CN115093503B - 一种耐氟化氢的聚合物、玻璃及其制备方法 - Google Patents

一种耐氟化氢的聚合物、玻璃及其制备方法 Download PDF

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CN115093503B
CN115093503B CN202210734833.5A CN202210734833A CN115093503B CN 115093503 B CN115093503 B CN 115093503B CN 202210734833 A CN202210734833 A CN 202210734833A CN 115093503 B CN115093503 B CN 115093503B
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acrylate
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glass
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CN115093503A (zh
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刘伟
朱敏
李勇
郑建楠
胡安福
徐俊淦
李旭
冯威
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Shandong Dongyue Polymer Material Co Ltd
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Abstract

本发明涉及玻璃防腐领域，具体提供一种耐氟化氢的聚合物，所述聚合物包括用于防氟化氢的源自单体(a)的重复单元、用于成膜的源自单体(b)的重复单元、用于耐久的源自单体(c)的重复单元、用于交联的源自单体(d)的重复单元。并提供了一种覆盖一层上述聚合物涂层的耐氟化氢的玻璃，所述聚合物涂层可防止氟化氢渗透从而腐蚀玻璃，且所述聚合物涂层与玻璃通过化学反应相结合，提高聚合物涂层与玻璃之间的牢固度。

Description

一种耐氟化氢的聚合物、玻璃及其制备方法
技术领域
本发明属于玻璃防腐领域，特别是涉及一种耐氟化氢的聚合物、玻璃及其制备方法。
背景技术
玻璃不仅是一种透明材料，且具有独特的透明性，在我们生活中各种不同领域发挥着重要的作用。它功能丰富，无论是用于居室或建筑设计，还是用于工业、军事、国防科研、能源生产、生态环境、现代通讯技术，其他材料都不能像玻璃这样用途广泛。
玻璃的主要成分是硅酸盐如硅酸钠、硅酸钙和硅酸铝等等，这些材料是会与氟化氢反应的，因此材料本身没有耐氟化氢性能。
因此在氟化氢生产、使用场所，所使用的玻璃如果接触氟化氢，会被腐蚀，极易造成安全事故，而出过事故之后，接触氟化氢的窗户、仪表、电子器械、设备均需更换。
专利CN108970944A公开了一种铝电解工业中玻璃防氟化氢腐蚀的方法，具体公开了通过依次对玻璃进行碱洗、清洗、表面活化、涂覆及干燥等步骤，在玻璃表面涂覆一层由酚醛树脂、硫酸钡、聚酰胺、石墨粉、纳米铬粉、丙酮组成的防腐涂层，从而防氟化氢且并不降低透光度。然而防腐蚀涂层需要经过包含上述五个步骤包括高达150-200℃的高温涂覆等繁琐复杂的程序才能与玻璃达到较好的牢固度，而且本质上还是通过物理隔离的方法使氟化氢不容易渗透，如果有漏点或穿孔，氟化氢渗透腐蚀玻璃风险是极高。
发明内容
为了避免玻璃被氟化氢腐蚀、防腐涂层与玻璃结合不牢固、防腐涂层涂覆过程繁杂等问题，本发明提供了一种耐氟化氢的聚合物、玻璃及其制备方法。
一种耐氟化氢的聚合物，所述聚合物包括源自单体(a)的重复单元、源自于单体(d)的重复单元。
所述单体(a)为：
其中：R为H，CH3，Cl中的一种或多种，n为0～20之间的整数，优选为3～5，特别优选为5。
所述单体(d)为非氟交联性单体；
所述非氟交联性单体不含氟原子且所述非氟交联性单体具有至少2个反应性基团和\或碳碳双键。
优选的，所述非氟交联性单体为具有至少2个碳碳双键的化合物、或所述非氟交联单体为具有至少1个碳碳双键和至少1个反应性基团的化合物。
优选的，所述非氟交联性单体为具有反应性基团的单(甲基)丙烯酸酯、二(甲基)丙烯酸酯或单(甲基)丙烯酰胺。
所述反应性基团包括：羟基、环氧基、氯甲基、封端异氰酸酯基、氨基、羧基。
所述非氟交联性单体包括但不限于：二丙酮(甲基)丙烯酰胺、N－羟甲基(甲基)丙烯酰胺、羟基甲基(甲基)丙烯酸酯、羟基乙基(甲基)丙烯酸酯、3-氯-2-羟基丙基(甲基)丙烯酸酯、2-乙酰乙酰氧基乙基(甲基)丙烯酸酯、丁二烯、异戊二烯、氯丁二烯、单氯乙酸乙烯酯、甲基丙烯酸乙烯酯、缩水甘油基(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯之一。
所述非氟交联性单体中的反应性基团与玻璃表面的硅羟基反应脱水缩合，使聚合物与玻璃通过化学反应相结合，提高聚合物涂层与玻璃之间的牢固度。
所述聚合物还包括源自于单体(b)的重复单元、源自于单体(c)的重复单元。
所述单体(b)为非氟非交联性单体；
所述非氟非交联性单体为不含氟原子且含至多一个反应性基团的单体。
所述非氟非交联性单体包括但不限于：(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸异丙酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸肉豆蔻酯、(甲基)丙烯酸鲸蜡酯、(甲基)丙烯酸硬脂基酯、(甲基)丙烯酸山嵛基酯、(甲基)丙烯酸异冰片酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸苄基酯、(甲基)丙烯酸金刚烷基酯、乙烯、乙酸乙烯酯、丙烯腈、苯乙烯、聚乙二醇(甲基)丙烯酸酯、聚丙二醇(甲基)丙烯酸酯、甲氧基聚乙二醇(甲基)丙烯酸酯、甲氧基聚丙二醇(甲基)丙烯酸酯和乙烯基烷基醚、聚硅氧烷(甲基)丙烯酸酯之一。
所述源自单体(b)的重复单元用于改善聚合物的成膜性能，增加聚合物与玻璃表面的牢固度。
单体(c)为卤代烯烃；
所述卤代烯烃为取代有1～10个氯原子或溴原子或碘原子的的烯烃，且所述烯烃碳原子数为2～20。
优选的，所述卤代烯烃为碳原子数2～20的氯代烯烃，
特别优选的，所述卤代烯烃具有1～5个氯原子，2～5个碳原子。
优选的，所述卤代烯烃不具有氟原子。
卤代烯烃可以列举为：卤代乙烯，例如：氯乙烯、溴乙烯、碘乙烯；偏卤乙烯，例如：偏氯乙烯、偏溴乙烯、偏碘乙烯。
优选的，所述卤代烯烃为氯乙烯、偏氯乙烯之一。
所述源自单体(c)的重复单元中，烯烃上的氢被卤素取代，聚合后不容易被空气氧化，从而使聚合物赋予的耐久性、尤其是洗涤耐久性提高。
所述单体的摩尔比为单体(a)：单体(b)：单体(c)：单体(d)＝(1～100)：(0:99)：(0～20)：(1～30)。
所述聚合物的分子量范围为5000～200000。
一种耐氟化氢的玻璃，所述玻璃表面覆盖上述聚合物涂层。
所述聚合物涂层厚度为0.1～0.5mm。
所述耐氟化氢玻璃的静态接触角(水)为113-119°。
上述具有聚合物涂层的防腐机理为：
在玻璃与氟化氢界面，所述聚合物的亲水基与玻璃表面相结合，亲油基使玻璃表面形成一层具有一定疏水性的保护膜，使氟化氢无法渗透到玻璃表面，从而起到保护玻璃的作用。
本发明还提供一种上述耐氟化氢的玻璃的制备方法，包括以下步骤：
S1：配制聚合物溶液；
S2：将S1获得的聚合物溶液涂覆至玻璃表面；
S3：对涂覆有聚合物的玻璃进行干燥处理。
步骤S1中所述聚合物溶液的溶剂为水，溶质为上述聚合物，质量浓度为1-50％。
步骤S2中所述涂覆方法为浸涂、滚涂或喷涂。
步骤S3中所述干燥处理的温度为100-160℃，干燥处理的时间为10～180min。
有益效果：
1、本发明提供了一种耐氟化氢腐蚀的玻璃及其制备方法，通过涂覆聚合物得到一种耐氟化氢腐蚀的玻璃，其静态水接触角可达113～119°，可有效防止氟化氢对玻璃的腐蚀。
2、本发明中玻璃与聚合物涂层的牢固度可达5B，具有良好的贴合性，不易脱附，耐久性较强。
3、本发明中聚合物涂覆后，玻璃仍保持透明。
附图说明
图1为实施例1制备得到的玻璃用30％氟化氢溶液浸泡3小时的图片；
图2为对比例1制备得到的玻璃被氟化氢吹拂30分钟的图片；
图3为对比例2制备得到的玻璃的图片。
具体实施方式
下述牢固度均为经ASTM-D3359标准检测得到。
实施例1
本实施例中单体(a)、(b)、(c)、(d)的摩尔比为1：1：1：1，其中单体a为全氟己基乙基丙烯酸酯，单体b为甲基丙烯酸月桂酸酯，单体c为氯乙烯，单体d为羟基乙基(甲基)丙烯酸酯，具体参数如表1所示。
将硅胶板所用玻璃片放入盛有1％质量浓度聚合物溶液的四氟乙烯塑料瓶中，浸泡12小时，取出后放入烘箱中于160℃的条件下干燥10min。将烘干后玻璃片放入质量分数为30％氟化氢水溶液中浸泡3h，取出用水冲洗，晾干。所得玻璃片如图1，从图中可以看出，玻璃表面完整、光滑。
实施例2～实施例10
除单体及其质量浓度变化外，其余均同实施例1，变化参数如表1所示。
实施例11
将1％质量浓度的聚合物溶液放在喷壶中向玻璃片上喷涂，随后放入烘箱中于100℃的条件下干燥10min。将烘干后玻璃片放入质量分数为30％的氟化氢水溶液中浸泡3h，取出用水冲洗，晾干。
实施例12
用1％质量浓度的聚合物溶液浸泡吸水滚筒后滚涂至玻璃片上，随后放入烘箱中于100℃的条件下干燥180min。将烘干后玻璃片放入质量分数为30％的氟化氢水溶液中浸泡3h，取出用水冲洗，晾干。
对比例1
将硅胶板所用玻璃片放入质量分数为30％的氢氟酸水溶液中，浸泡12小时，取出后放入烘箱中于160℃的条件下干燥10min。使用氟化氢对着玻璃片吹拂30分钟，所得玻璃如图2所示，从图中可以看出，经氟化氢吹拂后，玻璃表面粗糙、划痕明显。
从表2中可以看出经含聚合物的涂覆后，玻璃表面的静态接触角大幅提高，即玻璃的疏水性明显提升。
对比例2
本对比例将聚合物更换为偏氯乙烯与六氟丙烯的共聚物(其水溶液本身为透明溶液)，其余均同实施例1。本对比例聚合物参数参见表1。涂覆所得玻璃如图3所示，虽然能够改变接触角以防氟化氢，但是玻璃则失去了透明的特性。
对比例3
本对比例中不使用单体(d)，其余均同实施例2。本对比例聚合物参数见表1。
如表2所示，若不使用交联基团，则聚合物涂层与玻璃则仅通过物理作用进行结合，牢固度明显下降。
表1各实施例的参数值
表2各实施例的性能指标

Claims (12)

1.一种耐氟化氢的玻璃的制备方法，包括以下步骤：
S1：配制聚合物溶液；
S2：将S1获得的聚合物溶液涂覆至玻璃表面；
S3：对涂覆有聚合物的玻璃进行干燥处理；
步骤S1中所述聚合物溶液的溶剂为水，溶质为聚合物，质量浓度为1-50％；
步骤S2中所述涂覆方法为浸涂、滚涂或喷涂；
步骤S3中所述干燥处理的温度为100-160℃，干燥处理的时间为10～180min；
所述聚合物包括源自单体(a)的重复单元、源自于单体(d)的重复单元，
所述单体(a)为：
其中：R为CH3或Cl，n为0～20之间的整数；
所述单体(d)为非氟交联性单体；
所述非氟交联性单体具有至少2个碳碳双键、或所述非氟交联性单体具有至少1个碳碳双键和至少1个反应性基团；所述反应性基团包括：羟基、环氧基。
2.根据权利要求1所述的制备方法，其特征在于，单体(a)中，n为3～11之间的整数。
3.根据权利要求1所述的制备方法，其特征在于，所述聚合物还包括源自于单体(b)的重复单元、源自于单体(c)的重复单元；
所述单体(b)为非氟非交联性单体；
所述单体(c)为卤代烯烃。
4.根据权利要求3所述的制备方法，其特征在于，
所述卤代烯烃为取代有1～10个氯原子或溴原子或碘原子的烯烃，且所述烯烃的碳原子数为2～20；
所述聚合物中单体的重量份为：单体(a)为1～100份，单体(b)0～99份，单体(c)为0～20份，单体(d)为1～30份。
5.根据权利要求4所述的制备方法，其特征在于，所述非氟非交联性单体选自(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸异丙酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸肉豆蔻酯、(甲基)丙烯酸鲸蜡酯、(甲基)丙烯酸硬脂基酯、(甲基)丙烯酸山嵛基酯、(甲基)丙烯酸异冰片酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸苄基酯、(甲基)丙烯酸金刚烷基酯、乙烯、乙酸乙烯酯、丙烯腈、苯乙烯、乙烯基烷基醚和聚硅氧烷(甲基)丙烯酸酯之一。
6.根据权利要求5所述的制备方法，其特征在于，所述卤代烯烃为碳原子数2～20的氯代烯烃。
7.根据权利要求6所述的制备方法，其特征在于，所述氯代烯烃具有1～5个氯原子、2～5个碳原子。
8.根据权利要求7所述的制备方法，其特征在于，所述氯代烯烃为氯乙烯、偏氯乙烯之一。
9.根据权利要求4所述的制备方法，其特征在于，非氟交联性单体为具有反应性基团的单(甲基)丙烯酸酯、二(甲基)丙烯酸酯或单(甲基)丙烯酰胺。
10.根据权利要求1所述的制备方法，其特征在于，所述非氟交联性单体选自N－羟甲基(甲基)丙烯酰胺、羟基甲基(甲基)丙烯酸酯、羟基乙基(甲基)丙烯酸酯、3-氯-2-羟基丙基(甲基)丙烯酸酯、丁二烯、异戊二烯、氯丁二烯、缩水甘油基(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯之一。
11.根据权利要求1所述的制备方法，其特征在于，所述聚合物的分子量范围为5000～200000。
12.一种如权利要求1-11任一项所述的制备方法制得的耐氟化氢的玻璃，其特征在于，所述聚合物涂层厚度为0.1～0.5mm。
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103857715A (zh) * 2011-09-30 2014-06-11 大金工业株式会社 拨水拨油剂组合物
JP2015083619A (ja) * 2013-10-25 2015-04-30 ダイキン工業株式会社 含フッ素剥離剤組成物
CN107304323A (zh) * 2016-04-20 2017-10-31 大金工业株式会社 水性涂料组合物和涂装物品

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103857715A (zh) * 2011-09-30 2014-06-11 大金工业株式会社 拨水拨油剂组合物
JP2015083619A (ja) * 2013-10-25 2015-04-30 ダイキン工業株式会社 含フッ素剥離剤組成物
CN107304323A (zh) * 2016-04-20 2017-10-31 大金工业株式会社 水性涂料组合物和涂装物品

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