CN105778686A - 一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法 - Google Patents
一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法 Download PDFInfo
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- CN105778686A CN105778686A CN201610148794.5A CN201610148794A CN105778686A CN 105778686 A CN105778686 A CN 105778686A CN 201610148794 A CN201610148794 A CN 201610148794A CN 105778686 A CN105778686 A CN 105778686A
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Classifications
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Abstract
一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法的特征在于:加入去离子水、二丁基萘磺酸钠、OS‑15重量、丙烯酸,将反应温度升至50℃,搅拌反应40min,加入A单体,乳化时间60min;加入过硫酸铵溶液6.3g,滴加时间1h,保温反应1h,加入乙基氯硅烷、异丁基三乙氧基硅烷、三氟丙基甲基二氯硅烷和四丁基溴化铵,反应时间2h,得核层乳液;向核层乳液偶氮二异丁基脒盐酸盐,80℃保温反应时间2h,加入己二酸二辛酯,保温反应2h,降温到60℃,加氨水调pH值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料,所得涂料弥补了航空皮革坐垫用涂饰剂差的缺陷。
Description
技术领域
本发明涉及一种涂饰剂和涂料的制备方法,特别涉及一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法。
背景技术
防水材料主要应用领域包括房屋建筑的屋面、地下、外墙和室内;城市道路桥梁和地下空间等市政工程;高速公路和高速铁路的桥梁、隧道;地下铁道等交通工程;引水渠、水库、坝体、水利发电站及水处理等水利工程,适用于屋面和厕浴间、地下室、蓄水池、墙面的防水,防渗、防潮。按照应用材料来分可用于造纸、纺织、皮革等领域。
丙烯酸酯类树脂是目前广泛应用的一类涂料(用于皮革叫涂饰剂),广泛用于航空、造船、车辆、机械、电子工业、建筑、制革等领域,具有成膜柔韧、富有弹性,涂层耐光、耐老化、耐湿擦性能优异、成本低廉等优点。
但线性结构的丙烯酸类树脂涂料属于热塑性材料,容易产生“热粘冷脆”现象,目前常采用核壳乳液聚合法进行改进。
核壳乳液聚合法能较好地降低丙烯酸酯类树脂的玻璃化温度,提高涂料的耐寒性,但对于建筑外墙、制革涂料、机械等领域所使用的材料在较低的温度下使用,该法存在一定缺陷。
发明内容
本发明采用核壳技术分别制备丙烯酸酯类树脂,在核层中加入乙基氯硅烷、异丁基三乙氧基硅烷、三氟丙基甲基二氯硅烷、甲基苯基二氯硅烷重量、三甲基硅烷基二乙胺、一苯基三氯硅烷重量、六甲基环三硅氧烷和二苯基二氯硅烷重、3-烯丙氧丙基三甲氧基硅、十二烷基三苯基氯化鏻、乙烯基三甲氧基硅烷作为防水材料,利用四丁基溴化铵,三亚乙基四胺、三羟甲基丙烷、邻氨基苯酚和二亚乙基三胺作为防水材料的协效剂,提高丙烯酸酯类树脂的防水性,同时采用山柰酚-3-O-β-龙胆二糖苷作为耐寒材料,麦角固醇、2-甲基-2-硝基-1-丙醇、β-谷甾醇、乙酸异冰片酯、大黄酚对丙烯酸酯类树脂的壳层进行交联,提高丙烯酸酯类树脂的耐寒性,所得涂料具有良好的防水和耐候性,弥补了传统涂料该方面的缺陷。
1. 一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法,其特征在于:
(1)向250ml 三口瓶中加入去离子水50g、二丁基萘磺酸钠0.6g、OS-15重量0.3g、丙烯酸0.4g,将反应温度升至50℃,搅拌反应40min,加入A 单体,乳化时间60min;当温度升到70℃时通回流水,到温度80℃时开始滴加用6g水溶解的过硫酸铵溶液6.3g,滴加时间1h,保温反应1h,加入异丁基三乙氧基硅烷1g、三氟丙基甲基二氯硅烷0.2g和四丁基溴化铵0.05g,反应时间2h,得核层乳液;
A 单体及其用量:A 单体由丙烯酸羟乙酯4g、季戊四醇三丙烯酸酯3g、丙烯酸羟丙酯2.0g 混合组成;
(2)向200ml 烧杯中加入60g 的去离子水、纳米氧化锆3g、三聚磷酸钠4g 和海藻酸钠3g,温度为40℃,剪切搅拌速度800rpm,调节体系pH7~8,搅拌时间30min,得纳米材料分散液备用;
(3)向核层乳液中同时滴加B单体和用7g 水溶解的偶氮二异丁基脒盐酸盐溶液7.4g,滴加时间2h,80℃保温反应时间2h,滴加己二酸二辛酯3g、上述纳米材料分散液4g、山柰酚-3-O-β-龙胆二糖苷0.21g和麦角固醇0.26g,保温反应2h,降温到60℃,将OS-15 重量0.4g加入三口瓶中,反应时间40min,加氨水调pH 值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料;
B 单体及其用量:B 单体由丙烯酸羟丁酯4g、甲基丙烯酸甲酯1.5g、丙烯酸乙酯2.5g、丙烯酸十二酯4g 混合组成。
2. 一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法,其特征在于:
(1)向250ml 三口瓶中加入去离子水60g、二丁基萘磺酸钠1.6g、OS-15重量0.6g,丙烯酸5.0g,将反应温度升至55℃,搅拌反应40min,加入A单体,乳化时间60min;当温度升到70℃时通回流水,到温度80℃时开始滴加用6g去离子水溶解的过硫酸铵溶液6.5g,滴加时间2h,保温反应2h,加入甲基苯基二氯硅烷重量3g、三甲基硅烷基二乙胺1.2g和三亚乙基四胺0.1g,反应时间3h,得核层乳液;
A 单体及其用量:A 单体由丙烯酸羟乙酯7g、季戊四醇三丙烯酸酯5g、丙烯酸羟丙酯4g、2- 苯氧基乙基丙烯酸酯5g 混合组成;
(2)向200ml 烧杯中加入70g的去离子水、纳米三氧化二铬4g、六偏磷酸钠10g 和海藻酸钠4g,温度为40℃,剪切搅拌速度1500rpm,调节体系pH7~8,搅拌时间30min,得纳米材料分散液备用;
(3)向核层乳液中同时滴加B单体和用3g水溶解的偶氮二异丁咪唑啉盐酸盐溶液3.5g,滴加时间1h,90℃保温反应时间0.5h,滴加己二酸二异癸酯8g、上述纳米材料分散液12g和2-甲基-2-硝基-1-丙醇0.3g,保温反应2h,降温到40℃,将OS-15重量0.4g加入三口瓶中,反应时间40min,加氨水调pH 值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料;
B 单体及其用量:B 单体由丙烯酸羟丁酯重量4g、甲基丙烯酸甲酯重量3.8g、丙烯酸乙酯重量7.5g、丙烯酸十二酯重量4.5g 混合组成。
3. 一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法,其特征在于:
(1)向250ml 三口瓶中加入去离子水58g、二丁基萘磺酸钠0.8g、OS-15重量0.3g、丙烯酸2.4g,将反应温度升至55℃,搅拌40min,加入A 单体,乳化时间40min;当温度升到70℃时通回流水,到温度80℃时开始滴加用6g蒸馏水溶解的过硫酸铵溶液6.4g,滴加时间2.0h,保温反应2.0h,加入一苯基三氯硅烷4g、六甲基环三硅氧烷0.2g和二亚乙基三胺0.3g,反应时间2h,得核层乳液;
A 单体及其用量:A 单体由丙烯酸羟乙酯7.5g、季戊四醇三丙烯酸酯6g、丙烯酸羟丙酯4g、2-苯氧基乙基丙烯酸酯2.5g 混合组成;
(2)向200ml 烧杯中加入60g 的去离子水、纳米三氧化二铬 3.5g、焦磷酸钠8g 和海藻酸钠2.5g,温度为40℃,剪切搅拌速度800rpm,调节体系pH7~8,搅拌时间20min,得纳米材料分散液备用;
(3)向核层乳液中同时滴加B单体和用6g水溶解的偶氮二氰基戊酸溶液6.5g,滴加时间2.0h,85℃保温反应时间2.5h,滴加壬二酸二辛酯8.5g 、上述纳米材料分散液20g和β-谷甾醇0.6g,保温反应2h,降温到50℃,将OS-15重量0.4g 加入反应体系中,反应时间30min,加氨水调pH 值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料;
B 单体及其用量:B 单体由丙烯酸羟丁酯4g、甲基丙烯酸甲酯2g、丙烯酸乙酯5g、丙烯酸十二酯4g 混合组成。
4. 一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法,其特征在于:
(1)向250ml 三口瓶中加入去离子水48g、二丁基萘磺酸钠0.75g、OS-15重量0.25g、丙烯酸2.6g,将反应温度升至45℃,搅拌30min,加入A单体,乳化时间60min;当温度升到70℃时通回流水,到温度80℃时开始滴加用9g蒸馏水溶解的过硫酸铵溶液9.4g,滴加时间0.5h,保温反应0.5h,加入二苯基二氯硅烷5g、3-烯丙氧丙基三甲氧基硅2g和三羟甲基丙烷0.2g,反应时间3h,得核层乳液;
A 单体及其用量:A 单体由丙烯酸羟乙酯5.5g、季戊四醇三丙烯酸酯6g、丙烯酸羟丙酯4g、2- 苯氧基乙基丙烯酸酯2.5g 混合组成;
(2)向200ml 烧杯中加入65g 的去离子水、纳米铬酸镁 3.5g、三乙基己基磷酸25g 和羟丙基甲基纤维素3g,温度为30℃,剪切搅拌速度1600rpm,调节体系pH7~8,搅拌时间20min,得纳米材料分散液备用;
(3)向核层乳液中同时滴加B 单体和用5g 水溶解的偶氮二异丙基咪唑啉溶液6.5g,滴加时间2.5h,85℃保温反应时间1.5h,加入癸二酸二辛酯8.5g 、上述纳米材料分散液20g、乙酸异冰片酯0.31g和N-丁基二乙醇胺0.2g,保温反应2h,降温到50℃,将OS-15重量0.4g加入三口瓶中,反应时间60min,加氨水调pH 值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料;
B 单体及其用量:B 单体由丙烯酸羟丁酯5g、甲基丙烯酸甲酯3g、丙烯酸乙酯6g、丙烯酸十二酯4g 混合组成。
5. 一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法,其特征在于:
(1)向三口瓶中加入水50g、乳化剂十二烷基苯磺酸钠0.33g与脂肪醇聚氧乙烯醚0.17g、甲基丙烯酸0.3g,将反应温度升至40℃,搅拌15min,加入A单体,乳化时间30min。当温度升到70℃通回流水,到温度75℃时开始滴加用5g水溶解的过硫酸钾溶液5.2g,滴加时间1h,保温反应3h,加入十二烷基三苯基氯化鏻1g、乙烯基三甲氧基硅烷1.2g和邻氨基苯酚0.2g,搅拌反应时间1h,得核层乳液;
A单体及其用量:A单体由丙烯酸丁酯6g、甲基丙烯酸甲酯4g、丙烯酸乙酯2.5g的混合组成;
(2)向核层乳液中同时滴加B单体和用5g水溶解的过硫酸钾溶液5.3g,滴加时间1h,75℃保温反应时间2h,滴加邻碳硼烷10g,保温反应1h,再滴加3-羧基苯硼酸频那醇酯0.5g,保温反应时间1h,降温到50℃,将乳化剂十二烷基苯磺酸钠0.2g、脂肪醇聚氧乙烯醚0.1g、大黄酚0.21g和N,N-二苄基乙醇胺0.5g加入到三口瓶中,搅拌时间30min,加氨水调pH值7,得到航空皮革坐垫用涂饰剂;
B单体及其用量:B单体由丙烯酸丁酯3g、甲基丙烯酸甲酯3.5g、丙烯酸乙酯3.5g混合组成。
本发明具有以下特点:
(1)所制备的丙烯酸酯类树脂涂料相容性好,可明显改善传统丙烯酸类树脂冷脆的缺陷;
(2)利用乙基氯硅烷、异丁基三乙氧基硅烷、三氟丙基甲基二氯硅烷、甲基苯基二氯硅烷重量、三甲基硅烷基二乙胺、一苯基三氯硅烷重量、六甲基环三硅氧烷和二苯基二氯硅烷重、3-烯丙氧丙基三甲氧基硅、十二烷基三苯基氯化鏻、乙烯基三甲氧基硅烷作为防水材料,利用四丁基溴化铵,三亚乙基四胺、三羟甲基丙烷、邻氨基苯酚和二亚乙基三胺作为防水材料的协效剂;
(3)有机硅化合物一般由碳、氢、氧、硅等元素构成,硅氧键键能高达 443.5 k J/mol,可对硅原子上连接的烃基受热氧化起屏蔽作用,赋予聚合物耐热、抗氧化、耐辐射等性能。硅氧烷分子呈螺旋状结构,如硅原子上连接有甲基,则甲基向外排列并绕硅氧键旋转,由于分子体积大,内部密度低,因而能阻止液态水通过,但气态水却能很顺利通过,从而赋予树脂涂层憎水、表面张力低、耐污染等性能。利用有机硅材料的上述特性,将硅氧烷大分子或带有烷氧基的硅氧烷引入到丙烯酸聚合物的主链上,可以使这类树脂兼有丙烯酸和有机硅两类树脂的优点。用这类树脂制备的施工于建筑物表面时,聚合物间、聚合物与基材之间可形成牢固的硅—氧—硅立体网状结构,使得涂膜强度增加,防水性及耐候性增强;
(4)山柰酚-3-O-β-龙胆二糖苷作为耐寒材料,麦角固醇、2-甲基-2-硝基-1-丙醇、β-谷甾醇、乙酸异冰片酯、大黄酚、N,N-二苄基乙醇胺、N-丁基二乙醇胺、柠檬酸钠、葡萄糖酸对丙烯酸酯类树脂的壳层进行交联,提高丙烯酸酯类树脂的耐寒性(耐候性);
(5) 脂肪醇聚氧乙烯醚的型号为OS-15,非离子型,购于江苏省海安石油化工厂,下同;
(6)纳米氧化锆增加涂饰剂的绝缘性。
具体实施方式
实例一
(1)向250ml 三口瓶中加入去离子水50g、二丁基萘磺酸钠0.6g、OS-15重量0.3g、丙烯酸0.4g,将反应温度升至50℃,搅拌反应40min,加入A 单体,乳化时间60min;当温度升到70℃时通回流水,到温度80℃时开始滴加用6g水溶解的过硫酸铵溶液6.3g,滴加时间1h,保温反应1h,加入异丁基三乙氧基硅烷1g、三氟丙基甲基二氯硅烷0.2g和四丁基溴化铵0.05g,反应时间2h,得核层乳液;
A 单体及其用量:A 单体由丙烯酸羟乙酯4g、季戊四醇三丙烯酸酯3g、丙烯酸羟丙酯2.0g 混合组成;
(2)向200ml 烧杯中加入60g 的去离子水、纳米氧化锆3g、三聚磷酸钠4g 和海藻酸钠3g,温度为40℃,剪切搅拌速度800rpm,调节体系pH7~8,搅拌时间30min,得纳米材料分散液备用;
(3)向核层乳液中同时滴加B单体和用7g 水溶解的偶氮二异丁基脒盐酸盐溶液7.4g,滴加时间2h,80℃保温反应时间2h,滴加己二酸二辛酯3g、加入上述纳米材料分散液4g、山柰酚-3-O-β-龙胆二糖苷0.21g和麦角固醇0.26g,保温反应2h,降温到60℃,将OS-15重量0.4g加入三口瓶中,反应时间40min,加氨水调pH 值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料;
B 单体及其用量:B 单体由丙烯酸羟丁酯4g、甲基丙烯酸甲酯1.5g、丙烯酸乙酯2.5g、丙烯酸十二酯4g 混合组成。
实例二
(1)向250ml 三口瓶中加入去离子水60g、二丁基萘磺酸钠1.6g、OS-15重量0.6g,丙烯酸5.0g,将反应温度升至55℃,搅拌反应40min,加入A单体,乳化时间60min;当温度升到70℃时通回流水,到温度80℃时开始滴加用6g去离子水溶解的过硫酸铵溶液6.5g,滴加时间2h,保温反应2h,加入甲基苯基二氯硅烷重量3g、三甲基硅烷基二乙胺1.2g和三亚乙基四胺0.1g,反应时间3h,得核层乳液;
A 单体及其用量:A 单体由丙烯酸羟乙酯7g、季戊四醇三丙烯酸酯5g、丙烯酸羟丙酯4g、2- 苯氧基乙基丙烯酸酯5g 混合组成;
(2)向200ml 烧杯中加入70g的去离子水、纳米三氧化二铬4g、六偏磷酸钠10g 和海藻酸钠4g,温度为40℃,剪切搅拌速度1500rpm,调节体系pH7~8,搅拌时间30min,得纳米材料分散液备用;
(3)向核层乳液中同时滴加B单体和用3g水溶解的偶氮二异丁咪唑啉盐酸盐溶液3.5g,滴加时间1h,90℃保温反应时间0.5h,滴加己二酸二异癸酯8g、加入上述纳米材料分散液12g和2-甲基-2-硝基-1-丙醇0.3g,保温反应2h,降温到40℃,将OS-15重量0.4g加入三口瓶中,反应时间40min,加氨水调pH 值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料;
B 单体及其用量:B 单体由丙烯酸羟丁酯重量4g、甲基丙烯酸甲酯重量3.8g、丙烯酸乙酯重量7.5g、丙烯酸十二酯重量4.5g 混合组成。
实例三
(1)向250ml 三口瓶中加入去离子水58g、二丁基萘磺酸钠0.8g、OS-15重量0.3g、丙烯酸2.4g,将反应温度升至55℃,搅拌40min,加入A 单体,乳化时间40min;当温度升到70℃时通回流水,到温度80℃时开始滴加用6g蒸馏水溶解的过硫酸铵溶液6.4g,滴加时间2.0h,保温反应2.0h,加入一苯基三氯硅烷4g、六甲基环三硅氧烷0.2g和二亚乙基三胺0.3g,反应时间2h,得核层乳液;
A 单体及其用量:A 单体由丙烯酸羟乙酯7.5g、季戊四醇三丙烯酸酯6g、丙烯酸羟丙酯4g、2-苯氧基乙基丙烯酸酯2.5g 混合组成;
(2)向200ml 烧杯中加入60g 的去离子水、纳米三氧化二铬 3.5g、焦磷酸钠8g 和海藻酸钠2.5g,温度为40℃,剪切搅拌速度800rpm,调节体系pH7~8,搅拌时间20min,得纳米材料分散液备用;
(3)向核层乳液中同时滴加B单体和用6g水溶解的偶氮二氰基戊酸溶液6.5g,滴加时间2.0h,85℃保温反应时间2.5h,滴加壬二酸二辛酯8.5g、加入上述纳米材料分散液20g和β-谷甾醇0.6g,保温反应2h,降温到50℃,将OS-15重量0.4g 加入反应体系中,反应时间30min,加氨水调pH 值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料;
B 单体及其用量:B 单体由丙烯酸羟丁酯4g、甲基丙烯酸甲酯2g、丙烯酸乙酯5g、丙烯酸十二酯4g 混合组成。
实例四
(1)向250ml 三口瓶中加入去离子水48g、二丁基萘磺酸钠0.75g、OS-15重量0.25g、丙烯酸2.6g,将反应温度升至45℃,搅拌30min,加入A单体,乳化时间60min;当温度升到70℃时通回流水,到温度80℃时开始滴加用9g蒸馏水溶解的过硫酸铵溶液9.4g,滴加时间0.5h,保温反应0.5h,加入二苯基二氯硅烷5g、3-烯丙氧丙基三甲氧基硅2g和三羟甲基丙烷0.2g,反应时间3h,得核层乳液;
A 单体及其用量:A 单体由丙烯酸羟乙酯5.5g、季戊四醇三丙烯酸酯6g、丙烯酸羟丙酯4g、2- 苯氧基乙基丙烯酸酯2.5g 混合组成;
(2)向200ml 烧杯中加入65g 的去离子水、纳米铬酸镁 3.5g、三乙基己基磷酸25g 和羟丙基甲基纤维素3g,温度为30℃,剪切搅拌速度1600rpm,调节体系pH7~8,搅拌时间20min,得纳米材料分散液备用;
(3)向核层乳液中同时滴加B 单体和用5g 水溶解的偶氮二异丙基咪唑啉溶液6.5g,滴加时间2.5h,85℃保温反应时间1.5h,加入癸二酸二辛酯8.5g、加入上述纳米材料分散液20g、乙酸异冰片酯0.31g和N-丁基二乙醇胺0.2g,保温反应2h,降温到50℃,将OS-15重量0.4g 加入三口瓶中,反应时间60min,加氨水调pH 值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料;
B 单体及其用量:B 单体由丙烯酸羟丁酯5g、甲基丙烯酸甲酯3g、丙烯酸乙酯6g、丙烯酸十二酯4g 混合组成。
实例五
(1)向三口瓶中加入水50g、乳化剂十二烷基苯磺酸钠0.33g与脂肪醇聚氧乙烯醚0.17g、甲基丙烯酸0.3g,将反应温度升至40℃,搅拌15min,加入A单体,乳化时间30min。当温度升到70℃通回流水,到温度75℃时开始滴加用5g水溶解的过硫酸钾溶液5.2g,滴加时间1h,保温反应3h,加入十二烷基三苯基氯化鏻1g、乙烯基三甲氧基硅烷1.2g和邻氨基苯酚0.2g,搅拌反应时间1h,得核层乳液;
A单体及其用量:A单体由丙烯酸丁酯6g、甲基丙烯酸甲酯4g、丙烯酸乙酯2.5g的混合组成;
(2)向核层乳液中同时滴加B单体和用5g水溶解的过硫酸钾溶液5.3g,滴加时间1h,75℃保温反应时间2h,滴加邻碳硼烷10g,保温反应1h,再滴加3-羧基苯硼酸频那醇酯0.5g,保温反应时间1h,降温到50℃,将乳化剂十二烷基苯磺酸钠0.2g、脂肪醇聚氧乙烯醚0.1g、大黄酚0.21g、N,N-二苄基乙醇胺0.5g、柠檬酸钠0.3g和葡萄糖酸0.1g加入到三口瓶中,搅拌时间30min,加氨水调pH值7,得到航空皮革坐垫用涂饰剂;
B单体及其用量:B单体由丙烯酸丁酯3g、甲基丙烯酸甲酯3.5g、丙烯酸乙酯3.5g混合组成。
下面结合实例进一步说明本发明。
表一和表二是本发明实例一到实例五所制备的航空皮革坐垫用涂饰剂的耐寒性温度,美利欧树脂A-777.A为市场涂饰剂,由克莱恩化工生产。
表一 航空皮革坐垫用涂饰剂耐寒温度
名称 | 实例一 | 实例二 | 实例三 | 实例四 | 实例五 | 市场 |
耐寒温度/℃ | -15 | -36 | -27 | -18 | -19 | -10 |
由表一可知,使用了本发明耐寒性丙烯酸酯类树脂涂饰剂所成膜后,耐寒温度大幅降低。
表二 航空皮革坐垫用涂饰剂在零下20℃的柔软性
表三 航空皮革坐垫用涂饰剂耐所成膜耐水性
实验组 | 实例一 | 实例二 | 实例三 | 实例四 | 实例五 | 市场 |
膜外观(耐水性48h) | 透明 | 透明 | 透明 | 透明 | 透明 | 发白 |
防水性采用取适量乳液均匀涂覆于玻璃板上,一定温度下干燥成膜后将玻璃板放入去离子水中浸泡,观察涂膜变蓝、发白、起泡、发皱、脱落的情况。
从表三可以发现,从膜的耐水性能较好。
Claims (5)
1.一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法,其特征在于:
(1)向250ml 三口瓶中加入去离子水50g、二丁基萘磺酸钠0.6g、OS-15重量0.3g、丙烯酸0.4g,将反应温度升至50℃,搅拌反应40min,加入A 单体,乳化时间60min;当温度升到70℃时通回流水,到温度80℃时开始滴加用6g水溶解的过硫酸铵溶液6.3g,滴加时间1h,保温反应1h,加入异丁基三乙氧基硅烷1g、三氟丙基甲基二氯硅烷0.2g和四丁基溴化铵0.05g,反应时间2h,得核层乳液;
A 单体及其用量:A 单体由丙烯酸羟乙酯4g、季戊四醇三丙烯酸酯3g、丙烯酸羟丙酯2.0g 混合组成;
(2)向200ml 烧杯中加入60g 的去离子水、纳米氧化锆3g、三聚磷酸钠4g 和海藻酸钠3g,温度为40℃,剪切搅拌速度800rpm,调节体系pH7~8,搅拌时间30min,得纳米材料分散液备用;
(3)向核层乳液中同时滴加B单体和用7g 水溶解的偶氮二异丁基脒盐酸盐溶液7.4g,滴加时间2h,80℃保温反应时间2h,滴加己二酸二辛酯3g、上述纳米材料分散液4g、山柰酚-3-O-β-龙胆二糖苷0.21g和麦角固醇0.26g,保温反应2h,降温到60℃,将OS-15 重量0.4g加入三口瓶中,反应时间40min,加氨水调pH 值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料;
B 单体及其用量:B 单体由丙烯酸羟丁酯4g、甲基丙烯酸甲酯1.5g、丙烯酸乙酯2.5g、丙烯酸十二酯4g 混合组成。
2.一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法,其特征在于:
(1)向250ml 三口瓶中加入去离子水60g、二丁基萘磺酸钠1.6g、OS-15重量0.6g,丙烯酸5.0g,将反应温度升至55℃,搅拌反应40min,加入A单体,乳化时间60min;当温度升到70℃时通回流水,到温度80℃时开始滴加用6g去离子水溶解的过硫酸铵溶液6.5g,滴加时间2h,保温反应2h,加入甲基苯基二氯硅烷重量3g、三甲基硅烷基二乙胺1.2g和三亚乙基四胺0.1g,反应时间3h,得核层乳液;
A 单体及其用量:A 单体由丙烯酸羟乙酯7g、季戊四醇三丙烯酸酯5g、丙烯酸羟丙酯4g、2- 苯氧基乙基丙烯酸酯5g 混合组成;
(2)向200ml 烧杯中加入70g的去离子水、纳米三氧化二铬4g、六偏磷酸钠10g 和海藻酸钠4g,温度为40℃,剪切搅拌速度1500rpm,调节体系pH7~8,搅拌时间30min,得纳米材料分散液备用;
(3)向核层乳液中同时滴加B单体和用3g水溶解的偶氮二异丁咪唑啉盐酸盐溶液3.5g,滴加时间1h,90℃保温反应时间0.5h,滴加己二酸二异癸酯8g、上述纳米材料分散液12g和2-甲基-2-硝基-1-丙醇0.3g,保温反应2h,降温到40℃,将OS-15重量0.4g加入三口瓶中,反应时间40min,加氨水调pH 值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料;
B 单体及其用量:B 单体由丙烯酸羟丁酯重量4g、甲基丙烯酸甲酯重量3.8g、丙烯酸乙酯重量7.5g、丙烯酸十二酯重量4.5g 混合组成。
3.一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法,其特征在于:
(1)向250ml 三口瓶中加入去离子水58g、二丁基萘磺酸钠0.8g、OS-15重量0.3g、丙烯酸2.4g,将反应温度升至55℃,搅拌40min,加入A 单体,乳化时间40min;当温度升到70℃时通回流水,到温度80℃时开始滴加用6g蒸馏水溶解的过硫酸铵溶液6.4g,滴加时间2.0h,保温反应2.0h,加入一苯基三氯硅烷4g、六甲基环三硅氧烷0.2g和二亚乙基三胺0.3g,反应时间2h,得核层乳液;
A 单体及其用量:A 单体由丙烯酸羟乙酯7.5g、季戊四醇三丙烯酸酯6g、丙烯酸羟丙酯4g、2-苯氧基乙基丙烯酸酯2.5g 混合组成;
(2)向200ml 烧杯中加入60g 的去离子水、纳米三氧化二铬 3.5g、焦磷酸钠8g 和海藻酸钠2.5g,温度为40℃,剪切搅拌速度800rpm,调节体系pH7~8,搅拌时间20min,得纳米材料分散液备用;
(3)向核层乳液中同时滴加B单体和用6g水溶解的偶氮二氰基戊酸溶液6.5g,滴加时间2.0h,85℃保温反应时间2.5h,滴加壬二酸二辛酯8.5g 、上述纳米材料分散液20g和β-谷甾醇0.6g,保温反应2h,降温到50℃,将OS-15重量0.4g 加入反应体系中,反应时间30min,加氨水调pH 值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料;
B 单体及其用量:B 单体由丙烯酸羟丁酯4g、甲基丙烯酸甲酯2g、丙烯酸乙酯5g、丙烯酸十二酯4g 混合组成。
4.一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法,其特征在于:
(1)向250ml 三口瓶中加入去离子水48g、二丁基萘磺酸钠0.75g、OS-15重量0.25g、丙烯酸2.6g,将反应温度升至45℃,搅拌30min,加入A单体,乳化时间60min;当温度升到70℃时通回流水,到温度80℃时开始滴加用9g蒸馏水溶解的过硫酸铵溶液9.4g,滴加时间0.5h,保温反应0.5h,加入二苯基二氯硅烷5g、3-烯丙氧丙基三甲氧基硅2g和三羟甲基丙烷0.2g,反应时间3h,得核层乳液;
A 单体及其用量:A 单体由丙烯酸羟乙酯5.5g、季戊四醇三丙烯酸酯6g、丙烯酸羟丙酯4g、2- 苯氧基乙基丙烯酸酯2.5g 混合组成;
(2)向200ml 烧杯中加入65g 的去离子水、纳米铬酸镁 3.5g、三乙基己基磷酸25g 和羟丙基甲基纤维素3g,温度为30℃,剪切搅拌速度1600rpm,调节体系pH7~8,搅拌时间20min,得纳米材料分散液备用;
(3)向核层乳液中同时滴加B 单体和用5g 水溶解的偶氮二异丙基咪唑啉溶液6.5g,滴加时间2.5h,85℃保温反应时间1.5h,加入癸二酸二辛酯8.5g 、上述纳米材料分散液20g、乙酸异冰片酯0.31g和N-丁基二乙醇胺0.2g,保温反应2h,降温到50℃,将OS-15重量0.4g加入三口瓶中,反应时间60min,加氨水调pH 值7~8,得到航空皮革坐垫用涂饰剂、建筑外墙涂料;
B 单体及其用量:B 单体由丙烯酸羟丁酯5g、甲基丙烯酸甲酯3g、丙烯酸乙酯6g、丙烯酸十二酯4g 混合组成。
5.一种航空皮革坐垫用涂饰剂、建筑外墙涂料的制备方法,其特征在于:
(1)向三口瓶中加入水50g、乳化剂十二烷基苯磺酸钠0.33g与脂肪醇聚氧乙烯醚0.17g、甲基丙烯酸0.3g,将反应温度升至40℃,搅拌15min,加入A单体,乳化时间30min;
当温度升到70℃通回流水,到温度75℃时开始滴加用5g水溶解的过硫酸钾溶液5.2g,滴加时间1h,保温反应3h,加入十二烷基三苯基氯化鏻1g、乙烯基三甲氧基硅烷1.2g和邻氨基苯酚0.2g,搅拌反应时间1h,得核层乳液;
A单体及其用量:A单体由丙烯酸丁酯6g、甲基丙烯酸甲酯4g、丙烯酸乙酯2.5g的混合组成;
(2)向核层乳液中同时滴加B单体和用5g水溶解的过硫酸钾溶液5.3g,滴加时间1h,75℃保温反应时间2h,滴加邻碳硼烷10g,保温反应1h,再滴加3-羧基苯硼酸频那醇酯0.5g,保温反应时间1h,降温到50℃,将乳化剂十二烷基苯磺酸钠0.2g、脂肪醇聚氧乙烯醚0.1g、大黄酚0.21g和N,N-二苄基乙醇胺0.5g加入到三口瓶中,搅拌时间30min,加氨水调pH值7,得到航空皮革坐垫用涂饰剂;
B单体及其用量:B单体由丙烯酸丁酯3g、甲基丙烯酸甲酯3.5g、丙烯酸乙酯3.5g混合组成。
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