CN108102061A - 一种水性三防漆用聚氨酯的合成方法 - Google Patents
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Abstract
本发明涉及水性漆领域,尤其涉及一种水性三防漆用聚氨酯的合成方法,采用聚酯多元醇3000和异氰酸酯反应,用羧酸盐和磺酸盐两种水性扩链剂双重扩链改性聚氨酯,使得做出来的聚氨酯固含量更高,可以达到45‑50%,水溶性更强,稳定性更好,用此树酯做出来的三防漆耐磨、耐化学性、耐高低温,耐湿热,耐盐雾性能优越,特别是以水为稀释剂,不含有机溶剂,具有无毒无害、无污染、安全环保、不燃不爆、施工方便和不影响生态环境等特点。适用于各种环境下、不同电子电气产品线路板的防腐,符合国家安全环保政策的要求。
Description
技术领域
本发明涉及三防漆技术领域,尤其涉及一种水性三防漆用聚氨酯的合成方法。
背景技术
随着环保要求的越来越高,溶剂型的涂料逐渐被淘汰,水性产品是必然的发展趋势,目前市面上三防漆主要还是以油性为主,使用大量的溶剂严重污染人们生活的环境,危害人们的身体健康,少量的水性产品又存在硬度低,耐盐雾性能差等缺点,因此开发一款耐磨、耐化学性、耐高低温,耐湿热,耐盐性能优越,而且是以水为稀释剂,不含有机溶剂,安全环保、不燃不爆、无毒、无害、无污染、施工方便、不影响生态平衡、符合国家环保政策的三防漆树脂显得尤为重要,具有广阔的市场前景。
发明内容
为解决上述问题,我们提出了一种水性三防漆用聚氨酯的合成方法,用此方法制得的三防漆耐盐雾、耐冷热循环、耐低温性能卓越。
为实现上述需求,本发明通过以下技术方案来实现上述目的:一种水性三防漆用聚氨酯的合成方法,包括以下步骤:
第一步,将一定量的聚酯多元醇加入四口瓶中于100-110℃条件下真空脱水0.5-1h,而后在80-85℃下加入羧酸型亲水扩链剂,搅拌10min后加入异氰酸酯和少量催化剂二月桂酸二丁基锡(DBTDL),温度控制在70-80℃反应1-3h,其中DBTDL的加入量为1-5‰,羧酸型亲水扩链剂的加入量为0.2-1%,R=NCO/OH=1.7-2.0;
第二步,在60-70℃条件下向所述第一步得到的体系中加入1,4-丁二醇于60-70℃左右反应2-4h,而后加入一定量的丙酮使粘度降到600-1200Pa·s,丙酮用量为乳液固含量的2-3倍;而后向上述体系中加入固含量0.01-0.08%的三乙胺和固含量2-8%的磺酸盐亲水扩链剂扩链45-70min至粘度稳定,温度保持在55-65℃,即得到聚氨酯预聚体。
第三步,将第二步所得的预聚体倒入分散桶中降低至室温,边高速搅拌边加水,形成自乳化体系,而后加入多元胺扩链5-15min,最后蒸出丙酮即得水性三防漆用聚氨酯,其中磺酸盐亲水扩链剂的用量占固体份的质量百分比为2-8%,水的加入量根据所需制得的固含量比值计算;
所述第一步中的多元醇分子量为2000-3000。
进一步地,一种水性三防漆用聚氨酯的合成方法,所述的二异氰酸酯为异氟尔酮二异氰酸酯IPDI、六亚甲基二异氰酸酯HDI、甲苯二异氰酸酯、4,4-二苯基甲烷二异氰酸酯、氢化苯基甲烷二异氰酸酯、环戊二异氰酸酯中的一种或几种混合物。
进一步地,一种水性三防漆用聚氨酯的合成方法,所述的羧酸型亲水扩链剂为二羟甲基丙酸、二羟甲基丁酸中的一种或几种混合物。
进一步地,一种水性三防漆用聚氨酯的合成方法,所述的磺酸盐亲水扩链剂为1,2-二羟基-3-丙磺酸钠、乙二胺基乙磺酸钠、1,4-丁二醇-2-磺酸钠、2,4-二氨基苯磺酸钠中的一种或多种混合物。
进一步地,一种水性三防漆用聚氨酯的合成方法,所述的有机胺中和剂为氨水、三乙醇胺、甲胺、三乙胺、二乙醇胺、N-甲基二乙醇胺、氨基甲酸甲酯、2-氨基-2-甲基1-丙醇(AMP)、乙二胺、乙胺中的一种或几种混合物。
进一步地,一种水性三防漆用聚氨酯的合成方法,所述的多元胺扩链剂为乙二胺、己二胺、二乙烯三胺、异氟尔酮二胺、2-甲基戊二胺中的一种或几种混合物。
更具体地,一种水性三防漆用聚氨酯的合成方法,包括以下步骤:
第一步,将一定量的聚酯多元醇(分子量2000-3000)加入四口瓶中于100-110℃条件下真空脱水0.5-1h,而后在80-85℃下加入羧酸型亲水扩链剂,搅拌10min后加入异氰酸酯和少量催化剂二月桂酸二丁基锡(DBTDL),温度控制在70-80℃反应1-3h,其中DBTDL的加入量为1-5‰,羧酸型亲水扩链剂的加入量为0.2-1%(质量百分比),R值调整到2左右;
第二步,在60~70℃条件下向步骤1)体系中加入1,4-BDO于60-70℃左右反应2-4h,而后加入一定量的丙酮降粘,丙酮用量为乳液固含量的2-3倍;而后向体系中加入一定量的三乙胺和磺酸盐亲水扩链剂扩链45-70min至粘度稳定,温度保持在55-65℃。
第三步,将步骤2)所得的预聚体倒入分散桶中将至室温,边高速搅拌边加水,形成自乳化体系,而后加入多元胺扩链5-15min,最后蒸出丙酮即得一种性能优越的水性三防漆用聚氨酯,其中磺酸盐亲水扩链剂的用量为2-8%(占固体份的质量百分比),水的加入量根据所需制得的固含量比值计算。。
更具体地,水性三防漆用聚氨酯的合成方法,所述的二异氰酸酯为异氟尔酮二异氰酸酯IPDI、六亚甲基二异氰酸酯HDI、甲苯二异氰酸酯、4,4-二苯基甲烷二异氰酸酯、氢化苯基甲烷二异氰酸酯、环戊二异氰酸酯中的一种或几种混合物。
更具体地,水性三防漆用聚氨酯的合成方法,所述的羧酸型亲水扩链剂为二羟甲基丙酸、二羟甲基丁酸中的一种或几种混合物。
更具体地,水性三防漆用聚氨酯的合成方法,所述的磺酸盐亲水扩链剂为1,2-二羟基-3-丙磺酸钠、乙二胺基乙磺酸钠、1,4-丁二醇-2-磺酸钠、2,4-二氨基苯磺酸钠中的一种或多种混合物。
更具体地,水性三防漆用聚氨酯的合成方法,所述的有机胺中和剂为氨水、三乙醇胺、甲胺、三乙胺、二乙醇胺、N-甲基二乙醇胺、氨基甲酸甲酯、2-氨基-2-甲基1-丙醇(AMP)、乙二胺、乙胺中的一种或几种混合物。
更具体地,水性三防漆用聚氨酯的合成方法,所述的多元胺扩链剂为乙二胺、己二胺、二乙烯三胺、异氟尔酮二胺、2-甲基戊二胺中的一种或几种混合物。
本发明的有益效果在于:本发明的优点:
(1)本发明采用羧酸型和磺酸盐性双重亲水扩链剂进行扩链,解决了单一使用磺酸盐性扩链剂制得的乳液分散乳化效果不好、产品易絮凝的缺点,做出来的产品稳定性好。
(2)本发明多元胺扩链剂选择在加水自乳化后加入,避免扩链反应剧烈,粘度剧增,出现爬杆现象。
(3)本发明为水性树脂,不含有机溶剂,环保安全毒性小。
(4)本发明做出来的树脂水溶性好,而且固含量可以达到50%左右,用此树脂调配出来的三防漆耐水、耐盐雾性能好。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例中的技术方案进行清楚、完整地描述。显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施案例1:
第一步,将480g的聚酯多元醇(分子量3000)加入四口瓶中于100-110℃条件下真空脱水0.5h,而后在85℃下加入1.5g DMPA亲水扩链剂,搅拌10min后加入71g IPDI和9滴催化剂二月桂酸二丁基锡(DBTDL),温度控制在70-80℃反应2.3h;
第二步,在65℃条件下向步骤1)体系中加入7g 1,4-BDO于65℃左右反应3h,而后加入400g丙酮降粘,而后向体系中加入0.98g的三乙胺和12.6g磺酸盐亲水扩链剂扩链AAS,反应60min至粘度稳定,温度保持在60-65℃。
第三步将第二步所得的预聚体倒入分散桶中将至室温,边高速搅拌边加水550g,形成自乳化体系,而后加入2.3g乙二胺扩链15min,最后蒸出丙酮即得一种性能优越的水性三防漆用聚氨酯,乳白色液体,固含量为50%左右,耐黄变性能优越。
实施案例2:
第一步,将480g的聚酯多元醇(分子量3000)加入四口瓶中于100-110℃条件下真空脱水0.5h,而后在85℃下加入1.5g DMPA亲水扩链剂,搅拌10min后加入48gHDI和8滴催化剂二月桂酸二丁基锡(DBTDL),温度控制在75℃反应2.5h,
第二步,在65℃条件下向第一步体系中加入7.2g 1,4-BDO于65℃左右反应3h,而后加入400g丙酮降粘,而后向体系中加入0.98g的三乙胺和12.6g磺酸盐亲水扩链剂扩链AAS,反应60min至粘度稳定,温度保持在60-65℃。
第三步,将步骤第二步所得的预聚体倒入分散桶中将至室温,边高速搅拌边加水600g,形成自乳化体系,而后加入2.5g乙二胺扩链15min,最后蒸出丙酮即得一种性能优越的水性三防漆用聚氨酯,乳白色液体,固含量为47%左右。
实施案例3:
第一步,将480g的聚酯多元醇(分子量3000)加入四口瓶中于100-110℃条件下真空脱水0.5h,而后在85℃下加入1.5g DMPA亲水扩链剂,搅拌10min后加入35g HDI和12gIPDI以及10滴催化剂二月桂酸二丁基锡(DBTDL),温度控制在70-80℃反应2.3h;
第二步,在65℃条件下向步骤1)体系中加入7g 1,4-BDO于65℃左右反应3h,而后加入400g丙酮降粘,而后向体系中加入0.98g的三乙胺和12.6g磺酸盐亲水扩链剂扩链AAS,反应60min至粘度稳定,温度保持在60-65℃。
第三步,将第二步所得的预聚体倒入分散桶中将至室温,边高速搅拌边加水550g,形成自乳化体系,而后加入2.3g乙二胺扩链15min,最后蒸出丙酮即得一种性能优越的水性三防漆用聚氨酯,乳白色液体,固含量为49%左右,耐黄变性能优越、附着力好、耐盐雾性能好。
实施案例4:
第一步,将480g的聚酯多元醇(分子量3000)加入四口瓶中于100-110℃条件下真空脱水0.5h,而后在85℃下加入1.5g DMPA亲水扩链剂,搅拌10min后加入50g甲苯二异氰酸酯以及8滴催化剂二月桂酸二丁基锡(DBTDL),温度控制在70-80℃反应2.3h;
第二步,在65℃条件下向第一步体系中加入7g 1,4-BDO于65℃左右反应3h,而后加入400g丙酮降粘,而后向体系中加入0.98g的三乙胺和12.6g磺酸盐亲水扩链剂扩链AAS,反应60min至粘度稳定,温度保持在60-65℃。
第三步,将第二步所得的预聚体倒入分散桶中将至室温,边高速搅拌边加水550g,形成自乳化体系,而后加入2.3g乙二胺扩链15min,最后蒸出丙酮即得一种性能优越的水性三防漆用聚氨酯,乳白色液体,固含量为50%左右,用此树脂做出来的三防漆经济实惠、附着力好、耐盐雾性能好。
Claims (6)
1.一种水性三防漆用聚氨酯的合成方法,其特征在于:包括以下步骤:
第一步,将一定量的聚酯多元醇加入四口瓶中于100-110℃条件下真空脱水0.5-1h,而后在80-85℃下加入羧酸型亲水扩链剂,搅拌10min后加入异氰酸酯和少量催化剂二月桂酸二丁基锡(DBTDL),温度控制在70-80℃反应1-3h,其中DBTDL的加入量为1-5‰,羧酸型亲水扩链剂的加入量为0.2-1%,R=NCO/OH=1.7-2.0;
第二步,在60-70℃条件下向所述第一步得到的体系中加入1,4-丁二醇于60-70℃左右反应2-4h,而后加入一定量的丙酮使粘度降到600-1200Pa·s,丙酮用量为乳液固含量的2-3倍;而后向上述体系中加入固含量0.01-0.08%的三乙胺和固含量2-8%的磺酸盐亲水扩链剂扩链45-70min至粘度稳定,温度保持在55-65℃,即得到聚氨酯预聚体。
第三步,将第二步所得的预聚体倒入分散桶中降低至室温,边高速搅拌边加水,形成自乳化体系,而后加入多元胺扩链5-15min,最后蒸出丙酮即得水性三防漆用聚氨酯,其中磺酸盐亲水扩链剂的用量占固体份的质量百分比为2-8%,水的加入量根据所需制得的固含量比值计算;
所述第一步中的多元醇分子量为2000-3000。
2.如权利要求1所述的水性三防漆用聚氨酯的合成方法,其特征在于:所述的二异氰酸酯为异氟尔酮二异氰酸酯IPDI、六亚甲基二异氰酸酯HDI、甲苯二异氰酸酯、4,4-二苯基甲烷二异氰酸酯、氢化苯基甲烷二异氰酸酯、环戊二异氰酸酯中的一种或几种混合物。
3.如权利要求1所述的水性三防漆用聚氨酯的合成方法,其特征在于:所述的羧酸型亲水扩链剂为二羟甲基丙酸、二羟甲基丁酸中的一种或几种混合物。
4.如权利要求1所述的水性三防漆用聚氨酯的合成方法,其特征在于:所述的磺酸盐亲水扩链剂为1,2-二羟基-3-丙磺酸钠、乙二胺基乙磺酸钠、1,4-丁二醇-2-磺酸钠、2,4-二氨基苯磺酸钠中的一种或多种混合物。
5.如权利要求1所述的水性三防漆用聚氨酯的合成方法,其特征在于:所述的有机胺中和剂为氨水、三乙醇胺、甲胺、三乙胺、二乙醇胺、N-甲基二乙醇胺、氨基甲酸甲酯、2-氨基-2-甲基1-丙醇(AMP)、乙二胺、乙胺中的一种或几种混合物。
6.如权利要求1所述的水性三防漆用聚氨酯的合成方法,其特征在于:所述的多元胺扩链剂为乙二胺、己二胺、二乙烯三胺、异氟尔酮二胺、2-甲基戊二胺中的一种或几种混合物。
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