CN105693985A - 一种水性荧光聚氨酯复合物的制备工艺 - Google Patents

一种水性荧光聚氨酯复合物的制备工艺 Download PDF

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CN105693985A
CN105693985A CN201610147307.3A CN201610147307A CN105693985A CN 105693985 A CN105693985 A CN 105693985A CN 201610147307 A CN201610147307 A CN 201610147307A CN 105693985 A CN105693985 A CN 105693985A
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盛建国
童何兵
徐卉
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Shandong Huamantian Cultural And Creative Industry Co ltd
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Abstract

本发明公开了一种水性荧光聚氨酯复合物的制备工艺,包括以下步骤:将各组分脱水备用;脱水后的聚丙二醇2000和二羟甲基丙酸加入三口烧瓶中,氮气保护下加热,滴入甲苯二异氰酸酯和丙酮,再加入二月桂酸二丁基锡,反应,反应过程中用二正丁胺反滴定;降温至40-50℃,加入三乙胺,反应;降至室温,加入去离子水和乙二胺,乳化,减压蒸馏,即得。本发明制得的水性荧光聚氨酯复合物固含量高,储存稳定性长,荧光量子产率高,荧光性能优越。

Description

一种水性荧光聚氨酯复合物的制备工艺
技术领域
本发明涉及高分子荧光材料,尤其是涉及一种水性荧光聚氨酯复合物的制备工艺。
背景技术
荧光材料分无机荧光材料和有机荧光材料,荧光材料具有光吸收能力强,转换效率高,发射谱带分布区域宽,荧光寿命长等特点。水性聚氨酯具有硬度高、附着力强、耐腐蚀、耐溶剂好、挥发性有机化合物(VOC)含量低等特点,而且使用方便。水性荧光聚氨酯的制备可以使水性聚氨酯中嵌入荧光材料以达到荧光效果,使得水性聚氨酯的使用更加广泛,如路面、城市街道上的井盖、灯柱等。
《水性聚氨酯荧光材料的制备及其荧光性能》(解芝茜、王继印、陶灿、杨明娣、黄毅萍、许戈文;《功能高分子学报》;2014、04期)公开了通过不同方式制备出的水性聚氨酯荧光材料来研究荧光性能的强弱,通过将4-胺基-4’-(N,N-二苯基氨基)-1,2-二苯乙烯(ADAS)溶解于N,N-二甲基甲酰胺(DMF)中后分别以混合和接枝的方式引入水性聚氨酯,制备了不同软段和扩链剂的水性聚氨酯荧光材料(FWPU);其中混合法制备的FWPU其荧光强度最大可以增加76倍,接枝法制备的FWPU最大可增加47倍。制得的水性聚氨酯荧光材料应用广泛,加上两种方法制备的水性聚氨酯荧光材料荧光强度不同,荧光量子产率分别是0.8,0.9,因此加强水性聚氨酯荧光材料的发展有着长远意义。
公开号为CN104177585A的中国专利申请,公开了一种荧光性聚氨酯乳液的制备方法,首先制备出聚氨酯的预聚体,用成盐剂反应形成聚氨酯离散体,然后进行乳化,同时加入小分子荧光材料制得荧光性聚氨酯乳液,制得的荧光性聚氨酯乳液的固含量和粘度较高,荧光量子产率是0.9,适用于印染、涂料、皮革、塑料等行业,但是荧光强度不足。
发明内容
本发明提供一种水性荧光聚氨酯复合物的制备工艺,制备的水性聚氨酯复合物具有固含量高,储存稳定性长,荧光量子产率高,荧光性能优越等特点。
一种水性荧光聚氨酯复合物的制备工艺,包括以下步骤:
(1)以重量份计,分别将30-70份聚丙二醇2000和2-7份二羟甲基丙酸加热至100-140℃,在真空度≤0.1MPa的条件下,脱水处理2-3h;丙酮、三乙胺采用4A分子筛脱水,备用;
(2)将脱水后的聚丙二醇2000和二羟甲基丙酸加入三口烧瓶中,氮气保护下加热至70-90℃,滴入10-15份甲苯二异氰酸酯和10-30份丙酮,再加入0.01-0.03份二月桂酸二丁基锡,反应2-4h,反应过程中用二正丁胺反滴定至游离的异氰酸酯量浓度为3-5%;
(3)将三口烧瓶中温度降至40-50℃,加入2-7份三乙胺中和,反应0.5-1h;
(4)将三口烧瓶中温度降至室温,在高速搅拌下加入100-400份去离子水和1-5份乙二胺,乳化,减压蒸馏,得到水性聚氨酯乳液。
优选地,上述步骤(2)中,反应2-4h后再加入10-30份1,1,2,2-四(4-羟苯基)乙烯,保持温度不变,二次反应2-4h,二正丁胺反滴定过程在二次反应中进行,使得游离的异氰酸酯浓度为1.8-2.5%。
优选地,上述1,1,2,2-四(4-羟苯基)乙烯加入之前需加热至50-70℃脱水2-3h。
优选地,上述步骤(3)中中和度为100%-120%。
优选地,上述步骤(4)中乳化时间为0.5-1h。
有益效果:本发明以甲苯二异氰酸脂和聚丙二醇2000、二羟甲基丙酸混合反应,形成长链,反应充分后,两端都是异氰酸酯根,然后再加入1.1.2.2-四(4-羟苯基)乙烯形成预聚物,再加入三乙胺形成亲水基团,最后加入去离子水和乙二胺的混合物,高速搅拌形成水性荧光聚氨酯;制得的水性荧光聚氨酯乳液能够有效的将荧光材料与水性聚氨酯复合,增强水性聚氨酯的荧光性,增大水性聚氨酯的使用范围,粒径小,固含量高,在30.6-41.3%之间,储存稳定性长,达到6个月,荧光量子产率高,在0.9-0.93之间,荧光性能优越。
具体实施方式
实施例1:
一种水性荧光聚氨酯复合物的制备工艺,包括以下步骤:
(1)以重量份计,分别将30份聚丙二醇2000和2份二羟甲基丙酸加热到100℃,真空度≤0.1MPa的条件下,脱水处理2h;丙酮、三乙胺采用4A分子筛脱水,备用;
(2)将脱水后的聚丙二醇2000和二羟甲基丙酸加入三口烧瓶中,通入氮气保护并且加热到70℃,缓慢滴入10份甲苯二异氰酸酯和10份丙酮,再加入0.01份二月桂酸二丁基锡,保持反应2h;反应过程中用二正丁胺反滴定,使得游离的异氰酸酯浓度为3-5%;
(3)将三口烧瓶中温度降至40℃,加入2份三乙胺中和,中和度为100%,反应0.5h;
(4)将三口烧瓶中温度降至室温,在高速搅拌下加入100份去离子水和1份乙二胺,乳化0.5h,减压蒸馏去除丙酮,得到水性聚氨酯乳液。
本实施例制得的水性荧光聚氨酯乳液的荧光量子产率为0.90,固含量为30.6%,呈微黄色乳液,机械离心后换算能够储存6个月。
实施例2:
一种水性荧光聚氨酯复合物的制备工艺,包括以下步骤:
(1)以重量份计,分别将40份聚丙二醇2000和4份二羟甲基丙酸加热到120℃,真空度≤0.1MPa的条件下,脱水处理2.5h;将20份1.1.2.2-四(4-羟苯基)乙烯加热到50℃,脱水处理2.5h;丙酮、三乙胺采用4A分子筛脱水,备用;
(2)将脱水后的聚丙二醇2000和二羟甲基丙酸加入三口烧瓶中,通入氮气保护并且加热到75℃,缓慢滴入15份甲苯二异氰酸酯和20份丙酮,再加入0.02份二月桂酸二丁基锡,保持反应3h;再加入20份1,1,2,2-四(4-羟苯基)乙烯,保持温度不变,二次反应2h,二次反应过程中用二正丁胺反滴定,使得游离的异氰酸酯浓度为1.8-2.5%;
(3)将三口烧瓶中温度降至45℃,加入3份三乙胺中和,中和度为110%,反应0.7h;
(4)将三口烧瓶中温度降至室温,在高速搅拌下加入150份去离子水和2份乙二胺,乳化0.7h,减压蒸馏去除丙酮,得到水性聚氨酯乳液。
本实施例制得的水性荧光聚氨酯乳液的荧光量子产率为0.92,固含量为41%,呈微黄色乳液,机械离心后换算能够储存6个月。
实施例3:
一种水性荧光聚氨酯复合物的制备工艺,包括以下步骤:
(1)以重量份计,分别将60份聚丙二醇2000和7份二羟甲基丙酸加热到140℃,真空度≤0.1MPa的条件下,脱水处理3h;将30份1.1.2.2-四(4-羟苯基)乙烯加热到70℃,脱水处理3h;丙酮、三乙胺采用4A分子筛脱水,备用;
(2)将脱水后的聚丙二醇2000和二羟甲基丙酸加入三口烧瓶中,通入氮气保护并且加热到90℃,缓慢滴入15份甲苯二异氰酸酯和20份丙酮,再加入0.03份二月桂酸二丁基锡,保持反应4h;再加入30份1,1,2,2-四(4-羟苯基)乙烯,保持温度不变,二次反应2h,二次反应过程中用二正丁胺反滴定,使得游离的异氰酸酯浓度为1.8-2.5%;
(3)将三口烧瓶中温度降至50℃,加入3份三乙胺中和,中和度为105%,反应0.5h;
(4)将三口烧瓶中温度降至室温,在高速搅拌下加入400份去离子水和5份乙二胺,乳化1h,减压蒸馏去除丙酮,得到水性聚氨酯乳液。
本实施例制得的水性荧光聚氨酯乳液的荧光量子产率为0.91,固含量为37.7%,呈微黄色乳液,机械离心后换算能够储存6个月。
实施例4:
一种水性荧光聚氨酯复合物的制备工艺,包括以下步骤:
(1)以重量份计,分别将70份聚丙二醇2000和5份二羟甲基丙酸加热到110℃,真空度≤0.1MPa的条件下,脱水处理2h;将10份1.1.2.2-四(4-羟苯基)乙烯加热到70℃,脱水处理2h;丙酮、三乙胺采用4A分子筛脱水,备用;
(2)将脱水后的聚丙二醇2000和二羟甲基丙酸加入三口烧瓶中,通入氮气保护并且加热到75℃,缓慢滴入13份甲苯二异氰酸酯和30份丙酮,再加入0.01份二月桂酸二丁基锡,保持反应3h;再加入10份1,1,2,2-四(4-羟苯基)乙烯,保持温度不变,二次反应2h,二次反应过程中用二正丁胺反滴定,使得游离的异氰酸酯浓度为1.8-2.5%;
(3)将三口烧瓶中温度降至50℃,加入7份三乙胺中和,中和度为120%,反应1h;
(4)将三口烧瓶中温度降至室温,在高速搅拌下加入300份去离子水和4份乙二胺,乳化0.5h,减压蒸馏去除丙酮,得到水性聚氨酯乳液。
本实施例制得的水性荧光聚氨酯乳液的荧光量子产率为0.93,固含量为41.3%,呈微黄色乳液,机械离心后换算能够储存6个月。

Claims (5)

1.一种水性荧光聚氨酯复合物的制备工艺,其特征在于:包括以下步骤:
(1)以重量份计,分别将30-70份聚丙二醇2000和2-7份二羟甲基丙酸加热至100-140℃,在真空度≤0.1MPa的条件下,脱水处理2-3h;丙酮、三乙胺采用4A分子筛脱水,备用;
(2)将脱水后的聚丙二醇2000和二羟甲基丙酸加入三口烧瓶中,氮气保护下加热至70-90℃,滴入10-15份甲苯二异氰酸酯和10-30份丙酮,再加入0.01-0.03份二月桂酸二丁基锡,反应2-4h,反应过程中用二正丁胺反滴定至游离的异氰酸酯浓度为3-5%;
(3)将三口烧瓶中温度降至40-50℃,加入2-7份三乙胺中和,反应0.5-1h;
(4)将三口烧瓶中温度降至室温,在高速搅拌下加入100-400份去离子水和1-5份乙二胺,乳化,减压蒸馏,得到水性聚氨酯乳液。
2.根据权利要求1所述的水性荧光聚氨酯复合物的制备工艺,其特征在于:所述步骤(2)中,反应2-4h后再加入10-30份1,1,2,2-四(4-羟苯基)乙烯,保持温度不变,二次反应2-4h,二正丁胺反滴定过程在二次反应中进行,使得游离的异氰酸酯浓度为1.8-2.5%。
3.根据权利要求2所述的水性荧光聚氨酯复合物的制备工艺,其特征在于:所述1,1,2,2-四(4-羟苯基)乙烯加入之前需加热至50-70℃脱水2-3h。
4.根据权利要求1所述的水性荧光聚氨酯复合物的制备工艺,其特征在于:所述步骤(3)中中和度为100%-120%。
5.根据权利要求1所述的水性荧光聚氨酯复合物的制备工艺,其特征在于:所述步骤(4)中乳化时间为0.5-1h。
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