CN109134749A - 一种含叠氮基团的超疏水抗腐材料的制备方法 - Google Patents
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Abstract
本发明公开了一种含叠氮基团的超疏水抗腐材料的制备方法,属于化学材料技术领域。本发明的超疏水抗腐蚀材料的制备方法,包括引发剂、催化剂2‑5份、叠氮单体20‑100份、含氟单体60‑200份、辅助催化剂3‑5份、纳米二氧化硅1‑3份、其中引发剂占总原料质量百分比为0.3‑1%。按上述配比,加入反应器中,抽掉其中的空气,在蓝灯下,搅拌10个小时,然后将反应液倒入正己烷中,得到析出的固体,将该固体融入溶剂中,制膜,在光固化灯下固化10分钟,得到改材料,其具有超疏水、抗腐蚀等优点。
Description
技术领域
本发明涉及一种含叠氮基团的超疏水抗腐材料的制备方法,属于高分子材料技术领域。
背景技术
通常环境介质对材料有各种不同的作用,其中有多种作用可导致材料遭受破坏,其中化学腐蚀在工业及生活中及其常见,随着含氟材料的高速发展,含氟聚合物尤其是氟碳聚合物及含氟硅聚合物的研究日益增多。含氟聚合物通常具有较好的憎油性、憎水性、耐热性、耐高低温性、耐化学药品性、耐候性。因而近年来已在建筑、化学工业、电器电子工业、机械工业、航空航天产业、家庭用品的各个领域得到广泛应用,而且实践证明含氟材料有其他材料无法替代的优势。
叠氮基团具有较高的反应活性,在热或光的作用下可以生成高反应活性的氮宾,可以与聚合物链或材料表面发生反应,因此叠氮聚合物也被广泛用作交联材料和表面改性材料。已有的发明中有使用叠氮基单体和含氟化合物以及碳纳米管制成了相似的超疏水材料,但是该材料在碱性条件下的抗腐蚀性能较差,而且该发明中使用热促进的聚合方法,团叠氮基易被破坏,不仅使得材料的粘结性能降低,且存在爆炸危险,使得改材料的应用性受到极大的限制,因此,一种在温和条件下高效合成能够耐酸耐碱腐蚀的含叠氮基超疏水材料有极大应用前景。
发明内容
本发明制备了一种含氟新型材料,其具有当水滴在材料表面时接触角在150°以上,在pH=1酸液和pH=13碱液腐蚀72小时后,接触角变化小于30°的抗腐蚀超疏水性能。
本发明提供了一种超疏水抗腐蚀材料,其原料包括:引发剂,催化剂2-5份,叠氮单体20-100份,含氟单体60-200份,辅助催化剂3-5份,纳米二氧化硅1-3份;其中引发剂占总原料质量百分比为0.3-1%。
在一种实施方式中,所述超疏水抗腐蚀材料的合成方法,是在去除氧气的反应器中加入引发剂、催化剂、叠氮单体、含氟单体、辅助催化剂、纳米二氧化硅。
在一种实施方式中,所述叠氮单体可以是含叠氮基的烯烃,比如对叠氮苯酯、烷基烯烃苯酯、芳基叠氮烯烃。
在一种实施方式中,所述含氟单体为甲基丙烯酸三氟乙酯、甲基丙烯酸六氟丁酯、甲基丙烯酸十氟辛酯中的一种。
在一种实施方式中,所述引发剂可以是α-溴苯基乙酸乙酯、全氟四氟化硼重氮盐。
在一种实施方式中,所述辅助催化剂可以是有机碱,比如三乙胺、五甲基二乙烯三胺、二乙胺中的一种。
在一种实施方式中,所述催化剂可以是曙红Y、曙红B、罗丹明B。优选为曙红Y。
在一种实施方式中,所述材料含有:引发剂0.3份,曙红Y为2份,叠氮单体20份,含氟单体70份,有机胺5份,纳米二氧化硅3份。
在一种实施方式中,所述合成方法,具体是:按质量份数,将原料加入加入反应器中,抽掉其中的空气,在LED灯光下,搅拌6-10个小时,然后将反应液倒入溶剂(比如正己烷)中,得到析出的固体,即为含叠氮基团的超疏水抗腐材料。
在一种实施方式中,所述光可以是可见光,具体是蓝色光、绿色光等。
在一种实施方式中,所述可见光光源设备为普通LED灯。
本发明的第二个目的是提供本发明的超疏水抗腐蚀材料的使用方法,将该固体叠氮基抗腐蚀材料融入溶剂中,将溶液均匀涂覆于纸张、家具、汽车等待处理物的表面,在160W、365nm波长的光固化灯下固化10分钟,得到具有超疏水抗腐蚀性能的改性产品。
本发明的第三个目的是提供含有本发明超疏水抗腐蚀材料的产品,比如用于建筑、化学工业、电器电子工业、机械工业、航空航天产业、家庭用品等各个领域的产品。
本发明的有益效果:
本发明以一步投料法直接自由基共聚,在引发剂的作用下直接制备含叠氮基团的含氟聚合物,避免了以往制备含氟聚合物采用多次滴加投料并严格控制体系温度和劲度的做法,保存了聚合物中的叠氮基团,使聚合物具有了较强的应用性。解决了以往在聚合工艺控制和设备方面要求高的难题,采用本发明的制备方法简单高效,反应条件温和,工艺好控制,设备要求低,并得到了低成本的含氟聚合物。
附图说明
图1为本发明的反应方程式。
具体实施方式
如图1所示,为本发明的反应方程式。本发明机理如下,在光照下催化剂进入激发态,和有机胺交换电子,成为自由基负离子,使得引发剂成为自由基,引发聚合反应,催化剂回到基态,聚合物自由基链和有机胺交换电子,完成反应。
实施例1
按照质量百分比引发剂0.3%,曙红Y为5%,叠氮单体20%,含氟单体70%,有机胺3%,纳米二氧化硅1.7%,将以上物质加入已除去氧气的反应器中,在7W蓝色LED灯光的照射下搅拌10小时后,将反应器中的物质倒入正己烷中,聚合物材料将会析出,叠氮保存率为100%,反应产率70%,材料分子量分布1.30。
将材料溶于二氯甲烷后涂在纸张上,在光固化灯下照射固化5分钟,纸张表面即覆盖一层具有超疏水抗腐蚀材料。测试经改性后的纸张接触角,在未酸碱腐蚀的情况下,接触角为141°,pH=1的酸液腐蚀24h后为140°,72h后为138°;pH=13的碱液腐蚀24h后为135°;72h后为122°。
实施例2
按照质量百分比引发剂0.3%,曙红Y为2%,叠氮单体20%,含氟单体69.7%,有机胺5%,纳米二氧化硅3%。将以上物质加入已出去氧气的反应器中,在7W蓝色LED灯光的照射下搅拌10小时后,将反应器中的物质倒入正己烷中,聚合物将会析出。叠氮保存率为100%,反应产率为85%,材料分子量分布1.41。
将材料溶于二氯甲烷后涂在纸张上,在光固化灯照射下固化5分钟,纸张表面即覆盖一层具有超疏水抗腐蚀材料。测试经改性后纸张的接触角,在未酸碱腐蚀的情况下,接触角为144°,pH=1的酸液腐蚀24h后为144°,72h后为140°;pH=13的碱液腐蚀24h后为132°;72h后为127°,
实施例3
按照质量百分比引发剂0.5%,曙红Y为3%,叠氮单体25%,含氟单体65%,有机胺4%,纳米二氧化硅2.5%。将以上物质加入已出去氧气的反应器中,在7W蓝色LED灯光的照射下搅拌10小时后,将反应器中的物质倒入正己烷中,聚合物将会析出。叠氮保存率为100%,反应产率为80%,材料分子量分布1.36。
将材料溶于二氯甲烷后涂在纸张上,在光固化灯照射下固化5分钟,将材料涂在纸张上,纸张表面即覆盖一层具有超疏水抗腐蚀材料。测试经改性后纸张的接触角,在未酸碱腐蚀的情况下,接触角为167°,pH=1的酸液腐蚀24h后为164°,72h后为160°;pH=13的碱液腐蚀24h后为155°;72h后为147°。
实施例4
按照质量百分比引发剂1%,曙红Y为4%,叠氮单体30%,含氟单体60%,有机胺4%,纳米二氧化硅1%。将以上物质加入已出去氧气的反应器中,在7W蓝色LED灯光的照射下搅拌10小时后,将反应器中的物质倒入正己烷中,聚合物将会析出。叠氮保存率为100%,反应产率为90%,材料分子量分布1.33。
将材料溶于二氯甲烷后涂在纸张上,在光固化灯照射下固化5分钟,将材料涂在纸张上,纸张表面即覆盖一层具有超疏水抗腐蚀材料。测试接触角,在未酸碱腐蚀的情况下,接触角为141°,pH=1的酸液腐蚀24h后为140°,72h后为138°;pH=13的碱液腐蚀24h后为135°;72h后为122°。
实施例5
与实施例1相比,区别仅仅在于用五甲基二乙烯三胺替换实施例1中的三乙胺,其他步骤或参数与实施例1一致。
结果显示,所得聚合物叠氮基含量减少15%,分子量分布为1.6。
在未酸碱腐蚀的情况下,以此聚合物改性后纸张的接触角为152°,pH=1的酸液腐蚀24h后为150°,72h后为148°;pH=13的碱液腐蚀24h后为146°;72h后为139°,反应产率60%,材料分子量分布1.6。
实施例6
与实施例1相比,区别仅仅在于用绿色LED灯替换实施例1中的蓝色灯,其他步骤或参数与实施例1一致。
结果显示,聚合物叠氮保存率为100%,反应产率90%,材料分子量分布1.15。产率为50%。在未酸碱腐蚀的情况下,以此聚合物改性后纸张的接触角为149°,pH=1的酸液腐蚀24h后为144°,72h后为141°;pH=13的碱液腐蚀24h后为139°;72h后为131°。
实施例7
与实施例1相比,区别仅仅在于曙红B替换实施例1中的曙红Y,其他步骤或参数与实施例1一致。
结果显示,聚合物叠氮保存率为100%,反应产率70%,材料分子量分布为1.81。在未酸碱腐蚀的情况下,以此聚合物改性后纸张的接触角为162°,pH=1的酸液腐蚀24h后为159°,72h后为154°;pH=13的碱液腐蚀24h后为155°;72h后为142°。
实施例8
与实施例1相比,区别仅仅在于罗丹明B替换实施例1中的曙红Y,其他步骤或参数与实施例1一致。
结果显示,该聚合物叠氮保存率为75%,反应产率90%,分子量分布为2.13。在未酸碱腐蚀的情况下,以此聚合物改性后纸张的接触角为154°,pH=1的酸液腐蚀24h后为153°,72h后为150°;pH=13的碱液腐蚀24h后为147°;72h后为137°。
对实施例1~实施例8得到的材料进行分析和性能测试,具体数据见表1。
表1实施例1~实施例8得到的材料
接触角测量由座滴法,液滴体积2ul,测试3次,取平均值。
叠氮保存率:保留有叠氮基的单体量/聚合物上参与的共聚的叠氮单体量*100%
对比例1
与实施例1相比,区别在于不在反应中加入三乙胺,其他步骤或参数与实施例1一致。
结果显示,无法得到目标聚合物。
对比例2
与实施例1相比,区别仅仅在于不抽真空替换实施例1中的无氧环境,其他步骤或参数与实施例1一致。
结果显示,无法得到目标聚合物。
虽然本发明已以较佳实施例公开如上,但其并非用以限定本发明,任何熟悉此技术的人,在不脱离本发明的精神和范围内,都可做各种的改动与修饰,因此本发明的保护范围应该以权利要求书所界定的为准。
Claims (10)
1.一种超疏水抗腐蚀材料,其特征在于,其原料包括:引发剂,催化剂2-5份,叠氮单体20-100份,含氟单体60-200份,辅助催化剂3-5份,纳米二氧化硅1-3份;其中引发剂占总原料质量百分比为0.3-1%。
2.根据权利要求1所述的超疏水抗腐蚀材料,其特征在于,所述辅助催化剂为有机碱。
3.根据权利要求1所述的超疏水抗腐蚀材料,其特征在于,所述超疏水抗腐蚀材料的合成方法,是在去除氧气的反应器中加入引发剂、催化剂、叠氮单体、含氟单体、辅助催化剂、纳米二氧化硅。
4.根据权利要求1所述的超疏水抗腐蚀材料,其特征在于,所述叠氮单体为含叠氮基的烯烃;所述含氟单体为甲基丙烯酸三氟乙酯、甲基丙烯酸六氟丁酯、甲基丙烯酸十氟辛酯中的一种或多种。
5.根据权利要求1所述的超疏水抗腐蚀材料,其特征在于,所述催化剂是曙红Y、曙红B、罗丹明B中的一种或多种。
6.一种制备权利要求1-5任一所述超疏水抗腐蚀材料的制备方法,包括:按配比,将原料加入加入反应器中,抽掉其中的空气,在LED灯光下,搅拌一段时间,然后将反应液倒入溶剂中,得到析出的该材料。
7.根据权利要求6所述的方法,其特征在于,所述光为可见光。
8.一种涂层,所述涂层是利用权利要求1-5任一所述的超疏水抗腐蚀材料制备得到的。
9.含有权利要求1-5任一所述的超疏水抗腐蚀材料或者涂层的产品。
10.根据权利要求9所述的产品,其特征在于,所述产品包括用于建筑、化学工业、电器电子工业、机械工业、航空航天产业、家庭的产品。
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