CN106423769A - 一种光学玻璃超疏水疏油抗污涂层的制备方法 - Google Patents
一种光学玻璃超疏水疏油抗污涂层的制备方法 Download PDFInfo
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Abstract
本发明属于传感器所用的光学材料领域,特别涉及一种光学玻璃超疏水疏油抗污涂层的制备方法。本发明采用有机玻璃作为在线浊度传感器的光学窗口,以特定的预处理工艺在有机玻璃表面清洗,并采用改性纳米颗粒和具有特定官能团的氟碳树脂形成涂层,加上特定工艺进行固化处理,形成的涂层既保持原有的透明度,又具有一定的抗磨性能,同时其表面呈现出一定的憎水憎油特性,增强了其抗污染性能,有效的延长了其在水环境中长期浸泡时的维护周期,适用于长期浸泡在水环境的光学传感器进行非接触性测量的光学窗口。
Description
技术领域
本发明属于传感器所用的光学材料领域,特别涉及一种光学玻璃超疏水疏油抗污涂层的制备方法。
背景技术
有机玻璃作为一种透明聚合物材料,具有密度小、耐冲击、耐腐蚀、耐溶剂、易加工等特点。但其缺点也是非常明显,耐磨性能不好,特别是长期在水环境中,容易在表面与水中物体刮碰而产生刮痕;另外对于复杂水质环境,其表面容易沾上有机污垢,影响其透光率。作为一种优异材料,其可以被作为一种光学器件的光学窗口用在水环境中。但在水环境中浸泡周期长后,必须定期取出维护、清洁,如表面处理不当,会导致数据准确度下降、维护周期缩短等问题。
专利CN102778434A公开一种用于水质在线检测的浊度传感器及其检测方法,其采用了石英玻璃作为光学窗口,但石英玻璃没做处理,不耐碰撞,并且作为在线系统,石英玻璃表面极易在有机污染物存在下发生吸附,形成污垢,进而影响效果。
专利 CN102928386A公开一种浊度传感器及其水体浊度在线检测方法,该浊度传感器采用了独特的结构设计,尽可能地避免了水体中的污物附着在透光镜片上而影响浊度检测精度,但依然采用了石英玻璃作为光学窗口,仍然存在易碎、易沾污垢的问题。
发明内容
针对上述的问题,本发明提供一种光学玻璃超疏水疏油抗污涂层的制备方法,形成的涂层既保持原有的透明度,又具有一定的抗磨性能,同时其表面呈现出一定的憎水憎油特性,增强了其抗污染性能,有效的延长了其在水环境中长期浸泡时的维护周期。
本发明的上述目的,可以通过如下方案予以实现:
一种光学玻璃超疏水疏油抗污涂层的制备方法,包含下列步骤:
S1: 涂层选用的基材要先经过预处理。所用的预处理工艺为:基材采用表面洗脱液在室温条件下浸泡4-25分钟后,用超纯水冲洗表面,然后置于强碱性电解水中浸泡,取出用超纯水冲洗表面,再用25-50℃的乙醇溶液浸泡1-10分钟,最后用超纯水冲洗,10-80℃条件下烘干,取出密封保存;
S2: 预处理后,将涂层溶液通过喷涂工艺覆盖在基材表面。在喷涂室内,20-45℃条件下,湿度控制在(65±5)%,用流变控制剂控制黏度,用自动喷涂机喷涂;
S3: 涂覆成膜后送进具有通风系统的微波室进行干燥固化;
S4: 喷涂后的基材经过低温烘烤工艺形成超疏水疏油抗污涂层。
优选地,S1中所选用的基材为聚甲基丙烯酸甲酯。
优选地,S1中烘干温度为45-70℃,干燥时间1-4h。
优选地,S1中表面洗脱液为三乙醇胺、焦磷酸钾、烷基酚聚氧乙烯醚、碳酸氢钠、乙醇中的一种或几种和纯水。
优选地,S2中涂层溶液的组分为改性二氧化硅、含羧基的氟碳树脂、乙苯。
优选地,S2中改性二氧化硅平均粒径为30-50nm,质量分数为1%-8%,其表面接枝有二嵌段聚合物。
优选地,S2中氟碳树脂为具有一定量羧基官能团的聚合物,氟碳树脂的质量分数在1%-20%。
优选地,S2中流变控制剂为氟化表面活性剂,主要结构为端基为多氟原子的烯烃化合物。
优选地,S3中固化时间控制在2-20分钟。
优选地,S4中烘烤温度控制在60℃-80℃,烘烤时间为15min-60min。
本发明的有益效果为,本发明采用有机玻璃作为在线浊度传感器的光学窗口,以特定的预处理工艺在有机玻璃表面清洗,并采用改性纳米颗粒和具有特定官能团的氟碳树脂形成涂层,加上特定工艺进行固化处理,形成的涂层既保持原有的透明度,又具有一定的抗磨性能,同时其表面呈现出一定的憎水憎油特性,增强了其抗污染性能,有效的延长了其在水环境中长期浸泡时的维护周期,适用于长期浸泡在水环境的光学传感器进行非接触性测量的光学窗口。
具体实施方式
以下结合具体实施例来进一步说明本发明,但实施例并不对本发明保护范围作限制。凡不脱离本发明基本构思所作的等同变换,均属于本发明的保护范围。
实施例1:
所选用的基材为聚甲基丙烯酸甲酯。预处理工艺为:基材采用表面洗脱液在室温条件下浸泡5min,表面洗脱液的组分及配比(v/v)为:三乙醇胺(12%)、烷基酚聚氧乙烯醚(6%)、碳酸氢钠(1.5%)、乙醇(8.5%)、纯水(72%)。
然后用超纯水冲洗表面,然后再放置在强碱性电解水中浸泡30sec,取出再用超纯水冲洗表面,再用40℃的乙醇溶液浸泡3min,最后用超纯水冲洗,放入65℃的烘箱中干燥3h,然后取出密封保存。
预处理后,将组分为改性二氧化硅、含羧基的氟碳树脂、乙苯的涂层溶液通过喷涂工艺覆盖在基材表面。改性二氧化硅平均粒径为50nm,质量分数为5%,其表面接枝有二嵌段聚合物;氟碳树脂为具有一定量羧基官能团的聚合物,氟碳树脂的质量分数在13%。在喷涂室内,25℃的条件下,湿度控制在(65±5)%,用流变控制剂RCA控制黏度,用自动喷涂机喷涂,涂覆成膜后送进具有通风系统的微波室进行干燥固化,固化时间控制在10min。
喷涂后的基材经过低温烘烤工艺形成超疏水疏油抗污涂层。烘烤温度控制在60℃,烘烤时间在30min。
实施例2:
所选用的基材为聚甲基丙烯酸甲酯。预处理工艺为:基材采用表面洗脱液在室温条件下浸泡5min,表面洗脱液的组分及配比(v/v)为:三乙醇胺(12%)、烷基酚聚氧乙烯醚(6%)、碳酸氢钠(1.5%)、乙醇(8.5%)、焦磷酸钾(2%)、纯水(70%)。
然后用超纯水冲洗表面,然后再放置在强碱性电解水中浸泡30s,取出再用超纯水冲洗表面,再用40℃的乙醇溶液浸泡3min,最后用超纯水冲洗,放入65℃的烘箱中干燥3h,然后取出密封保存。
预处理后,将组分为改性二氧化硅、含羧基的氟碳树脂、乙苯的涂层溶液通过喷涂工艺覆盖在基材表面。改性二氧化硅平均粒径为50nm,质量分数为6%,其表面接枝有二嵌段聚合物;氟碳树脂为具有一定量羧基官能团的聚合物,氟碳树脂的质量分数在15%。在喷涂室内,25℃的条件下,湿度控制在(65±5)%,用流变控制剂RCA控制黏度,用自动喷涂机喷涂,涂覆成膜后送进具有通风系统的微波室进行干燥固化,固化时间控制在20min。
喷涂后的基材经过低温烘烤工艺形成超疏水疏油抗污涂层。烘烤温度控制在80℃,烘烤时间在10min。
实施例3:
所选用的基材为聚甲基丙烯酸甲酯。预处理工艺为:基材采用表面洗脱液在室温条件下浸泡5min,表面洗脱液的组成分及配比(v/v)为:三乙醇胺(15%)、烷基酚聚氧乙烯醚(5%)、碳酸氢钠(1.5%)、乙醇(9.5%)、焦磷酸钾(2%)、纯水(67%)。
然后用超纯水冲洗表面,然后再放置在强碱性电解水中浸泡30秒,取出再用超纯水冲洗表面,再用40℃的乙醇溶液浸泡3min,最后用超纯水冲洗,放入65℃的烘箱中干燥3h,然后取出密封保存。
预处理后,将组分为改性二氧化硅、含羧基的氟碳树脂、乙苯的涂层溶液通过喷涂工艺覆盖在基材表面。改性二氧化硅平均粒径为30nm,质量分数为8%,其表面接枝有二嵌段聚合物;氟碳树脂为具有一定量羧基官能团的聚合物,氟碳树脂的质量分数在15%。在喷涂室内,25℃的条件下,湿度控制在(65±5)%,用流变控制剂RCA控制黏度,用自动喷涂机喷涂,涂覆成膜后送进具有通风系统的微波室进行干燥固化,固化时间控制在15min。
喷涂后的基材经过低温烘烤工艺形成超疏水疏油抗污涂层。烘烤温度控制在65℃,烘烤时间在60min。
实施例4:
所选用的基材为聚甲基丙烯酸甲酯。预处理工艺为:基材采用表面洗脱液在室温条件下浸泡5min,表面洗脱液的组分及配比(v/v)为:三乙醇胺(15%)、纯水(85%)。
然后用超纯水冲洗表面,然后再放置在强碱性电解水中浸泡30秒,取出再用超纯水冲洗表面,再用30℃的乙醇溶液浸泡3min,最后用超纯水冲洗,放入65℃的烘箱中干燥3h,然后取出密封保存。
预处理后,将组分为改性二氧化硅、含羧基的氟碳树脂、乙苯的涂层溶液通过喷涂工艺覆盖在基材表面。改性二氧化硅平均粒径为30nm,质量分数为8%,其表面接枝有二嵌段聚合物;氟碳树脂为具有一定量羧基官能团的聚合物,氟碳树脂的质量分数在15%。在喷涂室内,25℃的条件下,湿度控制在(65±5)%,用流变控制剂RCA控制黏度,用自动喷涂机喷涂,涂覆成膜后送进具有通风系统的微波室进行干燥固化,固化时间控制在15min。
喷涂后的基材经过低温烘烤工艺形成超疏水疏油抗污涂层。烘烤温度控制在60℃,烘烤时间在60min。
实施例5:
所选用的基材为聚甲基丙烯酸甲酯。预处理工艺为:基材采用表面洗脱液在室温条件下浸泡5min,表面洗脱液的组分及配比(v/v)为:三乙醇胺(11.5%)、乙醇(5%)、碳酸氢钠(3.5%)、纯水(80%)。
然后用超纯水冲洗表面,然后再放置在强碱性电解水中浸泡30秒,取出再用超纯水冲洗表面,再用30℃的乙醇溶液浸泡3min,最后用超纯水冲洗,放入65℃的烘箱中干燥3h,然后取出密封保存。
预处理后,将组分为改性二氧化硅、含羧基的氟碳树脂、乙苯的涂层溶液通过喷涂工艺覆盖在基材表面。改性二氧化硅平均粒径为40nm,质量分数为6%,其表面接枝有二嵌段聚合物;氟碳树脂为具有一定量羧基官能团的聚合物,氟碳树脂的质量分数在15%。在喷涂室内,25℃的条件下,湿度控制在(65±5)%,用流变控制剂RCA控制黏度,用自动喷涂机喷涂,涂覆成膜后送进具有通风系统的微波室进行干燥固化,固化时间控制在15min。
喷涂后的基材经过低温烘烤工艺形成超疏水疏油抗污涂层。烘烤温度控制在65℃,烘烤时间在70min。
实施例6:
所选用的基材为聚甲基丙烯酸甲酯。预处理工艺为:基材采用表面洗脱液在室温条件下浸泡5min,表面洗脱液的组分及配比(v/v):焦磷酸钾(11.5%)、乙醇(15%)、碳酸氢钠(3.5%)纯水(70%)。
然后用超纯水冲洗表面,然后再放置在强碱性电解水中浸泡30秒,取出再用超纯水冲洗表面,再用45℃的乙醇溶液浸泡3min,最后用超纯水冲洗,放入65℃的烘箱中干燥3h,然后取出密封保存。
预处理后,将组分为改性二氧化硅、含羧基的氟碳树脂、乙苯的涂层溶液通过喷涂工艺覆盖在基材表面。改性二氧化硅平均粒径为35nm,质量分数为9%,其表面接枝有二嵌段聚合物;氟碳树脂为具有一定量羧基官能团的聚合物,氟碳树脂的质量分数在15%。在喷涂室内,25℃的条件下,湿度控制在(65±5)%,用流变控制剂RCA控制黏度,用自动喷涂机喷涂,涂覆成膜后送进具有通风系统的微波室进行干燥固化,固化时间控制在15min。
喷涂后的基材经过低温烘烤工艺形成超疏水疏油抗污涂层。烘烤温度控制在60℃,烘烤时间在80min。
对比例:没有涂覆涂层的有机玻璃
测试结果对比如下表:
性能 | 对比样 | 实施例1 | 实施例2 | 实施例3 | 测试方法 |
硬度 | 3H | 5H | 5H | 4H | GB/T 6739-1996 |
耐沾污性能 | 有部分污染物残留 | 无残留 | 无残留 | 无残留 | GB/T 9780-1988 |
接触角测试 | 76° | 126° | 135° | 128° | 采用光学接触角测试仪 |
透明性测试 | 91% | 90% | 90% | 89% | 与基材的透光率曲线做对比 |
性能 | 对比样 | 实施例4 | 实施例5 | 实施例6 | 测试方法 |
硬度 | 3H | 4H | 5H | 5H | GB/T 6739-1996 |
耐沾污性能 | 有部分污染物残留 | 无残留 | 无残留 | 无残留 | GB/T 9780-1988 |
接触角测试 | 76° | 120° | 128° | 131° | 采用光学接触角测试仪 |
透明性测试 | 91% | 89.5% | 90% | 89% | 与基材的透光率曲线做对比 |
Claims (10)
1.一种光学玻璃超疏水疏油抗污涂层的制备方法,其特征在于,包括下列步骤:
S1: 涂层选用的基材要先经过预处理,所用的预处理工艺为:基材采用表面洗脱液在室温条件下浸泡4-20分钟,用超纯水冲洗表面,然后置于强碱性电解水中浸泡,取出用超纯水冲洗表面,再用25-50℃的乙醇溶液浸泡1-10分钟,最后用超纯水冲洗,10-80℃条件下烘干,取出密封保存;
S2: 预处理后,将涂层溶液通过喷涂工艺覆盖在基材表面;在喷涂室内,20-45℃条件下,湿度控制在(65±5)%,用流变控制剂控制黏度,用自动喷涂机喷涂;
S3: 涂覆成膜后送进具有通风系统的微波室进行干燥固化;
S4:喷涂后的基材经过低温烘烤工艺形成超疏水疏油抗污涂层。
2.根据权利要求1所述光学玻璃超疏水疏油抗污涂层的制备方法,其特征在于,涂层所选用的基材为聚甲基丙烯酸甲酯。
3.根据权利要求2所述光学玻璃超疏水疏油抗污涂层的制备方法,其特征在于,S1中烘干温度为45-70℃,干燥时间1-4h。
4.根据权利要求3所述光学玻璃超疏水疏油抗污涂层的制备方法,其特征在于,所述表面洗脱液为三乙醇胺、焦磷酸钾、烷基酚聚氧乙烯醚、碳酸氢钠、乙醇中的一种或几种和纯水,其中溶剂占70-90%(v/v),试剂占30%-10%(v/v)。
5.根据权利要求1所述光学玻璃超疏水疏油抗污涂层的制备方法,其特征在于,所述涂层溶液的组分为改性二氧化硅、含羧基的氟碳树脂、乙苯。
6.根据权利要求5所述光学玻璃超疏水疏油抗污涂层的制备方法,其特征在于,所述改性二氧化硅平均粒径为30-50nm,质量分数为1%-8%,其表面接枝有二嵌段聚合物。
7.根据权利要求6所述光学玻璃超疏水疏油抗污涂层的制备方法,其特征在于,所述氟碳树脂为具有一定量羧基官能团的聚合物,质量分数为1%-20%。
8.根据权利要求1所述光学玻璃超疏水疏油抗污涂层的制备方法,其特征在于,所述流变控制剂为氟化表面活性剂,主要结构为端基为多氟原子的烯烃化合物。
9.根据权利要求1所述光学玻璃超疏水疏油抗污涂层的制备方法,其特征在于,S3中固化时间控制在2-20分钟。
10.根据权利要求1-9任一项所述光学玻璃超疏水疏油抗污涂层的制备方法,其特征在于,S4中烘烤温度控制在60℃-80℃,烘烤时间为15min-60min。
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