CN116285556B - 一种用于路桥的重防腐乳液及其制备方法 - Google Patents
一种用于路桥的重防腐乳液及其制备方法 Download PDFInfo
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- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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Abstract
本发明公开了一种用于路桥的重防腐乳液及其制备方法,属于重度防锈防腐技术领域,按重量份数计,具有如下的组分组成:去离子水100份;环氧树脂30‑50份;丙烯酸系单体8‑14份;甲基丙烯酸缩水甘油醚1‑3份;碱金属硅酸盐2‑8份;二乙烯基苯1‑4份;反应型非离子环氧树脂乳化剂0.6‑3份;改性乳化剂1.5‑8份;固化剂4‑5份;引发剂0.2‑0.5份;氧化剂0.1‑0.4份;还原剂0.1‑0.4份;pH调节剂0‑1份;所述改性乳化剂为改性碳化钛;本发明所述乳液的固化涂膜具有强度高、韧性好、防腐性能优良、耐候性、致密性、连续性良好的特点,适用于路桥等大型钢结构的重防腐。
Description
技术领域
本发明涉及重度防锈防腐技术领域,具体涉及一种用于路桥的重防腐乳液及其制备方法。
背景技术
防锈防腐涂料是装备制造业的重要组成部分,是金属制品,特别是钢铁制品使用过程中不可或缺的防腐保护层。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,重防腐涂料是在近现代工业发展中提出的概念,普通的防腐涂料对环境的承受能力和使用寿命,在新工程、新领域中已经不能满足需求,而提出重防腐涂料的目的就是适应近现代工业发展中对防腐涂料的新要求;重防腐涂料作为防腐涂料的骄子,自上世纪六七十年代开始应用以来,得到了迅速发展,应用范围越来越广,进一步推动了重防腐涂料技术的革命。
传统重防腐涂料中大量使用有机溶剂为分散介质,在涂料的制备和固化过程中,溶剂的挥发容易对环境造成污染,甚至威胁到生产施工人员的身体健康,研发无毒环保的重防腐涂料是社会发展的必然趋势,因此,研究人员将研究重心逐渐由油性涂料转向水性涂料,水性涂料以水作为溶剂或分散介质,具有无毒、无味、价格低廉、原材料资源丰富等特点,是一种优良的环境友好型重防腐涂料,应用前景广阔。按成膜物质区分,当前主要的水性重防腐涂料主要包括环氧树脂型、聚氨酯型和丙烯酸型,其厚膜化的涂膜固化后容易造成收缩;另一方面,水性重防腐涂料中还需要添加多种外加剂,如为获得稳定的乳化效果需要加入乳化剂,为增强减缩需要加入填料,为提高防腐性能需要加入防腐颜料,多种类的外加剂降低了涂膜的连续性和致密性,进而导致防护性能严重下降,难以实现长效防腐,因此,水性重防腐涂料涂层的耐腐蚀性和防锈性能较差。
发明内容
针对上述问题,本发明提供一种用于路桥的重防腐乳液及其制备方法。
本发明的目的采用以下技术方案来实现:
一种用于路桥的重防腐乳液,按重量份数计,具有如下的组分组成:
其中,所述改性乳化剂为改性碳化钛。
优选的,所述改性碳化钛的制备方法包括以下步骤:
S1、称取碳化钛纳米片并超声分散在甲醇溶剂中,得到分散液;分别称取硝酸锌和5-氨基吲唑合并超声溶解在甲醇溶剂中,继续搅拌混合0.5-2h,得到种子溶液,将所述种子溶液加入到所述分散液中,充分搅拌混合后加入2-甲基咪唑的甲醇溶液,在室温下搅拌反应6-12h,反应完成后高速离心分离沉淀,沉淀以甲醇溶剂洗涤,制得产物A;
其中,所述碳化钛纳米片与所述硝酸锌、所述5-氨基吲唑、2-甲基咪唑的质量比例为1:(9-10):(8-9):(20-24);
S2、将所述产物A超声分散在甲醇溶剂中,加入氨基硅烷偶联剂,在室温下搅拌反应1h,反应完成后高速离心分离沉淀,沉淀以甲醇溶剂洗涤,真空干燥,制得产物B;
其中,所述产物A与所述氨基硅烷偶联剂的质量比例为1:(0.01-0.05);
S3、分别称取2-氨基-4-羟基-6-甲基嘧啶、六亚甲基二异氰酸酯和吡啶,混合后再在保护气氛下升温至90-100℃并保温搅拌回流反应过夜,反应完成后加入正己烷稀释,固液分离收集固体产物,将所述固体产物用丙酮溶剂洗涤以除去未反应的六亚甲基二异氰酸酯,真空干燥,得到产物C;
其中,所述2-氨基-4-羟基-6-甲基嘧啶与所述六亚甲基二异氰酸酯、所述吡啶的质量比例为1:(7-9):(0.5-0.7);
S4、称取所述产物C并分散溶解在无水氯仿中,加入所述产物B,在保护气氛下充分混合搅拌,升温至50-60℃并保温搅拌反应4-8h,反应完成后蒸除氯仿,产物用丙酮溶剂洗涤,固液分离收集沉淀,真空干燥,制得所述改性碳化钛;
其中,所述产物C与所述产物B的质量比例为1:(1.8-2.5)。
优选的,所述碳化钛纳米片的制备方法包括以下步骤:
将碳化钛铝微粉加入到氢氟酸溶液中,常温搅拌浸泡1-6h,固液分离收集沉淀,以去离子水洗涤至中性,将沉淀分散在聚乙二醇溶液中,在常温下搅拌过夜后固液分离收集沉淀,真空干燥后制得所述碳化钛纳米片;
其中,所述碳化钛铝微粉的粒径不大于50μm,所述氢氟酸溶液的质量浓度为50wt%,所述聚乙二醇溶液的质量浓度为0.5-1%。
优选的,所述氨基硅烷偶联剂为γ-氨丙基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷、N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷、N-(β-氨乙基)-γ-氨丙基三乙氧基硅烷、N-(β-氨乙基)-γ-氨丙基甲基二甲氧基硅烷、N-(β-氨乙基)-γ-氨丙基甲基二乙氧基硅烷、γ-氨丙基甲基二乙氧基硅烷、γ-氨丙基甲基二甲氧基硅烷、γ-氨丙基乙氧基二甲基硅烷中的一种或几种。
优选的,所述环氧树脂为双酚A型环氧树脂E-44或E-51。
优选的,所述丙烯酸系单体为丙烯酸、丙烯酸甲酯、丙烯酸乙酯和丙烯酸丁酯、甲基丙烯酸、甲基丙烯酸甲酯中的一种或多种。
优选的,所述引发剂为过硫酸钾或过硫酸铵;所述氧化剂为叔丁基过氧化氢;所述还原剂为甲醛次硫酸氢钠。
优选的,所述碱金属硅酸盐为硅酸钠或硅酸锂。
本发明的另一目的在于提供一种所述用于路桥的重防腐乳液的制备方法,具体包括以下步骤:
(1)按比称取各原料备用;
(2)将所述反应型非离子环氧树脂乳化剂和所述改性乳化剂加入到去离子水中,制得乳化剂溶液,加入所述环氧树脂、丙烯酸系单体、甲基丙烯酸缩水甘油醚和二乙烯基苯,搅拌混合后制得乳化液;
(3)将所述固化剂、引发剂、氧化剂、还原剂分别以去离子水溶解并依次加入到所述乳化液中,升温至70-80℃并保温0.5-2h,冷却后加入所述碱金属硅酸盐,加入所述pH调节剂调节pH至5-6.5,搅拌1-30min至均,过滤,制得所述重防腐乳液。
本发明的有益效果为:
(1)本发明在环氧树脂水性乳液的基础上复合丙烯酸系单体,降低了涂膜的固化收缩,同时涂膜兼具环氧树脂和丙烯酸树脂的优点,乳液在固化剂作用下共固化后,形成具有收缩小、强度高、韧性好、防腐性能优良、耐候性良好的防腐涂膜,同时以碳化钛纳米片为基底进行改性,得到一种兼具乳化、填充、交联、防腐作用的改性乳化剂,进一步提高涂膜的致密性、连续性及防腐性能,本发明所述乳液适用于路桥等大型钢结构的重防腐。
(2)碳化钛纳米片具有超薄的二维层状结构,其机械强度高、化学稳定性好,具有良好的抗腐蚀性和耐磨性,具有作为防腐蚀涂料的功能性填料的潜力,本发明以碳化钛纳米片为基底,以2-甲基咪唑为配体,在碳化钛纳米片间生成并嵌入疏水性的沸石咪唑骨架-8,同时在所述沸石咪唑骨架上原位嵌入与2-甲基咪唑结构相似的5-氨基吲唑作为缓蚀剂以提高防腐性能,最后再通过氨基对异氰酸酯基团的反应活性在表面接枝亲水性脲基嘧啶,得到一种兼具乳化、填充、交联、防腐作用的改性乳化剂材料,其中,随机层叠组装的纳米片形成多细小弯曲的通道,通过促进迷宫效应提高防腐性能,进一步的,表面亲水改性使所述碳化钛具备良好的乳化性能,同时,表面接枝的多元脲基嘧啶不仅具有良好的亲水性,基于其形成的多重氢键交联结构,进一步提高涂膜固化后的致密性和连续性,所述改性碳化钛还可以作为填料填充进一步增强减缩;碱金属硅酸盐则进一步促进成膜。
具体实施方式
结合以下实施例对本发明作进一步描述。
实施例1
本实施例涉及一种用于路桥的重防腐乳液,按重量份数计,具有如下的组分组成:
所述重防腐乳液的制备方法包括以下步骤:
(1)按比称取各原料备用;
(2)将所述反应型非离子环氧树脂乳化剂ER-10和所述乳化剂加入到去离子水中,制得乳化剂溶液,加入所述双酚A型环氧树脂E-44、甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸缩水甘油醚和二乙烯基苯,搅拌混合后制得乳化液;
(3)将所述CU-600固化剂、过硫酸钾、叔丁基过氧化氢、吊白块分别以去离子水溶解并依次加入到所述乳化液中,升温至72℃并保温1h,冷却后加入所述硅酸钠,加入所述氨水调节pH至5-6.5,搅拌30min至均,过滤,制得所述重防腐乳液;
所述乳化剂为改性碳化钛,其制备方法包括以下步骤:
S1、将过400目筛的碳化钛铝微粉加入到50wt%的氢氟酸溶液中,常温搅拌浸泡2h,固液分离收集沉淀,以去离子水洗涤至中性,将沉淀分散在0.5%的聚乙二醇溶液中,在常温下搅拌过夜后固液分离收集沉淀,真空干燥后制得所述碳化钛纳米片;
S2、称取碳化钛纳米片1g并超声分散在300mL甲醇溶剂中,得到分散液,分别称取六水合硝酸锌10g和5-氨基吲唑8g,并超声溶解在300mL甲醇溶剂中,继续搅拌混合1h,得到种子溶液,将所述种子溶液加入到所述分散液中,搅拌混合1h后加入含有22g2-甲基咪唑的甲醇溶液,在室温下搅拌反应8h,反应完成后高速离心分离沉淀,沉淀以甲醇溶剂洗涤,制得产物A;
S3、将所述产物A 10g超声分散在500mL甲醇溶剂中,加入γ-氨丙基三甲氧基硅烷0.2g进行表面改性,在室温下搅拌反应1h,反应完成后高速离心分离沉淀,沉淀以甲醇溶剂洗涤,真空干燥24h,制得产物B;
S4、称取2-氨基-4-羟基-6-甲基嘧啶10g、六亚甲基二异氰酸酯80mL和吡啶8mL,在保护气氛下升温至100℃并保温搅拌回流反应过夜,反应完成后加入50mL正己烷,过滤收集固体产物,将固体产物用丙酮洗涤三次以除去未反应的六亚甲基二异氰酸酯,真空干燥24h,得到白色粉末,记为产物C;
S5、称取所述产物C 6g并分散溶解在500mL无水氯仿中,加入所述产物B12g,在保护气氛下充分混合搅拌,升温至60℃并保温搅拌反应6h,反应完成后减压蒸除氯仿,产物用丙酮溶剂洗涤三次,过滤收集固体产物,真空干燥24h,制得所述改性碳化钛。
实施例2
一种防腐乳液,同实施例1,区别在于,所述乳化剂为反应型阴离子乳化剂SEN-10。
实施例3
一种防腐乳液,同实施例1,区别在于,所述改性碳化钛的制备方法中,步骤S2未加入5-氨基吲唑。
实施例4
一种防腐乳液,同实施例1,区别在于,乳化剂为实施例1步骤S1制备的碳化钛纳米片。
实施例5
一种防腐乳液,同实施例1,区别在于,所述改性碳化钛的制备方法包括以下步骤:
S1-S2同实施例1;
S3、将所述产物A 10g超声分散在1%的聚乙二醇溶液中,在常温下搅拌过夜后固液分离收集沉淀,真空干燥后制得。
实例验
耐水性能按GB/T1733-1993测定;耐盐雾性按照GB/T1771-2007测试;柔韧性能按GB/T1731-1993测试;耐冲击性能按GB/T1732-1993测试;附着力按照GB/T1720-1979测试;铅笔硬度按照GB/T6739-1996测试;
最后应当说明的是,以上实施例仅用以说明本发明的技术方案,而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细地说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。
Claims (7)
1.一种用于路桥的重防腐乳液,其特征在于,按重量份数计,具有如下的组分组成:
其中,所述改性乳化剂为改性碳化钛;
所述改性碳化钛的制备方法包括以下步骤:
S1、称取碳化钛纳米片并超声分散在甲醇溶剂中,得到分散液;分别称取硝酸锌和5-氨基吲唑合并超声溶解在甲醇溶剂中,继续搅拌混合0.5-2h,得到种子溶液,将所述种子溶液加入到所述分散液中,充分搅拌混合后加入2-甲基咪唑的甲醇溶液,在室温下搅拌反应6-12h,反应完成后高速离心分离沉淀,沉淀以甲醇溶剂洗涤,制得产物A;
其中,所述碳化钛纳米片与所述硝酸锌、所述5-氨基吲唑、2-甲基咪唑的质量比例为1:(9-10):(8-9):(20-24);
S2、将所述产物A超声分散在甲醇溶剂中,加入氨基硅烷偶联剂,在室温下搅拌反应1h,反应完成后高速离心分离沉淀,沉淀以甲醇溶剂洗涤,真空干燥,制得产物B;
其中,所述产物A与所述氨基硅烷偶联剂的质量比例为1:(0.01-0.05);
S3、分别称取2-氨基-4-羟基-6-甲基嘧啶、六亚甲基二异氰酸酯和吡啶,混合后再在保护气氛下升温至90-100℃并保温搅拌回流反应过夜,反应完成后加入正己烷稀释,固液分离收集固体产物,将所述固体产物用丙酮溶剂洗涤以除去未反应的六亚甲基二异氰酸酯,真空干燥,得到产物C;
其中,所述2-氨基-4-羟基-6-甲基嘧啶与所述六亚甲基二异氰酸酯、所述吡啶的质量比例为1:(7-9):(0.5-0.7);
S4、称取所述产物C并分散溶解在无水氯仿中,加入所述产物B,在保护气氛下充分混合搅拌,升温至50-60℃并保温搅拌反应4-8h,反应完成后蒸除氯仿,产物用丙酮溶剂洗涤,固液分离收集沉淀,真空干燥,制得所述改性碳化钛;
其中,所述产物C与所述产物B的质量比例为1:(1.8-2.5);
所述碳化钛纳米片的制备方法包括以下步骤:
将碳化钛铝微粉加入到氢氟酸溶液中,常温搅拌浸泡1-6h,固液分离收集沉淀,以去离子水洗涤至中性,将沉淀分散在聚乙二醇溶液中,在常温下搅拌过夜后固液分离收集沉淀,真空干燥后制得所述碳化钛纳米片;
其中,所述碳化钛铝微粉的粒径不大于50μm,所述氢氟酸溶液的质量浓度为50wt%,所述聚乙二醇溶液的质量浓度为0.5-1%。
2.根据权利要求1所述的一种用于路桥的重防腐乳液,其特征在于,所述氨基硅烷偶联剂为γ-氨丙基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷、N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷、N-(β-氨乙基)-γ-氨丙基三乙氧基硅烷、N-(β-氨乙基)-γ-氨丙基甲基二甲氧基硅烷、N-(β-氨乙基)-γ-氨丙基甲基二乙氧基硅烷、γ-氨丙基甲基二乙氧基硅烷、γ-氨丙基甲基二甲氧基硅烷、γ-氨丙基乙氧基二甲基硅烷中的一种或几种。
3.根据权利要求1所述的一种用于路桥的重防腐乳液,其特征在于,所述环氧树脂为双酚A型环氧树脂E-44或E-51。
4.根据权利要求1所述的一种用于路桥的重防腐乳液,其特征在于,所述丙烯酸系单体为丙烯酸、丙烯酸甲酯、丙烯酸乙酯和丙烯酸丁酯、甲基丙烯酸、甲基丙烯酸甲酯中的一种或多种。
5.根据权利要求1所述的一种用于路桥的重防腐乳液,其特征在于,所述引发剂为过硫酸钾或过硫酸铵;所述氧化剂为叔丁基过氧化氢;所述还原剂为甲醛次硫酸氢钠。
6.根据权利要求1所述的一种用于路桥的重防腐乳液,其特征在于,所述碱金属硅酸盐为硅酸钠或硅酸锂。
7.根据权利要求1-6之一所述的一种用于路桥的重防腐乳液的制备方法,其特征在于,包括以下步骤:
(1)按比称取各原料备用;
(2)将所述反应型非离子环氧树脂乳化剂和所述改性乳化剂加入到去离子水中,制得乳化剂溶液,加入所述环氧树脂、丙烯酸系单体、甲基丙烯酸缩水甘油醚和二乙烯基苯,搅拌混合后制得乳化液;
(3)将所述固化剂、引发剂、氧化剂、还原剂分别以去离子水溶解并依次加入到所述乳化液中,升温至70-80℃并保温0.5-2h,冷却后加入所述碱金属硅酸盐,加入所述pH调节剂调节pH至5-6.5,搅拌1-30min至均,过滤,制得所述重防腐乳液。
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