料中自由水的含量,因此,在硅水凝胶材料中引入能与水分子紧密结合的羟基或离子基团,能提高材料的抗脱水性能。
Description
技术领域
本发明涉及日抛透片领域,特别涉及一种高透氧超柔软的硅水凝胶日抛透片的制备方法。
背景技术
日抛是指隐形眼镜中的一种术语,意思是使用期限为一天,然后抛弃,该镜片的唯一的优点就是不用买护理液,不用天天护理。
硅水凝胶,是一种有机高分子材料,有亲水性,具有双位相材料构架,即拥有氟硅和水凝胶两种通道,常被用来制作高档隐形眼镜,现有的硅水凝胶日抛透片经使用中使用后,会常常产生脱水现象,导致使用者眼睛干燥,导致其佩戴不属实,且不够柔软,影响使用者的日常佩戴,透气性能不足,再佩戴久后,会出现供氧不足和二氧化碳的存在,导致会应发以下眼部疾病,危害使用者的眼部健康。
发明内容
本发明的主要目的在于提供一种高透氧超柔软的硅水凝胶日抛透片的制备方法,可以有效解决背景技术中的问题。
为实现上述目的,本发明采取的技术方案为:
一种高透氧超柔软的硅水凝胶日抛透片的制备方法,包括以下操作步骤:
S1:准备材料;准备试剂,包括:浓盐酸、甲苯、吡啶、无水碳酸钠、氢氧化钾、邻苯二甲酸酐、邻苯二甲酸氢钾、异丙醇、二正丁胺、异佛尔酮二异腈酸酯、二丁基二月桂酸锡、甲基丙烯酸羟乙酯、羟基烷基封端的聚二甲基硅氧烷,准备仪器,包括电子天平、傅立叶红外光谱、核磁共振;
S2:盐酸标准溶液的配置:量取约8.3ml浓盐酸到干燥的1000ml容量瓶中,用蒸馏水稀释至1000ml,在电子天平上准确称取无水碳酸钠三份,每份质量约0.106g~1.159g,分别置于250ml的键形瓶中,加入约20ml蒸馏水,振荡使无水碳酸钠溶解,然后每份无水碳酸钠溶液中滴入2-3滴甲基橙指示剂,用欲标定的盐酸溶液洗涤酸氏滴定管,每次5-10ml,然后,用盐酸溶液滴定标准的无水碳酸钠溶液,溶液颜色从黄色变为橙色时,停止滴定,在接近滴定终点时,应剧烈振荡除去溶液中溶解的二氧化碳,计下每次消耗的盐酸体积数,计算盐酸溶液的摩尔浓度,要求三份测定值与平均值的相对偏差小于0.2%;
S3:氢氧化钾标准溶液的配制:称取28g氢氧化钾固体于烧杯中,加入100ml蒸馏水,溶解后,将溶液转移至1000ml容量瓶中,用蒸馏水稀释至1000ml,用电子天平准确称取已在110℃-120℃温度下干燥2h的邻苯二甲酸钾三份,每份约2.0g~3.0g,以每份消耗0.5mol/LKOH溶液0~30m1为准,加入50m1蒸馏水,振荡使邻苯二甲酸钾溶解,然后加入3-5滴酚酞指示剂,用欲标定的KOH溶液洗涤碱氏滴定管三次,每次5-10ml,用KOH溶液滴定标准的邻苯二甲酸氢钾溶液,溶液颜色由无色变为微红色时,停止滴定,计下每次消耗的KOH溶液的体积数,计算KOH溶液的摩尔浓度,要求三份测定值与平均值的相对偏差小于0.5%;
S4:紫外光固化有机硅改性聚氨酯预聚物,在装有机械搅拌和干燥管的干燥四颈瓶中加入1.64g的异佛尔酮二异腈酸酯、0.12g的二丁基二月桂酸锡、11.03gF6002,通N2,40℃下搅拌反应数小时,以标准二正丁胺法测定反应物中-NCO含量来确定反应进程和反应时间,待-NCO含量达理论计算值且保持不到变时,加1.10g甲基丙烯酸羟乙酯、数滴二丁基二月桂酸锡、绿豆大小的阻聚剂对苯二酚到反应容器中,80℃下继续反应数小时,用标准二正丁胺法确定反应进度,再加入制好的氢氧化钾标准溶液和盐酸标准溶液,直到检测不出-NCO时,反应结束后,得到无色透明或淡黄色的目标产物,将产物密封,置于冰箱中保存;
S5:紫外光固化羟基改性有机硅预聚物的制备:在100ml三口瓶中,准确称取2份甲基丙烯酸羟乙酯,将一装有无水二氯化钙的干燥管插入瓶口,使反应容器内部与空气相通并隔绝外面的湿气进入瓶内,80℃下,机械搅拌反应约5h后结束,得到无色透明、有一定粘度的产物,将产物密封,置于冰箱中待用;
S6:硅水凝胶日抛透片材料的准备:紫外光固化羟基改性有机硅预聚物、紫外光固化有机硅改性聚氨酯预聚物、甲基丙烯酸羟乙酯、二甲基丙烯酰胺、光引发剂、异丙醇、无水乙醇、高纯N2、三甲基硅氧基、氟硅氧烷单体、亲水性物质、非亲水性物质、交联剂、紫外吸收剂;
S7:硅水凝胶日抛透片的制备:将各种材料、光引发剂和溶剂置于烧杯中,用滴管吸取配好的混合液,滴入普通玻璃制作的模具中,缓慢盖上表面覆盖有聚乙烯保鲜膜的玻璃板,确保溶液中没有气泡,用夹子夹紧模具四周,使反应体系处于密封状态,将密封的模具放置在高强度紫外灯下,照射约1h,熄灯后取出模具,将模具放入超声波中振荡数分钟,去除紧贴保鲜膜的玻璃板,剥去保鲜膜,将剩下玻璃板放入蒸馏水中浸泡过夜或水煮,使膜溶胀吸水,再将氟硅氧烷单体、亲水性物质、非亲水性物质、交联剂、紫外吸收剂加入其中进行混合,去除玻璃板后,即得到硅水凝胶日抛透片,其中以上所代表的化合物及类似结构化合物为氟硅氟烷材料:
其中R1-R3均为H或者F,R4为含-F取代基团的烷基或醇基团其中任一种,R4长度为2-4。
优选的,所述甲苯使用前用4A分子筛浸泡干燥,并重蒸后使用。
优选的,所述二正丁胺使用前用4A分子筛浸泡干燥,并重蒸收集158度的馏分。
优选的,所述甲基丙烯酸羟乙酯使用前用4A分子筛浸泡干燥,并做减压蒸馏。
优选的,所述羟基烷基封端的聚二甲基硅氧烷使用前在真空下干燥不少于五小时,温度约为六十度。
与现有技术相比,本发明具有如下有益效果:
本发明中,制备的硅水凝胶日抛透片具有优异的光学性能,在吸水平衡状态下,在可见光区的透光率大于95%,在从干燥状态到水合状态的变化过程中,硅水凝胶材料的透光率随水含量的增加而增大,通过加入的氢氧化钾标准溶液和盐酸标准溶液能降低材料中自由水的含量,因此,在硅水凝胶材料中引入能与水分子紧密结合的羟基或离子基团,能提高材料的抗脱水性能,有效提高了镜片的保水性能,降低了脱水现象,避免了使用者在使用时常常会产生眼睛干燥的现象,且制成的硅水凝胶日抛透片柔软度较高,穿戴时也较为舒适。
具体实施方式
下面将结合本发明的实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
本发明涉及一种高透氧超柔软的硅水凝胶日抛透片的制备方法,包括以下步骤:
具体实施例一:
(1):准备试剂,包括:浓盐酸、甲苯、吡啶、无水碳酸钠、氢氧化钾、邻苯二甲酸酐、邻苯二甲酸氢钾、异丙醇、二正丁胺、异佛尔酮二异腈酸酯、二丁基二月桂酸锡、甲基丙烯酸羟乙酯、羟基烷基封端的聚二甲基硅氧烷,准备仪器,包括电子天平、傅立叶红外光谱、核磁共振,二正丁胺使用前用4A分子筛浸泡干燥,并重蒸收集158度的馏分。
(2):量取约8.3ml浓盐酸到干燥的1000ml容量瓶中,用蒸馏水稀释至1000ml,在电子天平上准确称取无水碳酸钠三份,每份质量约0.106g~1.159g,分别置于250ml的键形瓶中,加入约20ml蒸馏水,振荡使无水碳酸钠溶解,然后每份无水碳酸钠溶液中滴入2-3滴甲基橙指示剂,用欲标定的盐酸溶液洗涤酸氏滴定管,每次5-10ml,然后,用盐酸溶液滴定标准的无水碳酸钠溶液,溶液颜色从黄色变为橙色时,停止滴定,在接近滴定终点时,应剧烈振荡除去溶液中溶解的二氧化碳,计下每次消耗的盐酸体积数,计算盐酸溶液的摩尔浓度,要求三份测定值与平均值的相对偏差小于0.2%。
(3):称取28g氢氧化钾固体于烧杯中,加入100ml蒸馏水,溶解后,将溶液转移至1000ml容量瓶中,用蒸馏水稀释至1000ml,用电子天平准确称取已在110℃-120℃温度下干燥2h的邻苯二甲酸钾三份,每份约2.0g~3.0g,以每份消耗0.5mol/LKOH溶液0~30m1为准,加入50m1蒸馏水,振荡使邻苯二甲酸钾溶解,然后加入3-5滴酚酞指示剂,用欲标定的KOH溶液洗涤碱氏滴定管三次,每次5-10ml,用KOH溶液滴定标准的邻苯二甲酸氢钾溶液,溶液颜色由无色变为微红色时,停止滴定,计下每次消耗的KOH溶液的体积数,计算KOH溶液的摩尔浓度,要求三份测定值与平均值的相对偏差小于0.5%。
(4):在装有机械搅拌和干燥管的干燥四颈瓶中加入1.64g的异佛尔酮二异腈酸酯、0.12g的二丁基二月桂酸锡、11.03gF6002,通N2,40℃下搅拌反应数小时,以标准二正丁胺法测定反应物中-NCO含量来确定反应进程和反应时间,待-NCO含量达理论计算值且保持不到变时,加1.10g甲基丙烯酸羟乙酯、数滴二丁基二月桂酸锡、绿豆大小的阻聚剂对苯二酚到反应容器中,80℃下继续反应数小时,用标准二正丁胺法确定反应进度,再加入制好的氢氧化钾标准溶液和盐酸标准溶液,直到检测不出-NCO时,反应结束后,得到无色透明或淡黄色的目标产物,将产物密封,置于冰箱中保存,甲基丙烯酸羟乙酯使用前用4A分子筛浸泡干燥,并做减压蒸馏。
(5):在100ml三口瓶中,准确称取2份甲基丙烯酸羟乙酯,将一装有无水二氯化钙的干燥管插入瓶口,使反应容器内部与空气相通并隔绝外面的湿气进入瓶内,80℃下,机械搅拌反应约5h后结束,得到无色透明、有一定粘度的产物,将产物密封,置于冰箱中待用,羟基烷基封端的聚二甲基硅氧烷使用前在真空下干燥不少于五小时,温度约为六十度。
(6):准备紫外光固化羟基改性有机硅预聚物、紫外光固化有机硅改性聚氨酯预聚物、甲基丙烯酸羟乙酯、二甲基丙烯酰胺、光引发剂、异丙醇、无水乙醇、高纯N2、三甲基硅氧基、氟硅氧烷单体、亲水性物质、非亲水性物质、交联剂、紫外吸收剂。
(7):将各种材料、光引发剂和溶剂置于烧杯中,用滴管吸取配好的混合液,滴入普通玻璃制作的模具中,缓慢盖上表面覆盖有聚乙烯保鲜膜的玻璃板,确保溶液中没有气泡,用夹子夹紧模具四周,使反应体系处于密封状态,将密封的模具放置在高强度紫外灯下,照射约1h,熄灯后取出模具,将模具放入超声波中振荡数分钟,去除紧贴保鲜膜的玻璃板,剥去保鲜膜,将剩下玻璃板放入蒸馏水中浸泡过夜或水煮,使膜溶胀吸水,再将氟硅氧烷单体、亲水性物质、非亲水性物质、交联剂、紫外吸收剂加入其中进行混合,去除玻璃板后,即得到硅水凝胶日抛透片,其中以上所代表的化合物及类似结构化合物为氟硅氟烷材料:
其中R1-R3均为H或者F,R4为含-F取代基团的烷基或醇基团其中任一种,R4长度为2-4。
具体实施例二:
表一:1~3的配比
表二:配方1~3后的处理条件及结果
表一,表二结果显示,当采用规定分量的无水碳酸钠、氢氧化钾固体和邻苯二甲酸钾所制成的硅水凝胶镜片可用本工艺得到较好外形,和较好表面质量的镜片。
根据具体实例一-二步骤制备的硅水凝胶日抛透片具有优异的光学性能,在吸水平衡状态下,在可见光区的透光率大于95%,在从干燥状态到水合状态的变化过程中,硅水凝胶材料的透光率随水含量的增加而增大,通过加入的氢氧化钾标准溶液和盐酸标准溶液能降低材料中自由水的含量,因此,在硅水凝胶材料中引入能与水分子紧密结合的羟基或离子基团,能提高材料的抗脱水性能,有效提高了镜片的保水性能,降低了脱水现象,避免了使用者在使用时常常会产生眼睛干燥的现象,且制成的硅水凝胶日抛透片柔软度较高,穿戴时也较为舒适。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (5)
1.一种高透氧超柔软的硅水凝胶日抛透片的制备方法,其特征在于:包括以下操作步骤:
S1:准备材料;准备试剂,包括:浓盐酸、甲苯、吡啶、无水碳酸钠、氢氧化钾、邻苯二甲酸酐、邻苯二甲酸氢钾、异丙醇、二正丁胺、异佛尔酮二异腈酸酯、二丁基二月桂酸锡、甲基丙烯酸羟乙酯、羟基烷基封端的聚二甲基硅氧烷,准备仪器,包括电子天平、傅立叶红外光谱、核磁共振;
S2:盐酸标准溶液的配置:量取约8.3ml浓盐酸到干燥的1000ml容量瓶中,用蒸馏水稀释至1000ml,在电子天平上准确称取无水碳酸钠三份,每份质量约0.106g~1.159g,分别置于250ml的键形瓶中,加入约20ml蒸馏水,振荡使无水碳酸钠溶解,然后每份无水碳酸钠溶液中滴入2-3滴甲基橙指示剂,用欲标定的盐酸溶液洗涤酸氏滴定管,每次5-10ml,然后,用盐酸溶液滴定标准的无水碳酸钠溶液,溶液颜色从黄色变为橙色时,停止滴定,在接近滴定终点时,应剧烈振荡除去溶液中溶解的二氧化碳,计下每次消耗的盐酸体积数,计算盐酸溶液的摩尔浓度,要求三份测定值与平均值的相对偏差小于0.2%;
S3:氢氧化钾标准溶液的配制:称取28g氢氧化钾固体于烧杯中,加入100ml蒸馏水,溶解后,将溶液转移至1000ml容量瓶中,用蒸馏水稀释至1000ml,用电子天平准确称取已在110℃-120℃温度下干燥2h的邻苯二甲酸钾三份,每份约2.0g~3.0g,以每份消耗0.5mol/LKOH溶液0~30m1为准,加入50m1蒸馏水,振荡使邻苯二甲酸钾溶解,然后加入3-5滴酚酞指示剂,用欲标定的KOH溶液洗涤碱氏滴定管三次,每次5-10ml,用KOH溶液滴定标准的邻苯二甲酸氢钾溶液,溶液颜色由无色变为微红色时,停止滴定,计下每次消耗的KOH溶液的体积数,计算KOH溶液的摩尔浓度,要求三份测定值与平均值的相对偏差小于0.5%;
S4:紫外光固化有机硅改性聚氨酯预聚物,在装有机械搅拌和干燥管的干燥四颈瓶中加入1.64g的异佛尔酮二异腈酸酯、0.12g的二丁基二月桂酸锡、11.03gF6002,通N2,40℃下搅拌反应数小时,以标准二正丁胺法测定反应物中-NCO含量来确定反应进程和反应时间,待-NCO含量达理论计算值且保持不到变时,加1.10g甲基丙烯酸羟乙酯、数滴二丁基二月桂酸锡、绿豆大小的阻聚剂对苯二酚到反应容器中,80℃下继续反应数小时,用标准二正丁胺法确定反应进度,再加入制好的氢氧化钾标准溶液和盐酸标准溶液,直到检测不出-NCO时,反应结束后,得到无色透明或淡黄色的目标产物,将产物密封,置于冰箱中保存;
S5:紫外光固化羟基改性有机硅预聚物的制备:在100ml三口瓶中,准确称取2份甲基丙烯酸羟乙酯,将一装有无水二氯化钙的干燥管插入瓶口,使反应容器内部与空气相通并隔绝外面的湿气进入瓶内,80℃下,机械搅拌反应约5h后结束,得到无色透明、有一定粘度的产物,将产物密封,置于冰箱中待用;
S6:硅水凝胶日抛透片材料的准备:紫外光固化羟基改性有机硅预聚物、紫外光固化有机硅改性聚氨酯预聚物、甲基丙烯酸羟乙酯、二甲基丙烯酰胺、光引发剂、异丙醇、无水乙醇、高纯N2、三甲基硅氧基、氟硅氧烷单体、亲水性物质、非亲水性物质、交联剂、紫外吸收剂;
S7:硅水凝胶日抛透片的制备:将各种材料、光引发剂和溶剂置于烧杯中,用滴管吸取配好的混合液,滴入普通玻璃制作的模具中,缓慢盖上表面覆盖有聚乙烯保鲜膜的玻璃板,确保溶液中没有气泡,用夹子夹紧模具四周,使反应体系处于密封状态,将密封的模具放置在高强度紫外灯下,照射约1h,熄灯后取出模具,将模具放入超声波中振荡数分钟,去除紧贴保鲜膜的玻璃板,剥去保鲜膜,将剩下玻璃板放入蒸馏水中浸泡过夜或水煮,使膜溶胀吸水,再将氟硅氧烷单体、亲水性物质、非亲水性物质、交联剂、紫外吸收剂加入其中进行混合,去除玻璃板后,即得到硅水凝胶日抛透片,其中以上所代表的化合物及类似结构化合物为氟硅氟烷材料:
其中R1-R3均为H或者F,R4为含-F取代基团的烷基或醇基团其中任一种,R4长度为2-4。
2.根据权利要求1所述的一种高透氧超柔软的硅水凝胶日抛透片的制备方法,其特征在于:所述甲苯使用前用4A分子筛浸泡干燥,并重蒸后使用。
3.根据权利要求1所述的一种高透氧超柔软的硅水凝胶日抛透片的制备方法,其特征在于:所述二正丁胺使用前用4A分子筛浸泡干燥,并重蒸收集158度的馏分。
4.根据权利要求1所述的一种高透氧超柔软的硅水凝胶日抛透片的制备方法,其特征在于:所述甲基丙烯酸羟乙酯使用前用4A分子筛浸泡干燥,并做减压蒸馏。
5.根据权利要求1所述的一种高透氧超柔软的硅水凝胶日抛透片的制备方法,其特征在于:所述羟基烷基封端的聚二甲基硅氧烷使用前在真空下干燥不少于五小时,温度约为六十度。
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