CN113103697B - 一种氟硅水凝胶彩色隐形眼镜及其制备工艺 - Google Patents
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Abstract
本发明涉及一种氟硅水凝胶彩色隐形眼镜及其制备工艺,包括以下步骤:用移印法将打底层转移到阳模的表面作为第一层,然后将油墨移印到经固化的打底层上,固化,再将氟硅水凝胶聚合液加入模具中,成型固化形成彩色隐形眼镜。其中,打底层主要包括氟硅氧烷预聚物一,油墨主要包括氟硅氧烷预聚物二及颜料,还包括各种助剂。本发明的氟硅水凝胶彩色隐形眼镜解决了镜片打底层透氧系数偏低、油墨易散色以及油墨树脂与镜片不兼容的问题。
Description
技术领域
本发明涉及软性角膜接触镜领域,尤其涉及一种氟硅水凝胶彩色隐形眼镜及其制备工艺。
背景技术
隐形眼镜分为硬性和软性隐形眼镜,其中,软性隐形眼镜的材质有两种:水凝胶和硅水凝胶。水凝胶是一类极为亲水的三维网络结构凝胶,在水中迅速溶胀并在此溶胀状态可以保持大量体积的水而不溶解;硅水凝胶是一种有机高分子材料,有亲水性,具有氧气和水的双通道。
各种各样水凝胶彩色隐形眼镜的制备方法被公开,基本都是包含至少一种颜料、具有相同官能团(例如:—COOH,—OH,—NH—R等)的粘合剂聚合物、稀释剂和附着促进剂,但适合硅水凝胶彩色隐形眼镜的生产工艺发展仍不完善。CN103091730B中公开了一种生产硅水凝胶彩色隐形眼镜的工艺,通过在粘结树脂中引入硅氧烷来达到目的。而生产硅水凝胶彩色隐形眼镜的工艺方法套用到氟硅水凝胶上会出现镜片不兼容的情况,主要表现为:所得彩色隐形眼镜镜片光学区透明度下降,移印可选择颜色少,多色移印时出现图案分辨率下降的现象。
另外,生产彩色隐形眼镜常用“三明治”工艺,顾名思义,三明治夹层的镜片为三层,油墨层被包覆在镜片中间层的中心位置,因此不存在色素脱落的潜在危险,为佩戴者的健康提供了保障。Dk指透氧系数,是表示隐形眼镜透氧量的重要指标,D是氧在镜片材料中的扩散系数,k是氧在该材料中的溶解系数,Dk指D*k的值。“三明治”工艺中,打底层必须具备高透氧,才不会对整个镜片的透氧系数产生影响。同时,油墨层的色素容易散色染到镜片其它部分。
因此仍需一种氟硅水凝胶隐形眼镜的制造方法解决油墨与镜片不兼容的问题,以及找到一种适合氟硅水凝胶的不散色油墨,同时解决“三明治”工艺中打底层透氧系数偏低的方法。
发明内容
为解决上述技术问题,本发明提供了一种适合氟硅水凝胶彩色隐形眼镜的全模压生产工艺,解决了打底层透氧系数偏低、油墨易散色以及油墨树脂与镜片不兼容的问题。
本发明的一种氟硅水凝胶彩色隐形眼镜的制备工艺,包括以下步骤:
(1)将分别含有通式I、II的氟硅氧烷聚合单体a、b,[甲基丙烯氧基(3-二甲硅基)丙基]封端正丁基封端聚(甲基-三氟丙基硅氧烷)、亲水聚合物、稀释剂、交联剂一和引发剂混合搅拌,加热,得到氟硅氧烷预聚物一,即打底层;
本发明的打底层中引入大分子的氟硅氧烷聚合单体,使打底层具有和镜片层接近的透氧系数,含氟组分提高氧在材料中的溶解能力的同时还可改善抗沉淀性,弥补有机硅材料亲脂性的缺点。
(2)将分别含有通式I、II的氟硅氧烷聚合单体a、b,亲水单体一,稀释剂,交联剂二、链转移剂和引发剂混合搅拌,加热,得到氟硅氧烷预聚物二,然后加入颜料研磨,最后加入固化促进剂,混合均匀得到油墨;
本发明的油墨层树脂中含有—NH、—COOH、—COO-、—HSO3-等锚固基团,这些极性基团能通过离子键、氢键以及范德华力等相互作用紧紧地吸附于色料表面,使油墨在移印过程中不易散色,提高花纹清晰度。
(3)将步骤(1)得到的氟硅氧烷预聚物一移印至阳模上,固化,再将步骤(2)得到的油墨移印至经固化的打底层上,固化;
(4)将氟硅水凝胶聚合液注入阴模,固化;其中,氟硅水凝胶聚合液由通式I所示的氟硅氧烷聚合单体a、通式II所示的氟硅氧烷聚合单体b、[甲基丙烯氧基(3-二甲硅基)丙基]封端正丁基封端聚(甲基-三氟丙基硅氧烷)、亲水单体二和助剂加入模具中发生聚合反应得到;
本发明在油墨层中引入与聚合液相同的单体,使油墨树脂与镜片材质相容。
(5)水化,脱模,得到镜片;
其中,通式I-II如下:
其中,R1和R3分别独立地选自氢或甲基;
进一步地,亲水单体一选自N-乙烯基吡咯烷酮、2-羟乙基丙烯酸酯、甲基丙烯酸、单甲醚二乙二醇甲基丙烯酸酯和2-甲基-2-丙烯酸-2-磺乙酯中的至少两种,优选甲基丙烯酸和2-甲基-2-丙烯酸-2-磺乙酯。
进一步地,亲水单体一的其中之一为2-甲基-2-丙烯酸-2-磺乙酯时,2-甲基-2-丙烯酸-2-磺乙酯与其它亲水单体一的质量比为1-2:1。2-甲基-2-丙烯酸-2-磺乙酯对颜料的包裹和吸附作用更强。
进一步地,在步骤(1)中,以氟硅氧烷预聚物一的总重为基准,各组分的含量为:通式I所示的氟硅氧烷聚合单体a 5-10%、通式II所示的氟硅氧烷聚合单体b 5-10%、[甲基丙烯氧基(3-二甲硅基)丙基]封端正丁基封端聚(甲基-三氟丙基硅氧烷)10-20%、亲水聚合物20-35%、稀释剂35-50%、交联剂一0.5-1.5%和引发剂0.5-1.5%。
进一步地,在步骤(1)中,交联剂一为二甲基丙烯酸乙二醇酯。
进一步地,在步骤(2)中,以油墨的总重为基准,各组分的含量为:通式I所示的氟硅氧烷聚合单体a 4-10%、通式II所示的氟硅氧烷聚合单体b 4-10%、亲水单体一15-30%、稀释剂25-45%、交联剂二4-10%、链转移剂4-10%、引发剂0.5-1.5%、颜料5-10%和固化促进剂2-5%。
进一步地,在步骤(2)中,交联剂二为N-[2-(2-甲基丙-2-烯基氨基)乙基]氨基甲酸乙酯。
进一步地,在步骤(4)中,以氟硅水凝胶聚合液的总重为基准,各组分的含量为:通式I所示的氟硅氧烷聚合单体a 10-15%、通式II所示的氟硅氧烷聚合单体b 10-20%、[甲基丙烯氧基(3-二甲硅基)丙基]封端正丁基封端聚(甲基-三氟丙基硅氧烷)15-25%、亲水单体二40-60%和助剂1-5%。
进一步地,在步骤(4)中,亲水单体二选自N-乙烯基吡咯烷酮、N,N-二甲基丙烯酰胺、2-羟乙基丙烯酸酯、N-乙烯基乙酰胺和单甲醚二乙二醇甲基丙烯酸酯中的至少两种。
进一步地,稀释剂为乙二醇单乙醚。
进一步地,引发剂为偶氮二异丁腈。
进一步地,在步骤(1)中,亲水聚合物为聚乙烯吡咯烷酮PVP,k值为30。k值指粘度或平均聚合度,表示聚合物分子量大小。
进一步地,在步骤(2)中,链转移剂选自2-巯基乙醇、十二烷基硫醇、烯丙基醚类和2,4-二苯基-4-甲基-1-戊烯中的一种或多种,优选2,4-二苯基-4-甲基-1-戊烯。
进一步地,在步骤(2)中,固化促进剂为二异氰酸酯化合物,优选2,4-甲苯二异氰酸酯。
进一步地,在步骤(2)中,颜料为粒径大小为5μm或更小的粉末。
进一步地,在步骤(3)中,模具的阳模材质为PBT。
进一步地,在步骤(3)中,打底层的固化条件:40-60℃,20-40min。
进一步地,在步骤(3)中,油墨层移印后固化条件:40-60℃,1-1.5h。
进一步地,在步骤(4)中,模具的阴模材质为PP。
进一步地,在步骤(4)中,氟硅水凝胶配方含水量为45-55%。
进一步地,在步骤(5)中,水化条件为乙醇水溶液,优选20%乙醇水溶液脱模,80%乙醇水溶液萃取。
本发明还要求保护上述制备工艺制备的氟硅水凝胶彩色隐形眼镜。
借由上述方案,本发明至少具有以下优点:
(1)本发明根据氟硅水凝胶中的单体成分,通过引入一样的单体,解决了油墨树脂与镜片材质不兼容的问题。
(2)本发明的油墨层引入大量具有锚固基团的单体,以达到油墨不散色的效果。
(3)本发明的打底层引入大分子的氟硅氧烷聚合单体,透氧性能好,增强了佩戴舒适度。
上述说明仅是本发明技术方案的概述,为了能够更清楚了解本发明的技术手段,并可依照说明书的内容予以实施,以下以本发明的较佳实施例说明如后。
具体实施方式
下面结合具体实施例对本发明作进一步说明,以使本领域的技术人员可以更好地理解本发明并能予以实施,但所举实施例不作为对本发明的限定。
实施例
(1)氟硅氧烷预聚物一的制备:
取2-[3-[甲基双(三氟甲基硅氧基)硅基]丙基氨甲酰氧基]2-甲基丙基-2-烯酸乙酯(氟硅氧烷聚合单体a),羟基-3-[3-三(三氟甲基硅氧基)硅丙基氨基]丙基]2-甲基丙基-2-烯酸乙酯(氟硅氧烷聚合单体b),[甲基丙烯氧基(3-二甲硅基)丙基]封端正丁基封端聚(甲基-三氟丙基硅氧烷)(氟硅氧烷聚合单体c),PVPK30(亲水聚合物),乙二醇单乙醚(稀释剂),二甲基丙烯酸乙二醇酯EGDMA(交联剂)和偶氮二异丁腈AIBN(引发剂),搅拌均匀后,将混合液置入65℃的恒温水浴锅中加热6h。然后降至20℃加入阻聚剂对苯二酚单甲醚MEHQ:0.05g,真空下除去多余的乙二醇单乙醚,得到无色粘稠拉丝状液体。氟硅氧烷预聚物一中各物质用量见表1(单位:g)。
表1氟硅氧烷预聚物一中各物质用量
(2)氟硅氧烷预聚物二粘结树脂的制备:
取2-[3-[甲基双(三氟甲基硅氧基)硅基]丙基氨甲酰氧基]2-甲基丙基-2-烯酸乙酯(氟硅氧烷聚合单体a),羟基-3-[3-三(三氟甲基硅氧基)硅丙基氨基]丙基]2-甲基丙基-2-烯酸乙酯(氟硅氧烷聚合单体b),甲基丙烯酸(亲水单体一1),2-甲基-2-丙烯酸-2-磺乙酯(亲水单体一2),再加入乙二醇单乙醚(稀释剂),N-[2-(2-甲基丙-2-烯基氨基)乙基]氨基甲酸乙酯(交联剂),最后加入AIBN(引发剂),2,4-二苯基-4-甲基-1-戊烯(链转移剂)。搅拌均匀后,将混合液置入60℃恒温水浴锅中加热24h。得到无色粘稠液体。氟硅氧烷预聚物二中各物质用量见表2(单位:g)。
表2氟硅氧烷预聚物二中各物质用量
(3)油墨的制备:
取(2)中得到的氟硅氧烷预聚物二和颜料加入球磨机研磨30min,得到细腻无颗粒的油墨。最后,加入2,4-甲苯二异氰酸酯(固化促进剂),混合均匀得到可移印油墨。不同颜色油墨中各物质及用量见表3(单位:g)。
表3不同颜色中各物质及用量
(4)打底层移印固化,油墨层移印固化:
用移印机将(1)得到的氟硅氧烷预聚物一移印到PBT阳模上。阳模入烘箱50℃烘烤30min,使打底层半固化。再用移印机将(3)得到的黑色油墨移印到PBT阳模上。阳模入烘箱50℃烘烤60min,得到花纹固化的阳模。
移印方法:取制得的彩色油墨涂布于一块刻蚀有图案的不锈钢板上,由一把光滑墨刀较快地把油墨刮过刻蚀槽,使刻蚀槽内嵌满油墨,然后用橡皮印把图案转移压印到隐形眼镜片表面上与眼球虹膜对应的区域。所用刻蚀有图案的不锈钢板为圆环状,其面积大于镜片上的彩色图案花纹。
(5)彩色隐形眼镜镜片的制备:
将配好的氟硅水凝胶聚合液通过注液机注入PP阴模,再与(4)得到的花纹已固化的阳模一起,合模固化得到镜片。
氟硅水凝胶聚合液配制:在500mL的单口瓶中依次加入下述物料:2-[3-[甲基双(三氟甲基硅氧基)硅基]丙基氨甲酰氧基]2-甲基丙基-2-烯酸乙酯(氟硅氧烷聚合单体a):12g;羟基-3-[3-三(三氟甲基硅氧基)硅丙基氨基]丙基]2-甲基丙基-2-烯酸乙酯(氟硅氧烷聚合单体b):15g;[甲基丙烯氧基(3-二甲硅基)丙基]封端正丁基封端聚(甲基-三氟丙基硅氧烷)(氟硅氧烷聚合单体c):20g;N-乙烯基吡咯烷酮(亲水单体二1):20g;N,N,-二甲基丙烯酰胺(亲水单体二2):15g;2-乙烯基羰基氧基乙基2-甲基丙-2-烯酸酯(交联剂):2g;偶氮二异丁腈(引发剂):0.5g;2-丙烯酸2-(4-苯甲酰-3-羟基苯氧基)乙基酯(紫外吸收剂):0.5g。25℃下搅拌使物料全部溶解,混合均匀,搅拌时间1h。所得混合液经过0.2微米孔径的压滤器过滤,得到氟硅水凝胶聚合液。
(6)成品镜片:
用模具分离机将阴模分离(镜片保留在阳模上),镜片经乙醇水溶液水化,萃取,灭菌得到最终镜片。
对油墨进行测试:
将所得镜片浸入5毫升无水乙醇中,超声处理90s。然后将其置于硼酸盐缓冲生理盐水中,平衡30min后,再次将镜片置入新鲜的硼酸盐缓冲生理盐水中平衡30min,检查是否有着色剂渗出、模糊或分层现象,若无此现象视为合格。不同颜色镜片参数见表4。
表4不同颜色镜片参数
其中,Dk单位为10-11(cm2/s)[mLO2/(mL.mmHg)]。
由表4可以看出,本发明制备的彩色隐形眼镜的透氧系数达到150左右,移印花纹清晰,均无着色剂渗出、模糊或分层现象。
显然,上述实施例仅仅是为清楚地说明所作的举例,并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本发明创造的保护范围之中。
Claims (7)
1.一种氟硅水凝胶彩色隐形眼镜的制备工艺,其特征在于,包括以下步骤:
(1)将分别含有通式I、II的氟硅氧烷聚合单体a、b,[甲基丙烯氧基(3-二甲硅基)丙基]封端正丁基封端聚(甲基-三氟丙基硅氧烷)、亲水聚合物、稀释剂、交联剂一和引发剂混合搅拌,加热,得到氟硅氧烷预聚物一;
(2)将分别含有通式I、II的氟硅氧烷聚合单体a、b,亲水单体一,稀释剂,交联剂二、链转移剂和引发剂混合搅拌,加热,得到氟硅氧烷预聚物二,然后加入颜料研磨,最后加入固化促进剂,混合均匀得到油墨;其中,以油墨的总重为基准,各组分的含量为:通式I所示的氟硅氧烷聚合单体a 4-10%、通式II所示的氟硅氧烷聚合单体b 4-10%、亲水单体一15-30%、稀释剂25-45%、交联剂二4-10%、链转移剂4-10%、引发剂0.5-1.5%、颜料5-10%和固化促进剂2-5%,所述交联剂二为N-[2-(2-甲基丙-2-烯基氨基)乙基]氨基甲酸乙酯;
(3)将步骤(1)得到的氟硅氧烷预聚物一移印至阳模上,固化,再将步骤(2)得到的油墨移印至经固化的氟硅氧烷预聚物一上,固化;
(4)将氟硅水凝胶聚合液注入阴模,固化;其中,所述氟硅水凝胶聚合液由通式I所示的氟硅氧烷聚合单体a、通式II所示的氟硅氧烷聚合单体b、[甲基丙烯氧基(3-二甲硅基)丙基]封端正丁基封端聚(甲基-三氟丙基硅氧烷)、亲水单体二和助剂加入模具中发生聚合反应得到;其中,以氟硅水凝胶聚合液的总重为基准,各组分的含量为:通式I所示的氟硅氧烷聚合单体a 10-15%、通式II所示的氟硅氧烷聚合单体b 10-20%、[甲基丙烯氧基(3-二甲硅基)丙基]封端正丁基封端聚(甲基-三氟丙基硅氧烷)15-25%、亲水单体二40-60%和助剂1-5%;
(5)水化,脱模,得到镜片;
其中,所述通式I-II如下:
其中,R1和R3分别独立地选自氢或甲基;
2.根据权利要求1所述的制备工艺,其特征在于:所述亲水单体一选自N-乙烯基吡咯烷酮、2-羟乙基丙烯酸酯、甲基丙烯酸、单甲醚二乙二醇甲基丙烯酸酯和2-甲基-2-丙烯酸-2-磺乙酯中的至少两种。
3.根据权利要求2所述的制备工艺,其特征在于:亲水单体一的其中之一为2-甲基-2-丙烯酸-2-磺乙酯时,2-甲基-2-丙烯酸-2-磺乙酯与其它亲水单体一的质量比为1-2:1。
4.根据权利要求1所述的制备工艺,其特征在于:在步骤(1)中,以氟硅氧烷预聚物一的总重为基准,各组分的含量为:通式I所示的氟硅氧烷聚合单体a 5-10%、通式II所示的氟硅氧烷聚合单体b 5-10%、[甲基丙烯氧基(3-二甲硅基)丙基]封端正丁基封端聚(甲基-三氟丙基硅氧烷)10-20%、亲水聚合物20-35%、稀释剂35-50%、交联剂一0.5-1.5%和引发剂0.5-1.5%。
5.根据权利要求1所述的制备工艺,其特征在于:在步骤(1)中,所述交联剂一为二甲基丙烯酸乙二醇酯。
6.根据权利要求1所述的制备工艺,其特征在于:在步骤(4)中,亲水单体二选自N-乙烯基吡咯烷酮、N,N-二甲基丙烯酰胺、2-羟乙基丙烯酸酯、N-乙烯基乙酰胺和单甲醚二乙二醇甲基丙烯酸酯中的至少两种。
7.一种权利要求1-6任一项所述的制备工艺制备的氟硅水凝胶彩色隐形眼镜。
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