CN105218778B - 一种端环氧基水性聚氨酯树脂及其制备方法 - Google Patents
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Abstract
本发明公开了一种端环氧基水性聚氨酯树脂及其制备方法,所述树脂通过以下步骤制得:植物油多元醇、小分子多元醇、二异氰酸酯和亲水扩链剂在有机溶剂中,在催化剂作用下,加成反应得到端异氰酸酯聚氨酯预聚体;加入端羟基环氧化合物反应,得到端环氧基聚氨酯;再加入胺进行中和,滴加水进行相反转,保温,减压蒸馏除去有机溶剂,得到端环氧基水性聚氨酯树脂。所述树脂为水性涂料,没有挥发性有机物污染,环境友好;是由聚氨酯与环氧树脂化学方法结合制得,所述树脂不仅具有聚氨酯的柔韧性,还具有环氧树脂的刚性、粘结性的特点;采用植物油多元醇作原料,相比于传统的石油化工类二元醇产品做原料,具有价格低廉、环保、原料可再生等优点。
Description
技术领域
本发明涉及环氧树脂领域,具体涉及一种端环氧基水性聚氨酯树脂及其制备方法。
背景技术
环氧树脂具有很好的粘结性、机械强度、电绝缘性等特性,因而广泛应用于国民经济各个工业领域。但是传统的环氧树脂含有大量的芳环结构,其玻璃化温度高,较脆,抗冲击性能较差,使其应用受到一定限制,难以满足许多工程技术日益严格的要求。例如混凝土涂料应用的环氧树脂需要具有较好的延展性,以保证其裂缝追随性,实现对混凝土的有效保护。因此如何提高环氧树脂的柔韧性,已经成为了环氧树脂技术的一个重要研究方向。
随着世界环保法规的日益完善,环保要求的日益提高,传统的溶剂型涂料因为挥发性有机物的排放受到了极大的冲击,其市场份额正迅速缩小,而具有环保特性的水性涂料、紫外光固化涂料、高固体分涂料和粉末涂料则迅速增长。其中,水性涂料因其具有环保、涂料性能接近传统涂料、对现有涂装技术改动小的特点,因而发展迅速。在过去的几年中,水性涂料在木器、皮革、汽车、工业等行业中都有着十分迅速的发展。目前市场上还没有柔韧性好的水性环氧树脂,开发一种柔韧性好的水性环氧树脂具有重要意义。
发明内容
本发明所要解决的技术问题是提供一种端环氧基水性聚氨酯树脂及其制备方法。
本发明所采取的技术方案是:
一种端环氧基水性聚氨酯树脂的制备方法,包括以下步骤:
S1:植物油多元醇、小分子多元醇、二异氰酸酯和亲水扩链剂在有机溶剂中,在催化剂作用下,发生加成反应,得到端异氰酸酯聚氨酯预聚体;
S2:取S1所得的端异氰酸酯聚氨酯预聚体与端羟基环氧化合物反应,得到端环氧基聚氨酯;
S3:向S2所得的端环氧基聚氨酯中加入胺进行中和,滴加水进行相反转,保温,减压蒸馏除去有机溶剂,得到端环氧基水性聚氨酯树脂。
优选地,所述植物油多元醇为蓖麻油多元醇、大豆油多元醇、棕榈油多元醇中的至少一种。
优选地,所述小分子多元醇为乙二醇、丙二醇、一缩二乙二醇、1,4-丁二醇、三羟甲基丙烷中的至少一种。
优选地,所述二异氰酸酯为甲苯二异氰酸酯、六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、四甲基苯二亚甲基二异氰酸酯中的至少一种。
优选地,所述催化剂为钛酸异丙酯、辛酸亚锌、二月桂酸二丁基锡中的任一种。
优选地,所述亲水扩链剂为二羟甲基丙酸。
优选地,所述端羟基环氧化合物为2,3-环氧-1-丙醇。
优选地,所述胺是三乙醇胺、N,N-二甲基乙醇胺中的至少一种。
进一步优选地,所述植物油多元醇、小分子多元醇、二异氰酸酯、亲水扩链剂、催化剂、端羟基环氧化合物和胺的质量比为(300-670):(10-45):(160-250):(20-48):(0.8-2.0):(5-14):(10-35)。
本发明还提供了一种端环氧基水性聚氨酯树脂,采用上述的制备方法制备得到。
本发明的有益效果是:本发明提供了一种端环氧基水性聚氨酯树脂及其制备方法,所述树脂通过以下步骤制得:S1:植物油多元醇、小分子多元醇、二异氰酸酯和亲水扩链剂在有机溶剂中,在催化剂作用下,发生加成反应,得到端异氰酸酯聚氨酯预聚体;S2:取S1所得的端异氰酸酯聚氨酯预聚体与端羟基环氧化合物反应,得到端环氧基聚氨酯;S3:向S2所得的端环氧基聚氨酯中加入胺进行中和,滴加水进行相反转,保温,减压蒸馏除去有机溶剂,得到端环氧基水性聚氨酯树脂。本发明所述端环氧基水性聚氨酯树脂为水性涂料,使用过程不会有挥发性有机物污染,环境友好;是由聚氨酯与环氧树脂化学方法结合,所述树脂不仅具有聚氨酯的柔韧性,还具有环氧树脂的刚性、粘结性的特点;采用植物油多元醇作原料,相比于传统的石油化工类二元醇产品做原料,具有价格低廉、环保、原料可再生等优点。
具体实施方式
实施例1:
步骤一,将100克丙酮、398克大豆油多元醇、40.5克1,4-丁二醇、37.4克二羟甲基丙酸、222克异佛尔酮二异氰酸酯投入到反应釜中,升温到60℃使物料溶解,加入1.4克的二月桂酸二丁基锡催化剂,升温到70℃反应3小时,得到端异氰酸酯的聚氨酯预聚体。
步骤二,向所得的端异氰酸酯的聚氨酯预聚体中,加入11.8克的2,3-环氧-1-丙醇进反应釜,在60℃反应4小时得到棕黄色端环氧基聚氨酯树脂;
步骤三,维持反应温度60℃,向反应釜中滴加21克N,N-二甲基乙醇胺进行中和,中和完后,分2小时向反应釜滴加990克去离子水进行相反转,保温1小时后,升温到80℃,减压蒸馏除去丙酮,即得到淡黄色带蓝光的端环氧基水性聚氨酯树脂。本实施例中所述原料均为市场上可采购原料,制备所得产物固含量为42.1%,粘度为1500mPa·S,酸值为23.8mgKOH/g。
实施例2:
步骤一,将85克丙酮、334克蓖麻油多元醇、24.1克三羟甲基丙烷、26.5克二羟甲基丙酸、174克甲苯二异氰酸酯投入到反应釜中,升温到60℃使物料溶解,加入1.1克的二月桂酸二丁基锡催化剂,升温到70℃反应3小时,得到端异氰酸酯的聚氨酯预聚体。
步骤二,向所得的端异氰酸酯的聚氨酯预聚体中,加入6.7克的2,3-环氧-1-丙醇进反应釜,在60℃反应4小时得到棕黄色端环氧基聚氨酯树脂;
步骤三,维持反应温度60℃,向反应釜中滴加15克N,N-二甲基乙醇胺进行中和,中和完后,分2小时向反应釜滴加820克去离子水进行相反转,保温1小时后,升温到80℃,减压蒸馏除去丙酮,即得到淡黄色带蓝光的端环氧基水性聚氨酯树脂。本实施例中所述原料均为市场上可采购原料,制备所得产物固含量为42.4%,粘度为5300 mPa·S,酸值为22.5mgKOH/g。
实施例3:
步骤一,将90克丙酮、353克棕榈油多元醇、13.6克乙二醇、27.9克二羟甲基丙酸、168克六亚甲基二异氰酸酯投入到反应釜中,升温到60℃使物料溶解,加入1.1克的二月桂酸二丁基锡催化剂,升温到70℃反应3小时,得到端异氰酸酯的聚氨酯预聚体。
步骤二,向所得的端异氰酸酯的聚氨酯预聚体中,加入8.7克的2,3-环氧-1-丙醇进反应釜,在60℃反应4小时得到棕黄色端环氧基聚氨酯树脂;
步骤三,维持反应温度60℃,向反应釜中滴加16克N,N-二甲基乙醇胺进行中和,中和完后,分2小时向反应釜滴加820克去离子水进行相反转,保温1小时后,升温到80℃,减压蒸馏除去丙酮,即得到淡黄色带蓝光的端环氧基水性聚氨酯树脂。本实施例中所述原料均为市场上可采购原料,制备所得产物固含量为42.7%,粘度为1100 mPa·S,酸值为23.2mgKOH/g。
实施例4:
步骤一,将110克丙酮、561克大豆油多元醇、36.0克一缩二乙二醇、42.6克二羟甲基丙酸、222克异佛尔酮二异氰酸酯投入到反应釜中,升温到60℃使物料溶解,加入1.7的钛酸异丙酯催化剂,升温到70℃反应3小时,得到端异氰酸酯的聚氨酯预聚体。
步骤二,向所得的端异氰酸酯的聚氨酯预聚体中,加入10.5克的2,3-环氧-1-丙醇进反应釜,在60℃反应4小时得到棕黄色端环氧基聚氨酯树脂;
步骤三,维持反应温度60℃,向反应釜中滴加24克N,N-二甲基乙醇胺进行中和,中和完后,分2小时向反应釜滴加1200克去离子水进行相反转,保温1小时后,升温到80℃,减压蒸馏除去丙酮,即得到淡黄色带蓝光的端环氧基水性聚氨酯树脂。本实施例中所述原料均为市场上可采购原料,制备所得产物固含量为42.8%,粘度为2200 mPa·S,酸值为21.8mgKOH/g。
实施例5:
步骤一,将110克丙酮、461克大豆油多元醇、28.8克1,4-丁二醇、42.6克二羟甲基丙酸、244克四甲基苯二亚甲基二异氰酸酯投入到反应釜中,升温到60℃使物料溶解,加入1.7克的辛酸亚锌催化剂,升温到70℃反应3小时,得到端异氰酸酯的聚氨酯预聚体。
步骤二,向所得的端异氰酸酯的聚氨酯预聚体中,加入13.7克的2,3-环氧-1-丙醇进反应釜,在60℃反应4小时得到棕黄色端环氧基聚氨酯树脂;
步骤三,维持反应温度60℃,向反应釜中滴加24克N,N-二甲基乙醇胺进行中和,中和完后,分2小时向反应釜滴加1240克去离子水进行相反转,保温1小时后,升温到80℃,减压蒸馏除去丙酮,即得到淡黄色带蓝光的端环氧基水性聚氨酯树脂。本实施例中所述原料均为市场上可采购原料,制备所得产物固含量为42.5%,粘度为3500 mPa·S,酸值为22.4mgKOH/g。
实施例6:
步骤一,将110克丙酮、461克大豆油多元醇、28.8克1,4-丁二醇、42.6克二羟甲基丙酸、244克四甲基苯二亚甲基二异氰酸酯投入到反应釜中,升温到60℃使物料溶解,加入1.7克的二月桂酸二丁基锡催化剂,升温到70℃反应3小时,得到端异氰酸酯的聚氨酯预聚体。
步骤二,向所得的端异氰酸酯的聚氨酯预聚体中,加入13.7克的2,3-环氧-1-丙醇进反应釜,在60℃反应4小时得到棕黄色端环氧基聚氨酯树脂;
步骤三,维持反应温度60℃,向反应釜中滴加24克N,N-二甲基乙醇胺进行中和,中和完后,分2小时向反应釜滴加1240克去离子水进行相反转,保温1小时后,升温到80℃,减压蒸馏除去丙酮,即得到淡黄色带蓝光的端环氧基水性聚氨酯树脂。本实施例中所述原料均为市场上可采购原料,制备所得产物固含量为42.2%,粘度为4200 mPa·S,酸值为22.3mgKOH/g。
实施例7:
步骤一,将100克丙酮、312克大豆油多元醇、93克蓖麻油多元醇、34.2克1,4-丁二醇、37.4克二羟甲基丙酸、244克四甲基苯二亚甲基二异氰酸酯投入到反应釜中,升温到60℃使物料溶解,加入1.4克的二月桂酸二丁基锡催化剂,升温到70℃反应3小时,得到端异氰酸酯的聚氨酯预聚体。
步骤二,向所得的端异氰酸酯的聚氨酯预聚体中,加入8.2克的2,3-环氧-1-丙醇进反应釜,在60℃反应4小时得到棕黄色端环氧基聚氨酯树脂;
步骤三,维持反应温度60℃,向反应釜中滴加21克N,N-二甲基乙醇胺进行中和,中和完后,分2小时向反应釜滴加1020克去离子水进行相反转,保温1小时后,升温到80℃,减压蒸馏除去丙酮,即得到淡黄色带蓝光的端环氧基水性聚氨酯树脂。本实施例中所述原料均为市场上可采购原料,制备所得产物固含量为42.4%,粘度为3200 mPa·S,酸值为23.4mgKOH/g。
实施例8:
步骤一,将90克丙酮、249克大豆油多元醇、139克蓖麻油多元醇、34.2克1,4-丁二醇、31.9克二羟甲基丙酸、222克异佛尔酮二异氰酸酯投入到反应釜中,升温到60℃使物料溶解,加入1.3克的二月桂酸二丁基锡催化剂,升温到70℃反应3小时,得到端异氰酸酯的聚氨酯预聚体。
步骤二,向所得的端异氰酸酯的聚氨酯预聚体中,加入11.8克的2,3-环氧-1-丙醇进反应釜,在60℃反应4小时得到棕黄色端环氧基聚氨酯树脂;
步骤三,维持反应温度60℃,向反应釜中滴加18克N,N-二甲基乙醇胺进行中和,中和完后,分2小时向反应釜滴加950克去离子水进行相反转,保温1小时后,升温到80℃,减压蒸馏除去丙酮,即得到淡黄色带蓝光的端环氧基水性聚氨酯树脂。本实施例中所述原料均为市场上可采购原料,制备所得产物固含量为42.8%,粘度为3600 mPa·S,酸值为22.1mgKOH/g。
实施例9:
步骤一,将90克丙酮、208克大豆油多元醇、185克棕榈油多元醇、28.8克1,4-丁二醇、31.9克二羟甲基丙酸、222克异佛尔酮二异氰酸酯投入到反应釜中,升温到60℃使物料溶解,加入1.3克的二月桂酸二丁基锡催化剂,升温到70℃反应3小时,得到端异氰酸酯的聚氨酯预聚体。
步骤二,向所得的端异氰酸酯的聚氨酯预聚体中,加入10.6克的2,3-环氧-1-丙醇进反应釜,在60℃反应4小时得到棕黄色端环氧基聚氨酯树脂;
步骤三,维持反应温度60℃,向反应釜中滴加31克三乙醇胺进行中和,中和完后,分2小时向反应釜滴加950克去离子水进行相反转,保温1小时后,升温到80℃,减压蒸馏除去丙酮,即得到淡黄色带蓝光的端环氧基水性聚氨酯树脂。本实施例中所述原料均为市场上可采购原料,制备所得产物固含量为42.6%,粘度为4200 mPa·S,酸值为22.4 mgKOH/g。
Claims (2)
1.一种端环氧基水性聚氨酯树脂的制备方法,其特征在于,包括以下步骤:
S1:植物油多元醇、小分子多元醇、二异氰酸酯和亲水扩链剂在有机溶剂中,在催化剂作用下,升温到70℃发生加成反应3小时,得到端异氰酸酯聚氨酯预聚体;
S2:取S1所得的端异氰酸酯聚氨酯预聚体与端羟基环氧化合物在60℃反应4小时,得到端环氧基聚氨酯;
S3:维持反应温度60℃,向S2所得的端环氧基聚氨酯中加入胺进行中和,中和完后,分2小时滴加水进行相反转,保温1小时,升温到80℃,减压蒸馏除去有机溶剂,得到端环氧基水性聚氨酯树脂;
所述植物油多元醇为蓖麻油多元醇、大豆油多元醇、棕榈油多元醇中的至少一种;所述小分子多元醇为乙二醇、丙二醇、一缩二乙二醇、1,4-丁二醇、三羟甲基丙烷中的至少一种;所述二异氰酸酯为甲苯二异氰酸酯、六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、四甲基苯二亚甲基二异氰酸酯的至少一种;所述催化剂为钛酸异丙酯、辛酸亚锌、二月桂酸二丁基锡中的任一种;所述亲水扩链剂为二羟甲基丙酸;所述端羟基环氧化合物为2,3-环氧-1-丙醇;所述胺是三乙醇胺、N,N-二甲基乙醇胺中的至少一种;所述有机溶剂是丙酮;所述植物油多元醇、小分子多元醇、二异氰酸酯、亲水扩链剂、催化剂、端羟基环氧化合物和胺的质量比为(300-670):(10-45):(160-250):(20-48):(0.8-2.0):(5-14):(10-35)。
2.一种端环氧基水性聚氨酯树脂,其特征在于,采用权利要求1所述的制备方法制备得到。
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