CN107033743A - 一种磁性微球溶胶保温涂料的制备方法 - Google Patents
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Abstract
本发明公开了一种磁性微球溶胶保温涂料的制备方法,本发明以聚酯为模板,钛酸四丁酯为前驱体,通过水解,磁性原料的水热反应,将磁性溶胶沉积到聚酯表面,然后将聚酯溶解消去,得到中空磁性微球,该中空磁性微球相对于传统的空心玻璃微珠,不仅具有很好的保温性,还具有很好的磁性、稳定性和表面强度,微球不易破裂,同时通过羧基与氨基的反应,将该磁性微球酰胺化,增强了其在水溶液中的分散性,有效的降低了团聚,避免了涂料的沉积,提高了涂料的贮存稳定性。
Description
技术领域
本发明属于涂料领域,具体涉及一种磁性微球溶胶保温涂料的制备方法。
背景技术
环氧树脂具有优异的耐化学腐蚀性,对众多底材具有极佳的附着力,能与多种固化剂固化,涂膜的致密性好、刚性强、耐热耐磨性都很好,在防腐涂料中占据着重要地位,通过添加不同的填料和调整固化剂品种,可以制成性能各异的环氧树脂防腐涂料、适用于不同的防腐场合,达到良好的保护效果。每年世界上约有 40%的环氧树脂应用于制造环氧涂料,大部分应用于防腐领域。在我国,大约有 30%-40%的环氧树脂被加工成各种各样的涂料,在船舶、土木工程、家用电器、机电工业等领域有着广泛的用途;
目前,随着广告行业的发展越来越迅速,广告展示的底板有木质板材、塑料板材、木塑板材、金属板材等,传统直接将广告采用喷印或者涂刷等方式容易造成严重的资源浪费,更换广告还需要进行清洗等处理,费时费力又不方便,因此本发明打算研究一种全新的磁性涂料,该涂料对于各种基材的粘结强度高,通过将基材表面赋予磁性,然后将广告做成磁性的贴膜,在更换广告时,只需要更换磁性贴膜即可,解决了传统的大面积需要经常更换画面的广告所面临的运输成本高,安装限时,费时和安装人力成本高的问题,同时本发明的涂料可以自由选择涂覆面积,根据广告贴膜的大小来对基材进行磁性涂覆,选择性好,实用性强,同时,本发明的涂料也可以用于广告贴膜的磁性涂覆,该贴膜也可以做成木质、塑料、金属等材质,然后采用本发明的涂料进行涂覆,改变了传统的广告展示模式,具有很好的社会效益。
同时作为保温涂料来说,空心玻璃微珠是最常用的添加剂,但是其表面稳定性差,容易破损。
发明内容
本发明的目的在于针对现有技术的缺陷和不足,提供一种磁性微球溶胶保温涂料的制备方法。
为实现上述目的,本发明采用以下技术方案:
一种磁性微球溶胶保温涂料的制备方法,包括以下步骤:
(1)取20-30重量份的钛酸四丁酯,加入到其重量30-40倍的去离子水中,搅拌均匀,得预溶胶;
(2)取25-30重量份的六水三氯化铁,加入到其重量4-6倍的乙二醇中,搅拌均匀,与上述预溶胶混合,搅拌均匀,加入0.7-1重量份的3-氨丙基三乙氧基硅烷,在50-60℃下保温搅拌1-2小时,得磁性氨基溶胶;
(3)取1-2重量份的硬脂酸、17-20重量份的甲基丙烯酸甲酯混合,加入到混合料重量16-20倍的去离子水中,搅拌均匀,送入到反应釜中,加入0.6-0.8重量份的过硫酸铵,通入氮气,调节反应釜温度为70-75℃,保温搅拌3-4小时,出料,得羧基化聚酯;
(4)取上述羧基化聚酯,加入到磁性氨基溶胶中,搅拌均匀,超声3-5分钟,升高温度为40-50℃,滴加20-27重量份的、10-13%的氨水,滴加完毕后搅拌反应1-2小时,送入到反应釜中,加入6-9重量份的尿素,调节反应釜温度为150-160℃,搅拌反应3-4小时,出料,在80-85℃的烘箱中干燥1-2小时,出料,冷却至常温,得酰胺化磁性聚酯溶胶;
(5)取上述酰胺化磁性聚酯溶胶,加入到其重量16-20倍的溶解液中,搅拌2-3小时,过滤,将沉淀水洗,常温干燥,得酰胺化磁性溶胶空心球;
(6)取上述酰胺化磁性溶胶空心球、30-40重量份的环氧树脂E44混合,加入到混合料重量2-3倍的去离子水中,搅拌均匀,送入到反应釜中,调节反应釜温度为56-70℃,保温搅拌10-20分钟,通入氮气,加入0.4-0.7重量份的三氟化硼乙醚,搅拌反应3-4小时,出料冷却,得酰胺化环氧树脂预聚物溶液;
(7)取上述酰胺化环氧树脂预聚物溶液,与150-170重量份的环氧树脂E44、3-4重量份的聚乙二醇、60-80重量份的去离子水混合,1600-2000转/分搅拌1-2小时,即得所述磁性微球溶胶保温涂料。
所述的溶解液为体积比为6-10:1-2的二氯乙烷、丙酮的混合溶液。
本发明的涂料在使用时,将磁性微球溶胶保温涂料与其重量20-25%的三聚氰胺甲醛树脂固化剂混合,搅拌均匀,即可进行涂覆。
本发明的优点:
本发明首先以钛酸四丁酯为前驱体,分散到去离子水中,然后将氯化铁与其混合,通过3-氨丙基三乙氧基硅烷处理,得磁性氨基溶胶,然后以甲基丙烯酸甲酯为单体,通过硬脂酸掺杂,在过硫酸铵作用下聚合,得到羧基化聚酯;然后将其分散到磁性氨基溶胶中,通过羧基与氨基的作用,将溶胶分散到聚酯表面,再通过滴加氨水,使得溶胶充分水解,得到二氧化钛溶胶,然后与尿素混合,通过水热处理,将得到的氧化物磁性二氧化钛溶胶沉积到聚酯表面,得酰胺化磁性聚酯溶胶,然后将其加入到溶解液中,将聚酯溶解消去,得到空心酰胺化磁性溶胶空心球,然后将其与环氧树脂E44混合,在水溶液中预聚合、分散,即得;
本发明以聚酯为模板,钛酸四丁酯为前驱体,通过水解,磁性原料的水热反应,将磁性溶胶沉积到聚酯表面,然后将聚酯溶解消去,得到中空磁性微球,该中空磁性微球相对于传统的空心玻璃微珠,不仅具有很好的保温性,还具有很好的磁性、稳定性和表面强度,微球不易破裂,同时通过羧基与氨基的反应,将该磁性微球酰胺化,增强了其在水溶液中的分散性,有效的降低了团聚,避免了涂料的沉积,提高了涂料的贮存稳定性;
本发明的涂料主要用于广告展示,通过将基材表面赋予磁性,然后将广告做成磁性的贴膜,在更换广告时,只需要更换磁性贴膜即可,解决了传统的大面积需要经常更换画面的广告所面临的运输成本高,安装限时,费时和安装人力成本高的问题,同时本发明的涂料可以自由选择涂覆面积,根据广告贴膜的大小来对基材进行磁性涂覆,选择性好,实用性强,同时,本发明的涂料也可以用于广告贴膜的磁性涂覆,该贴膜也可以做成木质、塑料、金属等材质,然后采用本发明的涂料进行涂覆,改变了传统的广告展示模式,具有很好的社会效益,本发明的涂料对于冬天户外广告的展示具有很好的适应性,不会造成广告贴膜的脱落、不粘等现象。
具体实施方式
实施例1
一种磁性微球溶胶保温涂料的制备方法,包括以下步骤:
(1)取20重量份的钛酸四丁酯,加入到其重量30倍的去离子水中,搅拌均匀,得预溶胶;
(2)取25重量份的六水三氯化铁,加入到其重量4倍的乙二醇中,搅拌均匀,与上述预溶胶混合,搅拌均匀,加入0.7重量份的3-氨丙基三乙氧基硅烷,在50℃下保温搅拌1小时,得磁性氨基溶胶;
(3)取1重量份的硬脂酸、17重量份的甲基丙烯酸甲酯混合,加入到混合料重量16倍的去离子水中,搅拌均匀,送入到反应釜中,加入0.6重量份的过硫酸铵,通入氮气,调节反应釜温度为70℃,保温搅拌3小时,出料,得羧基化聚酯;
(4)取上述羧基化聚酯,加入到磁性氨基溶胶中,搅拌均匀,超声3分钟,升高温度为40℃,滴加20-27重量份的、10%的氨水,滴加完毕后搅拌反应1小时,送入到反应釜中,加入6重量份的尿素,调节反应釜温度为150℃,搅拌反应3小时,出料,在80℃的烘箱中干燥1小时,出料,冷却至常温,得酰胺化磁性聚酯溶胶;
(5)取上述酰胺化磁性聚酯溶胶,加入到其重量16-20倍的溶解液中,搅拌2-3小时,过滤,将沉淀水洗,常温干燥,得酰胺化磁性溶胶空心球;
(6)取上述酰胺化磁性溶胶空心球、30重量份的环氧树脂E44混合,加入到混合料重量2倍的去离子水中,搅拌均匀,送入到反应釜中,调节反应釜温度为56℃,保温搅拌10分钟,通入氮气,加入0.4重量份的三氟化硼乙醚,搅拌反应3小时,出料冷却,得酰胺化环氧树脂预聚物溶液;
(7)取上述酰胺化环氧树脂预聚物溶液、150重量份的环氧树脂E44、3重量份的聚乙二醇、60重量份的去离子水混合,1600转/分搅拌1小时,即得所述磁性微球溶胶保温涂料。
所述的溶解液为体积比为6:1的二氯乙烷、丙酮的混合溶液。
实施例2
一种磁性微球溶胶保温涂料的制备方法,包括以下步骤:
(1)取30重量份的钛酸四丁酯,加入到其重量40倍的去离子水中,搅拌均匀,得预溶胶;
(2)取30重量份的六水三氯化铁,加入到其重量6倍的乙二醇中,搅拌均匀,与上述预溶胶混合,搅拌均匀,加入1重量份的3-氨丙基三乙氧基硅烷,在60℃下保温搅拌2小时,得磁性氨基溶胶;
(3)取2重量份的硬脂酸、20重量份的甲基丙烯酸甲酯混合,加入到混合料重量20倍的去离子水中,搅拌均匀,送入到反应釜中,加入0.8重量份的过硫酸铵,通入氮气,调节反应釜温度为75℃,保温搅拌4小时,出料,得羧基化聚酯;
(4)取上述羧基化聚酯,加入到磁性氨基溶胶中,搅拌均匀,超声5分钟,升高温度为50℃,滴加27重量份的、13%的氨水,滴加完毕后搅拌反应2小时,送入到反应釜中,加入9重量份的尿素,调节反应釜温度为160℃,搅拌反应4小时,出料,在85℃的烘箱中干燥2小时,出料,冷却至常温,得酰胺化磁性聚酯溶胶;
(5)取上述酰胺化磁性聚酯溶胶,加入到其重量20倍的溶解液中,搅拌2-3小时,过滤,将沉淀水洗,常温干燥,得酰胺化磁性溶胶空心球;
(6)取上述酰胺化磁性溶胶空心球、40重量份的环氧树脂E44混合,加入到混合料重量3倍的去离子水中,搅拌均匀,送入到反应釜中,调节反应釜温度为70℃,保温搅拌20分钟,通入氮气,加入0.7重量份的三氟化硼乙醚,搅拌反应3-4小时,出料冷却,得酰胺化环氧树脂预聚物溶液;
(7)取上述酰胺化环氧树脂预聚物溶液、170重量份的环氧树脂E44、4重量份的聚乙二醇、80重量份的去离子水混合,2000转/分搅拌2小时,即得所述磁性微球溶胶保温涂料。
所述的溶解液为体积比为10:2的二氯乙烷、丙酮的混合溶液。
性能测试:性能测试:
本发明涂料无结块无沉积,涂层平整光滑无颗粒;
附着力:1级;
不透水性:0.3MPa、30min无渗透;
低温柔性:-25℃、30min,无裂纹、无断裂;
粘结强度:0.6-0.8MPa;
耐热度:100℃、30min,无流淌,无断裂;
涂膜的热导率:0.20-0.27 W/m.k;
传统水性环氧涂料的附着力为2级、在-25℃、30min下涂膜断裂,粘结强度为0.5-0.6MPa,热导率为0.45-0.6 W/m.k。
Claims (2)
1.一种磁性微球溶胶保温涂料的制备方法,其特征在于,包括以下步骤:
(1)取20-30重量份的钛酸四丁酯,加入到其重量30-40倍的去离子水中,搅拌均匀,得预溶胶;
(2)取25-30重量份的六水三氯化铁,加入到其重量4-6倍的乙二醇中,搅拌均匀,与上述预溶胶混合,搅拌均匀,加入0.7-1重量份的3-氨丙基三乙氧基硅烷,在50-60℃下保温搅拌1-2小时,得磁性氨基溶胶;
(3)取1-2重量份的硬脂酸、17-20重量份的甲基丙烯酸甲酯混合,加入到混合料重量16-20倍的去离子水中,搅拌均匀,送入到反应釜中,加入0.6-0.8重量份的过硫酸铵,通入氮气,调节反应釜温度为70-75℃,保温搅拌3-4小时,出料,得羧基化聚酯;
(4)取上述羧基化聚酯,加入到磁性氨基溶胶中,搅拌均匀,超声3-5分钟,升高温度为40-50℃,滴加20-27重量份的、10-13%的氨水,滴加完毕后搅拌反应1-2小时,送入到反应釜中,加入6-9重量份的尿素,调节反应釜温度为150-160℃,搅拌反应3-4小时,出料,在80-85℃的烘箱中干燥1-2小时,出料,冷却至常温,得酰胺化磁性聚酯溶胶;
(5)取上述酰胺化磁性聚酯溶胶,加入到其重量16-20倍的溶解液中,搅拌2-3小时,过滤,将沉淀水洗,常温干燥,得酰胺化磁性溶胶空心球;
(6)取上述酰胺化磁性溶胶空心球、30-40重量份的环氧树脂E44混合,加入到混合料重量2-3倍的去离子水中,搅拌均匀,送入到反应釜中,调节反应釜温度为56-70℃,保温搅拌10-20分钟,通入氮气,加入0.4-0.7重量份的三氟化硼乙醚,搅拌反应3-4小时,出料冷却,得酰胺化环氧树脂预聚物溶液;
(7)取上述酰胺化环氧树脂预聚物溶液,与150-170重量份的环氧树脂E44、3-4重量份的聚乙二醇、60-80重量份的去离子水混合,1600-2000转/分搅拌1-2小时,即得所述磁性微球溶胶保温涂料。
2.根据权利要求1所述的一种磁性微球溶胶保温涂料的制备方法,其特征在于,所述的溶解液为体积比为6-10:1-2的二氯乙烷、丙酮的混合溶液。
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