CN116854958B - 一种防蓝光光致变色镜片基片的制备方法 - Google Patents
一种防蓝光光致变色镜片基片的制备方法 Download PDFInfo
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Abstract
一种防蓝光光致变色镜片基片的制备方法,该方法包括将热固性或热塑性光学树脂单体25~100重量份、稀释剂0~0.8重量份、光致变色材料0.6~3重量份、固化剂0.5~3重量份、卟吩金属络合物0.1~1重量份和喹酞酮化合物0.2~0.8重量份制成镜片基材混料,然后浇筑在模具中,通过程序升温固化成型。该方法制备的镜片能实现对室内LED光源高能蓝光防护与户外光照变色后紫外线防护双功能。由卟吩金属络合物和喹酞酮化合物复配的蓝光吸收材料,在保持高透光率的前提下,对400‑435nm光谱区高能蓝光有特征吸收,且对紫外光有部分透过,不影响光致变色材料在强光下的的变色功能,耐候性佳。
Description
技术领域
本发明涉及一种防蓝光光致变色树脂镜片基片的制备方法,具体涉及一类在400-435nm光谱区对高能蓝光有效吸收的光致变色树脂镜片基片的制备方法,属于树脂镜片制造技术领域。
背景技术
白光LED作为显示器件背光系统的显示制造技术成为现有电子显示技术的主流产品技术,此类显示屏幕被广泛应用于移动通讯终端设备、计算机设备、家用及商用显示设备及娱乐设备等。因白光LED所带来的蓝光危害和“富蓝化”的光生物安全问题是该类显示屏幕的重大技术缺陷。白光LED的光辐射危害主要表现为峰值在435nm左右的短波长高能蓝光会引起视网膜光化学损伤和色素上表皮细胞的凋亡。短波蓝光具有较高的能量和较强的组织穿透能力,对于哺乳动物的生物光敏基团具有确定的破坏作用,可造成视网膜病变。病理研究证实白光LED中的高能蓝光在年龄相关性黄斑变性形成机制中起到一定的加速作用。由于儿童的视网膜黄斑对蓝光的吸收能力弱,同样的光照强度下,透过的蓝光辐射量约为成年人的两倍,蓝光辐射对儿童视网膜危害更甚。处于生长发育期的低龄人群若长期处于高能蓝光照明环境,轻者诱发致盲眼病,重者造成终身视力低下。
紫外线区约占太阳总辐射能量的7%,户外活动过量的紫外线辐照会引起生物组织光化学反应,尤其对人类的皮肤、眼睛以及免疫系统等均会造成伤害。人眼是对紫外线最敏感的部位,紫外线长期、多次暴晒,可引起急性结膜炎、视网膜疾病,紫外线辐射同时也是老年性白内障的重要诱因。
因而保护视力、捍卫眼睛健康的功能性防护镜片现已成为镜片市场的高利润产品。针对户外活动强光环境下的光致变色镜片的开发技术已成熟稳定,各类浅底色无底色变色太阳镜产品销售多年获得市场认可;针对室内暗光环境中的高能蓝光防护眼镜也已成为镜片市场的热门产业;在此基础上,结合接触电子显示设备人员的高能蓝光防护需求,近年来出现了同时具有户外光致变色与室内高能蓝光防护双功能的创新眼镜产品。
人眼对400-440nm范围蓝光的视物和辨色不敏感,且该波段光波波长短能量高,对眼睛伤害大为有害蓝光,高能蓝光防护镜片对这部分蓝光应保持低透过率;440-500nm范围为中长波蓝光对人眼伤害相对较小,且可以有效调节人体生物节律与视神经反馈作用,使人眼对观测物体的色彩判断保持准确,对这部分蓝光应保持一定的透过率。
光致变色镜片亦称为“感光镜片”,是根据光色互变可逆的分子反应机理,镜片在室内光线和室外光线切换时,在室外光线中的紫外线照射下,可迅速变暗阻挡强光并吸收紫外线但对可见光透过不吸收;转回室内低紫外线或无紫外线环境中,镜片可迅速褪色恢复无色透明状态保证镜片的透光度。因此光致变色镜片于室内室外使用均可,能够有效防止阳光、紫外光、眩光对眼睛的伤害。
将光致变色镜片与蓝光防护功能结合主要的技术难题在于现有使用量最大的各类有机蓝光吸收防护材料在紫外光区,特别是在可引发光致变色材料变色的特定紫外光谱区存在一定的光谱吸收,将其与光致变色材料共混后生产防蓝光光致变色镜片将倍数级增大光致变色材料的添加量,极大提升了制造成本;且影响作为变色镜片功能时的变色与褪色速度,表现为变色强度低,褪色不彻底存在底色,给消费者带来较差的使用体验。
因此,在保证对高能蓝光有效吸收的前提下,寻找开发在紫外光区无吸收、工业化生产加工成本较低、具备高耐候性的有机蓝光吸收材料应用于防蓝光光致变色镜片和防蓝光膜片产品具有明显的商业价值。
发明内容
针对现有技术的上述问题,本发明提供一种含有复配蓝光吸收材料和光致变色材料的防蓝光光致变色镜片基片的制备方法,该方法制备的镜片基片可实现对室内LED光源高能蓝光防护与户外光照变色后紫外线防护双功能。由卟吩金属络合物和喹酞酮化合物复配的蓝光吸收材料,在保持高透光率的前提下,对400-435nm光谱区高能蓝光有特征吸收,且对紫外光有部分透过,不影响光致变色材料在强光下的的变色功能,耐候性佳。
为实现上述目的,本发明包括如下技术方案:
一种防蓝光光致变色镜片基片的制备方法,包括如下步骤:
I.基材配料
按照以下成分和配比准备基材配料:热固性或热塑性光学树脂单体25~100重量份、稀释剂0~0.8重量份、光致变色材料0.6~3重量份、固化剂0.5~3重量份、卟吩金属络合物0.1~1重量份和喹酞酮化合物0.2~0.8重量份;
该卟吩金属络合物选自以下结构的至少一种:A型,八乙基卟吩锌;B型,八乙基卟吩镍;C型,5,10,15,20-四(五氟苯基)卟吩锌;D型,四苯基卟吩锌;
该喹酞酮化合物的结构式如下:
II.制备镜片基材混料
a.制备丙烯酸酯类基材采用以下操作:将上述各基材配料除固化剂外准确称量,混合后搅拌直至完全溶解,保持温度在20~30℃加入固化剂,搅拌1~2小时使其均匀混合,即制得镜片基材混料;
b.制备聚氨酯树脂类基材采用以下操作:将上述各基材配料除固化剂外准确称量,混合后搅拌直至完全溶解,加入固化剂,在30-40℃温度下密封搅拌,冰水降温至15-20℃,真空搅拌,真空度为-0.09MPa,停止搅拌后至室温,即制得镜片基材混料。
III.浇筑成型
将镜片基材混料脱泡后,保持料温为15-30℃,惰性气体加压条件下通<0.1μm孔径四氟乙烯滤网过滤后,通过加料装置注入镜片模具中,在计算机控温的固化炉中程序升温固化成型,降温至70-80℃脱模具,即可制得镜片基片。
如上所述的制备方法,优选地,所述步骤III程序升温操作是在18~22小时内从室温程序升温至95~100℃,然后保持该温度1.5~2.0小时,完成固化成型。
如上所述的制备方法,优选地,所述步骤I按照以下成分和配比准备基材配料:热固性或热塑性光学树脂材料50~100重量份、稀释剂0~0.6重量份、光致变色材料0.6~2.5重量份、固化剂0.5~3重量份、卟吩金属络合物0.1~1重量份和喹酞酮化合物0.2~0.8重量份。
如上所述的制备方法,优选地,所述热固性或热塑性光学树脂单体选自间苯二亚甲基二异氰酸酯、苯乙烯、甲基丙烯酸、聚乙二醇二甲基丙烯酸酯、季戊四醇四丙烯酸酯、乙氧化壬基酚丙烯酸酯、环氧丙烯酸酯、双酚A环氧丙烯酸酯、甲基苯乙烯、聚丙烯酸酯、乙氧化双酚A二丙烯酸酯和甲基丙烯酸丁酯中的一种或多种。
如上所述的制备方法,优选地,所述固化剂选自二月桂酸二丁基锡、过氧化二碳酸二异丙酯、过氧化-2-乙基己基碳酸叔丁酯、1,1′-偶氮(氰基环己烷)、偶氮二甲酸二异丙酯、偶氮二异庚腈、偶氮二异丁酸二甲酯、偶氮二异丁酸二乙酯、异丙苯过氧化氢、叔丁基过氧化氢中的一种或多种。
如上所述的制备方法,优选地,所述光致变色材料为螺吡喃类和/或螺噁嗪类光致变色材料。
如上所述的制备方法,优选地,所述光致变色材料为N-(β-羟乙基)-3,3-二甲基-6-硝基螺吲哚啉苯并吡喃、1,3,3-三甲基吲哚-6-硝基苯并二氢吡喃并螺烷和/或1,3,3-三甲基吲哚-β-萘基二氢呋喃。
如上所述的制备方法,优选地,所述稀释剂为甲苯、二甲苯、甲基丙烯酸烷基酯、甲基丙烯酸羟乙酯、季戊四醇、乙二醇、丙二醇、丁二醇、己二醇、新戊二醇、正丁醇、三羟甲基丙烷中的一种或多种的混合物。
本发明的有益效果在于以下几个方面:
1.本发明将现有技术所使用的二苯甲酮类、苯并三氮唑类或烷基吲哚类等常规有机小分子蓝光吸收剂替换为具有吸收选择性的卟吩配合物和喹酞酮复合蓝光吸收材料。该复合蓝光吸收材料在紫外光谱区有一定透过,保证光致变色所需的紫外辐射强度,避免了防蓝光材料对光致变色材料的变色干扰;同时,在保持高透光率的前提下,对400-435nm光谱区高能蓝光有特征吸收,实现对室内LED光源高能蓝光防护与户外光照变色后紫外线防护双功能。
2.与现有技术比较,更少添加量条件下,本发明采用的复合蓝光吸收材料防蓝光效果显著,对于400-435nm波长的蓝光的平均截止率达到80%以上,且光致变色材料添加量也相对减少50%以上,降低了生产成本,对镜片的各项物理性能影响较小。
3.本发明制备的防蓝光光致变色镜片光稳定性强、耐候性佳。解决了现有防蓝光光致变色树脂镜片生产技术中存在的变色强度低、褪色不彻底的问题,可广泛应用于汽车车窗、光学防护玻璃、LED灯防护膜、手机防护屏、眼科防护装备等领域,解决紫外线与LED光源有害高能蓝光对人眼造成的伤害。
附图说明
图1为实施例2制备的镜片光谱透射比曲线图。
图2为对比例1制备的镜片光谱透射比曲线图。
图3为对比例2制备的镜片光谱透射比曲线图。
图4为对比例3和对比例4制备的镜片光谱透射比对比曲线图。
图5为对比例5制备的镜片光谱透射比曲线图。
图6为对比例6制备的镜片光谱透射比曲线图。
图7为对比例7制备的镜片光谱透射比曲线图。
图8为对比例8制备的镜片光谱透射比曲线图。
图9为对比例9制备的镜片光谱透射比曲线图。
具体实施方式
以下通过具体的实施例对本发明的内容作进一步详细的说明。实施例和对比例中所用的原料、试剂或装置如无特殊说明,均可从常规商业途径得到,或者可以通过现有技术方法得到。除非特别说明,试验或测试方法均为本领域的常规方法。本发明的实施方式并不受以下实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
以下实施例中部分原料的来源如下:
八乙基卟吩锌(A型):江苏视科新材料股份有限公司,商品名:SK408
八乙基卟吩镍(B型):江苏视科新材料股份有限公司,商品名:SK316
5,10,15,20-四(五氟苯基)卟吩锌(C型):江苏视科新材料股份有限公司,商品名:SK318
四苯基卟吩锌(D型):江苏视科新材料股份有限公司,商品名:SK320
N-(β-羟乙基)-3,3-二甲基-6-硝基螺吲哚啉苯并吡喃:江苏视科新材料股份有限公司,商品名:兰274
1,3,3-三甲基吲哚-6-硝基苯并二氢吡喃并螺烷:江苏视科新材料股份有限公司,商品名:兰275
1,3,3-三甲基吲哚-β-萘基二氢呋喃:江苏视科新材料股份有限公司,商品名:兰276
式I所示的喹酞酮化合物,根据中国专利号:ZL 201710101651.3所述方法制备。
实施例1防蓝光光致变色镜片(一)
I.制备A型防蓝光变色复合树脂
称取聚乙二醇二甲基丙烯酸酯1500g,然后加入A型卟吩金属络合物8g,喹酞酮(式I)7g,N-(β-羟乙基)-3,3-二甲基-6-硝基螺吲哚啉苯并吡喃光致变色材料20g和二甲苯稀释剂0.4g,加入间苯二亚甲基二异氰酸酯(XDI)500g和偶氮二甲酸二异丙酯固化剂15g,在40℃温度下密封搅拌30分钟。冰水降温至18℃,真空搅拌60分钟,真空度为-0.09MPa,停止搅拌后至室温,得到含A型蓝光吸收剂的光致变色复合树脂。
II.制备防蓝光光致变色基片
将含A型蓝光吸收剂的光致变色复合树脂超声脱泡后,保持料温为20℃,经氮气增压通过孔径为0.1μm的聚四氟乙烯滤网过滤后注入镜片模具中,放入计算机控温的固化炉中程序升温固化成型。热固化温度曲线如下:40℃保温8小时,在6小时内均匀升温至65℃,继续升温4小时至100℃并恒温2小时,在1小时内降温至70℃,完成固化,获得(聚氨酯类)树脂防蓝光光致变色基片。
实施例2防蓝光光致变色镜片(二)
I.制备B型防蓝光变色复合树脂
称取甲基苯乙烯25g、聚丙烯酸酯25g、乙氧化双酚A二丙烯酸酯25g、甲基丙烯酸丁酯25g,然后加入B型卟吩金属络合物0.3g,喹酞酮(式I)0.25g,1,3,3-三甲基吲哚-6-硝基苯并二氢吡喃并螺烷光致变色材料1.2g,1,3,3-三甲基吲哚-β-萘基二氢呋喃光致变色材料0.8g,二甲苯稀释剂0.4g加入锥形瓶中搅拌1小时,加入偶氮二异庚腈固化剂2.0g在室温下抽真空30分钟,在此过程中不断搅拌混合均匀。再将温度控制在35℃,搅拌速率500r/min,静置抽真空90分钟。得到含B型蓝光吸收剂的光致变色复合树脂。
II.制备防蓝光光致变色镜片基片
将含B型蓝光吸收剂的光致变色复合树脂混料超声脱泡后,保持料温为20℃(具体温度),经过0.1μm的聚四氟乙烯滤网过滤器自然过滤后注入镜片模具中密封,在计算机控温的固化炉中经过20小时从室温程序升温至100℃,程序升温曲线:①0~4h保持35℃;②4~12h匀速升至60℃;③12~18h匀速升至100℃;④18~20h保持100℃;⑤冷却至70℃后开模得到,获得(丙烯酸酯类)树脂防蓝光光致变色基片。
实施例3防蓝光光致变色镜片(三)
I.制备C型防蓝光变色复合树脂
称取甲基苯乙烯25g、聚丙烯酸酯25g、乙氧化双酚A二丙烯酸酯25g、甲基丙烯酸丁酯25g,然后加入C型卟吩金属络合物0.5g,喹酞酮(式I)0.35g,1,3,3-三甲基吲哚-6-硝基苯并二氢吡喃并螺烷光致变色材料1.0g,1,3,3-三甲基吲哚-β-萘基二氢呋喃光致变色材料0.5g,二甲苯稀释剂0.4g加入锥形瓶中搅拌1小时,加入偶氮二异庚腈固化剂2.0g在室温下抽真空30分钟,在此过程中不断搅拌混合均匀。再将温度控制在35℃,搅拌速率500r/min,静置抽真空90分钟。得到含C型蓝光吸收剂的光致变色复合树脂。
II.制备防蓝光光致变色镜片基片
将含C型蓝光吸收剂的光致变色复合树脂超声脱泡后,保持料温为20℃(具体温度),经过0.1μm的聚四氟乙烯滤网过滤器自然过滤后注入镜片模具中密封,在计算机控温的固化炉中经过20小时从室温程序升温至100℃,程序升温曲线:①0~4h保持35℃;②4~12h匀速升至60℃;③12~18h匀速升至100℃;④18~20h保持100℃;⑤冷却至70℃后开模得到,获得(丙烯酸酯类)树脂防蓝光光致变色基片,清洗干燥。
实施例4防蓝光光致变色镜片(四)
I.制备D型防蓝光变色复合树脂
称取甲基苯乙烯25g、聚丙烯酸酯25g、乙氧化双酚A二丙烯酸酯25g、甲基丙烯酸丁酯25g,然后加入D型卟吩金属络合物1.0g,喹酞酮(式I)0.6g,1,3,3-三甲基吲哚-6-硝基苯并二氢吡喃并螺烷光致变色材料1.8g,1,3,3-三甲基吲哚-β-萘基二氢呋喃光致变色材料0.6g,二甲苯稀释剂0.4g加入锥形瓶中搅拌1小时,加入偶氮二异庚腈固化剂2.2g在室温下抽真空30分钟,在此过程中不断搅拌混合均匀。再将温度控制在35℃,搅拌速率500r/min,静置抽真空90分钟。得到含D型蓝光吸收剂的光致变色复合树脂。
II.制备防蓝光光致变色镜片基片
将含D型蓝光吸收剂的光致变色复合树脂超声脱泡后,保持料温为20℃(具体温度),经过0.1μm的聚四氟乙烯滤网过滤器自然过滤后注入镜片模具中密封,在计算机控温的固化炉中经过20小时从室温程序升温至100℃,程序升温曲线:①0~4h保持35℃;②4~12h匀速升至60℃;③12~18h匀速升至100℃;④18~20h保持100℃;⑤冷却至70℃后开模得到,获得(丙烯酸酯类)树脂防蓝光光致变色基片,清洗干燥。
实施例5防蓝光光致变色镜片(五)
I.制备A型防蓝光变色复合树脂
称取甲基苯乙烯25g、聚丙烯酸酯25g、乙氧化双酚A二丙烯酸酯25g、甲基丙烯酸丁酯25g,然后加入A型卟吩金属络合物0.8g,喹酞酮(式I)0.5g,1,3,3-三甲基吲哚-6-硝基苯并二氢吡喃并螺烷光致变色材料0.8g,1,3,3-三甲基吲哚-β-萘基二氢呋喃光致变色材料0.2g,二甲苯稀释剂0.4g加入锥形瓶中搅拌1小时,加入偶氮二异庚腈固化剂2.2g在室温下抽真空30分钟,在此过程中不断搅拌混合均匀。再将温度控制在35℃,搅拌速率500r/min,静置抽真空90分钟。得到含A型蓝光吸收剂的光致变色复合树脂。
II.制备防蓝光光致变色镜片基片
将含A型蓝光吸收剂的光致变色复合树脂超声脱泡后,保持料温为20℃,经过0.1μ0m的聚四氟乙烯滤网过滤器自然过滤后注入镜片模具中密封,在计算机控温的固化炉中经过20小时从室温程序升温至100℃,程序升温曲线:①0~4h保持35℃;②4~12h匀速升至60℃;⑦12~18h匀速升至100℃;④18~20h保持100℃;④冷却至70℃后开模得到,获得丙烯酸酯类树脂防蓝光光致变色基片,清洗干燥。
对比例1-9
对比例1-9分别采用对应实施例的制备条件,只是更换了蓝光吸收剂,或者减少某些组分,具体配方条件详见表1。各对比例蓝光吸收剂总量与对应实施例的蓝光吸收剂总量相同,各对比例变色材料与对应实施例相同或不添加。
作为对比的市场广泛销售的传统蓝光吸收剂采用4,4-(1,4-亚苯基)双(1-(4-丁氧基苯基)-1,3-丙二酮(中国发明专利CN108191624A)。
表1不同配方条件下制备的对比例样品对比表
| 样品 | 市售蓝光吸收剂 | 卟吩金属络合物 | 喹酞酮 | 变色材料 | 对应实施例 |
| 对比例1 | 0.3g | / | 0.25g | √ | 实施例2 |
| 对比例2 | / | / | 0.55g | √ | 实施例2 |
| 对比例3 | / | 0.3g | 0.25g | / | 实施例2 |
| 对比例4 | / | 0.85g | / | / | 实施例3 |
| 对比例5 | / | 1.6g | / | √ | 实施例4 |
| 对比例6 | 0.5g | 0.8g | / | √ | 实施例5 |
| 对比例7 | 15g | / | / | √ | 实施例1 |
| 对比例8 | / | 0.85 | / | √ | 实施例3 |
| 对比例9 | / | / | 1.3g | / | 实施例5 |
实施例6:防蓝光光致变色镜片基片光致变色性能试验
(一)光致变色响应值试验
检测步骤及方法:被测样品在褪色状态下的光透射比tV(0)和经过光照时间(15min)变色状态下的光透射比tV(1)之间的比值,即:光致变色响应值=tV(0)÷tV(1),以确定被测样品在不同温度下的光致变色响应值。将太阳模拟器辐射强度衰减25%后,以中等光照强度照射样品,测试结果如图1-9所示,检测结果见表2。
(二)光致变色光谱响应时间检测
检测步骤及方法:将实施例1-5和对比例1-9制备的镜片基片分别放入测试箱子,打开太阳光模拟器光源,记录镜片从无色变成有色反应所需时间;照射10分钟后关闭模拟光源,记录镜片从有色到恢复无色状态所需时间,检测结果见表2。
表2检测样品光致变色响应值情况
结论:本发明制造的含有复配蓝光吸收材料的光学材料及镜片,对变色性能影响较小,具有光致变色响应时间短,光致变色响应值高等优点。
实施例7:防蓝光光致变色镜片基片光学性能试验
对实施例1-5和对比例1-9制备的树脂镜片基片分别进行光透射比(T/%)性能检测,选用上海元析仪器有限公司UV-8000紫外可见光光度计。检测方法:直接将实施例1-5和对比例1-8制备的树脂镜片涂在紫外可见光光度计的棱镜中测定透光率,波长范围为380~780nm的可见光区和波长范围为280~380nm的紫外光区,采用不同的发光体作为仪器的光源。代表波长透射比列于表3。
表3镜片样品光透射比检测情况表单位:T%
结果与讨论:
对比以上数据可知,对比例1中,卟吩络合物换成市场上普通的蓝光吸收剂,由于普通蓝光吸收剂同时吸收紫外光,导致光致变色材料紫外光吸收不足,变色时间长、变色效果低,达不到强光下快速变色防护的效果;
对比例2不含卟吩络合物仅含喹酞酮,在紫外区防护低于国标(GB10810.3-2006)要求(≤1%),紫外线防护项不合格;
对比例3由于未添加变色材料制品不变色,且335nm附近紫外区有透射;
对比例4只添加了卟吩络合物,不含喹酞酮和变色材料,335nm附近紫外区有较高透过率,435nm蓝光透射比高于实施例1-5;
对比例5未添加喹酞酮,在435nm蓝光透射比高于实施例1-5;
对比例6由于添加了部分市售蓝光吸收剂,未添加喹酞酮,导致变色效率低,435nm蓝光透射比较高;
对比例7市售蓝光吸收剂代替本发明复合蓝光吸收剂,导致变色效率较低,同时在435nm处透射比较高;
对比例8只添加了卟吩络合物,不含喹酞酮,435nm蓝光透射比较高;
对比例9仅含喹酞酮,不含卟吩络合物和变色材料,在335nm附近紫外区有较高透射比。
本发明所采用的卟吩金属络合物(A-D)和喹酞酮相结合,对400nm-435nm波长的蓝光可有效吸收,同时,不影响光致变色性能。
Claims (6)
1.一种防蓝光光致变色镜片基片的制备方法,其特征在于,该方法包括如下步骤:
I.基材配料
按照以下成分和配比准备基材配料:热固性或热塑性光学树脂单体50~100重量份、稀释剂0~0.6重量份、光致变色材料0.6~2.5重量份、固化剂0.5~3重量份、卟吩金属络合物0.1~1重量份和喹酞酮化合物0.2~0.8重量份;
该光致变色材料为螺吡喃类和/或螺噁嗪类光致变色材料;
该卟吩金属络合物选自以下结构的至少一种:A型,八乙基卟吩锌;B型,八乙基卟吩镍;C型,5,10,15,20-四(五氟苯基)卟吩锌;D型,四苯基卟吩锌;
该喹酞酮化合物的结构式如下:
II.制备镜片基材混料
a.制备丙烯酸酯类基材采用以下操作:将上述各基材配料除固化剂外准确称量,混合后搅拌直至完全溶解,保持温度在20~30℃加入固化剂,搅拌1~2小时使其均匀混合,即制得镜片基材混料;
b.制备聚氨酯树脂类基材采用以下操作:将上述各基材配料除固化剂外准确称量,混合后搅拌直至完全溶解,加入固化剂,在30-40℃温度下密封搅拌,冰水降温至15-20℃,真空搅拌,真空度为-0.09MPa,停止搅拌后至室温,即制得镜片基材混料;
III.浇注成型
将镜片基材混料脱泡后,保持料温为15-30℃,惰性气体加压条件下通<0.1μm孔径四氟乙烯滤网过滤后,通过加料装置注入镜片模具中,在计算机控温的固化炉中程序升温固化成型,降温至70-80℃脱模具,即可制得镜片基片。
2.如权利要求1所述的制备方法,其特征在于,所述步骤III程序升温操作是在18~22小时内从室温程序升温至95~100℃,然后保持该温度1.5~2.0小时,完成固化成型。
3.如权利要求1或2所述的制备方法,其特征在于,所述热固性或热塑性光学树脂单体选自苯乙烯、甲基丙烯酸、季戊四醇四丙烯酸酯、乙氧化壬基酚丙烯酸酯、环氧丙烯酸酯、双酚A环氧丙烯酸酯、甲基苯乙烯、聚丙烯酸酯、乙氧化双酚A二丙烯酸酯和甲基丙烯酸丁酯中的一种或多种。
4.如权利要求1或2所述的制备方法,其特征在于,所述固化剂选自过氧化二碳酸二异丙酯、过氧化-2-乙基己基碳酸叔丁酯、1,1′-偶氮(氰基环己烷)、偶氮二甲酸二异丙酯、偶氮二异庚腈、偶氮二异丁酸二甲酯、偶氮二异丁酸二乙酯、异丙苯过氧化氢、叔丁基过氧化氢中的一种或多种。
5.如权利要求1或2所述的制备方法,其特征在于,所述光致变色材料为N-(β-羟乙基)-3,3-二甲基-6-硝基螺吲哚啉苯并吡喃、1,3,3-三甲基吲哚-6-硝基苯并二氢吡喃并螺烷和/或1,3,3-三甲基吲哚-β-萘基二氢呋喃。
6.如权利要求1或2所述的制备方法,其特征在于,所述稀释剂为甲苯、二甲苯、甲基丙烯酸烷基酯、甲基丙烯酸羟乙酯、季戊四醇、乙二醇、丙二醇、丁二醇、己二醇、新戊二醇、正丁醇、三羟甲基丙烷中的一种或多种的混合物。
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