CN109337425A - 一种醇溶性有机富锌底漆的制备方法 - Google Patents
一种醇溶性有机富锌底漆的制备方法 Download PDFInfo
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Abstract
本发明属防腐涂料制备领域,具体为一种醇溶性有机富锌底漆的制备方法。该方法主要包括成膜预聚物的合成及底漆配制两部分。成膜预聚物主要是丙烯酸、丙烯酸正丁醇、乙酸乙烯酯等单体在引发剂过氧化苯甲酰作用下经过多步反应合成的丙烯酸预聚物;然后缓慢加入用酒精等醇类溶剂润湿分散的锌粉、碳纤维短纤、鳞片石墨混合填料,搅拌均匀后,即可在钢铁基体表面进行施工。所制备的富锌底漆1)成膜预聚物是低分子量高固含量;2)成膜预聚物能够在锌粉的作用下发生交联反应;3)成膜预聚物能够溶解在醇类溶剂中;4)所制备的涂料有较好的导电性,能充分发挥锌粉的牺牲阳极作用;5)以无水乙醇为溶剂快速挥发缩短固化时间,无污染属于环境友好型。
Description
技术领域
本发明防腐涂料制备领域,具体为一种醇溶性有机富锌底漆的制备方法。
背景技术
防腐涂料,一般分为常规防腐涂料和重防腐涂料,是油漆涂料中必不可少的一种涂料。常规防腐涂料是在一般条件下,对金属等起到防腐蚀的作用,保护有色金属使用的寿命;重防腐涂料是指相对常规防腐涂料而言,能在相对苛刻腐蚀环境里应用,并具有能达到比常规防腐涂料更长保护期的一类防腐涂料。
富锌涂料是一种环氧富锌重防腐粉末涂料,锌粉含量在85—95%之间,涂膜仅厚100微米,成本低,性能优异的涂料。漆膜坚硬、附着力好、防锈能力强等优点,已经成为钢铁等黑色金属防腐应用领域中最普遍、最重要的底漆。其主要的防腐机理为前期牺牲阳极的阴极电化学保护作用;后期锌粉腐蚀产物形成堵塞涂膜孔隙的物理屏蔽作用;涂膜的自修补和钝化作用。
目前应用的富锌底漆主要有两大类:以硅酸盐等无机物为黏结剂的无机富锌底漆和以环氧树脂为黏结剂的有机富锌底漆。环氧富锌底漆目前仍以溶剂型为主,不利于环保;而无机富锌底漆对钢铁表面处理的要求较严格,施工与固化受环境温度、湿度影响较大。
发明内容
本发明的目的在于针对上述技术问题,提供一种易于施工的、利于环保的醇溶性有机富锌底漆的制备方法。
为了实现以上发明目的,本发明的具体技术方案如下:
一种醇溶性有机富锌底漆的制备方法,其包括以下步骤:
(1)成膜预聚物的合成:
(1.1)称取一定量的引发剂过氧化苯甲酰,加入一定量的酒精混合均匀后,取总质量的20%~90%加入到四口烧瓶中,并以30~800转/分的速度搅拌;过氧化苯甲酰与酒精的质量比为5%~30%。引发剂过氧化苯甲酰的加入量为单体质量的0.8~4%。
(1.2)按质量比1:1:1~3:1:30称取丙烯酸、丙烯酸正丁酯、乙酸乙烯酯(或乙烯甲酯),并混合均匀,用氨水中和至pH=7~8,取总质量的10%~40%加入到(1.1)中的四口烧瓶中,剩余的60%~90%加入到滴液漏斗中;
(1.3)称取一定量的二甲基苯胺促进剂,并用酒精混合均匀后,取10%~80%加入到(1.1)中的四口烧瓶中,剩余的20%~90%加入到(1.2)中滴液漏斗中,并以0.5~10g/小时的速度滴加到(1.1)中的四口烧瓶中;二甲基苯胺促进剂与用酒精的质量比为1%~20%。
(1.4)反应2~8小时后开始以5~20℃/分钟的速度进行升温,升温至60~90℃,待滴液漏斗中溶液滴加完毕之后,继续反应10~60分钟;
(1.5)往(1.1)中的四口烧瓶中补加一定量的丙烯酸及剩余的10%~80%过氧化苯甲酰酒精混合液,继续反应1~5小时后,冷却,用氨水调制pH为7~8。丙烯酸的添加量为0%~5%。
(2)醇溶性有机富锌底漆的配制:
(2.1)以质量计,将酒精与正丁醇按比例1:1~5:1的比例配制成混合液,再按质量比为0.5:10~20:1的比例分2~10次缓慢加入混合填料并混合均匀,该混合填料中含有锌粉、碳纤维短纤和鳞片石墨,按质量计,锌粉、碳纤维短纤与鳞片石墨的比例关系为1~2:0.1~0.5:1~0.5;选用锌粉、碳纤维短纤、鳞片石墨的混合填料,可以降低锌粉的用量、提高涂层的导电性。
(2.2)称取一定量的合成树脂,分2~10次加入(2.1)的混合物中,继续搅拌0.5~10小时后,得到醇溶性有机富锌底漆,并进行涂刷施工。合成树脂与(2.1)中混合物的质量比为1:0.6~1:1.5。
作为优选,单体选用丙烯酸、乙酸乙烯酯可提高成膜预聚物的醇溶性。选用丙烯酸、丙烯酸正丁酯、乙酸乙烯酯(或乙酸甲酯)作为单体制备的成膜预聚物能够和锌粉填料发生交联反应。
本发明的积极效果体现在:
(一)、易于施工的、利于环保。
(二)、涂层附着力好,涂层耐冲击性强,涂层耐盐雾300h无变化。
(三)成膜预聚物是低分子量高固含量;成膜预聚物能够在锌粉填料的作用下发生交联反应;所合成的成膜预聚物能够溶解在醇类溶剂中。
(四)所制备的涂料有较好的导电性,能充分发挥锌粉的牺牲阳极作用;以无水乙醇为溶剂快速挥发缩短固化时间,无污染无公害属于环境友好型;涂料受施工环境影响较小。
具体实施方式
下面结合具体实施例和比较例进一步阐述本发明。应理解为,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解为,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
本发明中所采用的原料均为市售产品。
实施例1:
一种醇溶性有机富锌底漆的制备方法,包括以下步骤:
(1)、低分子量高固含成膜预聚物的制备:
(1.1)称取1g引发剂过氧化苯甲酰,加入50g酒精混合均匀后,取总质量的80%加入到四口烧瓶中,并以300转/分的速度搅拌;
(1.2)称取丙烯酸10g、丙烯酸正丁酯10g、乙酸乙烯酯30g,并混合均匀,用氨水中和pH=7,取总质量的50%加入到(1.1)中的四口烧瓶中,剩余的50%加入到滴液漏斗中;
(1.3)称取1g的二甲基苯胺促进剂,并用酒精混合均匀后,取60%加入到(1.1)中的四口烧瓶中,剩余的40%加入到(1.2)中滴液漏斗中,并以1.5g/小时的速度滴加到(1.2)中的四口烧瓶中;
(1.4)反应4小时后开始以10℃/分钟的速度进行升温,升温至80℃,待滴液漏斗中溶液滴加完毕之后,继续反应30分钟;
(1.5)往(1.1)中的四口烧瓶中补加一定量的丙烯酸及剩余的20%过氧化苯甲酰酒精混合液,继续反应2小时后,冷却,用氨水调制pH为7。
(2)醇溶性有机富锌底漆的配制:
(2.1)以酒精:正丁醇为3:1的比例配制成混合液,并搅拌加热到30℃,按1:1的比例分5次缓慢加入锌粉、碳纤维短纤和鳞片石墨的混合物,锌粉、碳纤维短纤与鳞片石墨的质量比为1:0.2:0.6,混合均匀;
(2.2)称取一定量的合成树脂,分5次加入(2.1)的混合物中,合成树脂和混合物的质量比为1:1;继续搅拌1.5小时后,得到醇溶性有机富锌底漆,并进行涂刷施工。
实施例2:
(1)成膜树脂的制备:
(1.1)称取1.2g引发剂过氧化苯甲酰,加入50g酒精混合均匀后,取总质量的70%加入到四口烧瓶中,并以300转/分的速度搅拌;
(1.2)称取丙烯酸10g、乙酸乙烯酯100g,并混合均匀,氨水中和pH=8,取总质量的50%加入到(1.1)中的四口烧瓶中,剩余的50%加入到滴液漏斗中;
(1.3)称取0.5g的二甲基苯胺促进剂,并用酒精混合均匀后,取60%加入到(1.1)中的四口烧瓶中,剩余的40%加入到(1.2)中滴液漏斗中,并以1.5g/小时的速度滴加到(1.1)中的四口烧瓶中;
(1.4)反应4小时后开始以10℃/分钟的速度进行升温,升温至80℃,待滴液漏斗中溶液滴加完毕之后,继续反应30分钟;
(1.5)往(1.1)中的四口烧瓶中补加一定量的丙烯酸及剩余的30%氧化苯甲酰酒精混合液,继续反应2小时后,冷却,用氨水调制pH为8。
(2)醇溶性有机富锌底漆的配制:
(2.1)称取一定量的酒精,并搅拌加热到30℃,按2:1的比例分4次缓慢加入锌粉:碳纤维短纤:鳞片石墨=1.5:0.2:0.5,混合均匀;
(2.2)称取一定量的合成树脂,分4次加入(2.1)的混合物中,合成树脂和混合物的质量比为1:1.5,继续搅拌1小时后,得到醇溶性有机富锌底漆,并进行涂刷施工。
实施例3:
(1)成膜树脂的制备:
(1.1)称取2g引发剂过氧化苯甲酰,加入50g酒精混合均匀后,取总质量的80%加入到四口烧瓶中,并以以300转/分的速度搅拌;
(1.2)称取丙烯酸30g、丙烯酸正丁酯30g、乙酸乙烯酯100g,并混合均匀,氨水中和pH=7,取总质量的50%加入到(1.1)中的四口烧瓶中,剩余的50%加入到滴液漏斗中;
(1.3)称取1g的二甲基苯胺促进剂,并用酒精混合均匀后,取60%加入到(1.1)中的四口烧瓶中,剩余的40%加入到(1.2)中滴液漏斗中,并以1.5g/小时的速度滴加到(1.1)中的四口烧瓶中;
(1.4)反应4小时后开始以10℃/分钟的速度进行升温,升温至80℃,待滴液漏斗中溶液滴加完毕之后,继续反应30分钟;
(1.5)往(1.1)中的四口烧瓶中补加一定量的丙烯酸及剩余的20%过氧化苯甲酰酒精混合液,继续反应2小时后,冷却,用氨水调制pH为7。
(2)醇溶性有机富锌底漆的配制:
(2.1)称取一定量的酒精,并搅拌加热到30℃,按2:1的比例分5次缓慢加入锌粉:碳纤维短纤:鳞片石墨=1.3:0.3:0.5,混合均匀;
(2.2)称取一定量的合成树脂,分5次加入(2.1)的混合物中,继续搅拌2小时后,得到醇溶性有机富锌底漆,并进行涂刷施工。
将实施例1至3制备的醇溶性有机富锌底漆进行性能测试,测试结果列于表1。
表1醇溶性有机富锌底漆性能测试结果
以上所述实例仅是本专利的优选实施方式,但本专利的保护范围并不局限于此。应当指出,对于本技术领域的普通技术人员来说,在不脱离本专利原理的前提下,根据本专利的技术方案及其专利构思,还可以做出若干改进和润饰,这些改进和润饰也应视为本专利的保护范围。
Claims (8)
1.一种醇溶性有机富锌底漆的制备方法,其特征在于包括以下步骤:
(1)成膜预聚物的合成:
(1.1)向引发剂过氧化苯甲酰中加入酒精混合均匀后,然后将其分为两次使用,第一次取总质量的20%~90%加入到四口烧瓶中,并以30~800转/分的速度搅拌;
(1.2)按比例称取丙烯酸、丙烯酸正丁酯、乙酸乙烯酯或乙酸甲酯,并混合均匀,用氨水中和pH=7~8,取总质量的10%~40%加入到(1.1)中的四口烧瓶中,剩余的60%~90%加入到滴液漏斗中;
(1.3)称取一定量的二甲基苯胺促进剂,用酒精混合均匀后,取10%~80%加入到(1.1)中的四口烧瓶中,剩余的20%~90%加入到(1.2)的滴液漏斗中后,并以0.5~10g/小时的速度滴加到(1.1)中的四口烧瓶中;
(1.4)反应2~8小时后开始以5~20℃/分钟的速度进行升温,升温至60~90℃,待滴液漏斗中溶液滴加完毕之后,继续反应10~60分钟;
(1.5)往(1.1)中的四口烧瓶中补加一定量的丙烯酸及剩余的10%~80%过氧化苯甲酰酒精混合液,继续反应1~5小时后,冷却,用氨水调制pH为7~8;
(2)醇溶性有机富锌底漆的配制:
(2.1)将酒精与正丁醇按比例配制成混合液,再分2~10次缓慢加入混合填料,混合填料中;
(2.2)称取一定量的合成树脂,分2~10次加入(2.1)的混合物中,继续搅拌0.5~10小时后,得到醇溶性有机富锌底漆。
2.根据权利要求1所述醇溶性有机富锌底漆的制备方法,其特征在于:所述引发剂过氧化苯甲酰的加入量为单体质量的0.8~4%。
3.根据权利要求1所述醇溶性有机富锌底漆的制备方法,其特征在于:过氧化苯甲酰与酒精的质量比为5%~30%。
4.根据权利要求1所述所述醇溶性有机富锌底漆的制备方法,其特征在于:丙烯酸、丙烯酸正丁酯、乙酸乙烯酯或乙酸甲酯的质量比为1:1:1~3:1:30。
5.根据权利要求1所述所述醇溶性有机富锌底漆的制备方法,其特征在于:二甲基苯胺促进剂与酒精的质量比为1%~20%。
6.根据权利要求1所述所述醇溶性有机富锌底漆的制备方法,其特征在于:将酒精与正丁醇质量比为1:1~5:1的比例。
7.根据权利要求1所述所述醇溶性有机富锌底漆的制备方法,其特征在于:混合填料中各成分以质量计,锌粉:碳纤维短纤:鳞片石墨=1~2:0.1~0.5:1~0.5。
8.根据权利要求1所述所述醇溶性有机富锌底漆的制备方法,其特征在于:步骤(2.2)中,合成树脂与(2.1)中混合物的质量比为1:0.6~1:1.5。
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