CN113603858A - 一种水性聚合物无机复合纳米颗粒及应用 - Google Patents
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Abstract
本发明公开了一种水性聚合物无机复合纳米颗粒及应用,具体操作步骤包括:取3~5份的聚四氢呋喃醚二醇、2,2‑二羟甲基丙酸和含双聚硅氧烷支链的二醇置于三口烧瓶中搅拌后,在120℃下,减压脱水2h,冷却至室温;按顺序向步骤一中制得的混合溶液中加入1~2份的4,4‑二环己基甲烷二异氰酸酯后,再加入二月桂酸二丁基锡在85~90℃下反应,与现有技术相比,本发明的有益效果是:该水性的聚合物/无机纳米粒子复合纳米颗粒及应用,通过对纳米颗粒表面进行包覆,从而使得纳米颗粒之间建立起一道“屏障”,进而降低其化学活性的同时,提高了分散性,保证了纳米颗粒之间不会发生聚合,使得纳米颗粒可以保持稳定性进而保证其使用效果。
Description
技术领域
本发明涉及纳米颗粒技术领域,具体为一种水性聚合物无机复合纳米颗粒及应用。
背景技术
水性的聚合物/无机纳米粒子复合纳米颗粒是上个世纪80年代发展起来的新材料,它是指分散相尺寸至少有一相的一维尺寸小于10nm的复合材料,由于纳米粒子体积小,所以表面可产生一系列效应,使其具有增强和增韧的特性,因此纳米材料也被称为“21世纪最有前途的材料”。
然而现有的水性的聚合物/无机纳米粒子复合纳米颗粒因为自身的粒径极小,所以表面具有极大活性,因此会使得各个纳米粒子聚合,增大体积,失去原有的效果。针对上述问题,急需在原有水性的聚合物/无机纳米粒子复合纳米颗粒的基础上进行创新设计。
发明内容
本发明的目的在于提供一种水性聚合物无机复合纳米颗粒及应用,以解决上述背景技术提出现有的水性的聚合物/无机纳米粒子复合纳米颗粒因为自身的粒径极小,所以表面具有极大活性,因此会使得各个纳米粒子聚合,增大体积,失去原有的效果的问题。
为实现上述目的,本发明提供如下技术方案:一种水性聚合物无机复合纳米颗粒及应用,具体操作步骤包括:
1)取3~5份的聚四氢呋喃醚二醇、2,2-二羟甲基丙酸和含双聚硅氧烷支链的二醇置于三口烧瓶中搅拌后,在120℃下,减压脱水2h,冷却至室温。
2)按顺序向步骤一中制得的混合溶液中加入1~2份的4,4-二环己基甲烷二异氰酸酯后,再加入二月桂酸二丁基锡在85~90℃下反应。
3)向步骤二制得的混合溶液中加入丙酮后,再加入1~2份的三乙胺反应。
4)向步骤三中加入蒸馏水,然后高速分散后,再加入1~2份的异佛尔酮二胺反应15min。
5)在60℃下,减压除去丙酮,即可得到含聚硅氧烷侧链的聚氨酯。
6)将纳米二氧化钛粉末与蒸馏水混合后再与步骤五制得的溶液通入差速反应器中,启动反应器,在离心力的作用下,二者混合,并且成品纳米晶粒会从反应器的出口离开。
优选的,所述步骤一中聚四氢呋喃醚二醇的相对分子质量为2000,所述 2,2-二羟甲基丙酸中的—COOH的质量分数为1%且相对分子质量为396、1156、 1773和2215。
优选的,所述步骤二中反应的时间为2.5~3h,所述步骤三的反应时间为 0.5h。
优选的,所述步骤五制得的含聚硅氧烷侧链的聚氨酯反含固量为35%,所述n(—NCO):n(—OH)=1.3:1。
优选的,所述步骤六中蒸馏水:二氧化钛=4~6:1。
优选的,所述步骤六离心时间为3h,所述离心的温度为80~110℃。
与现有技术相比,本发明的有益效果是:该水性聚合物无机复合纳米颗粒及应用,通过对纳米颗粒表面进行包覆,从而使得纳米颗粒之间建立起一道“屏障”,进而降低其化学活性的同时,提高了分散性,保证了纳米颗粒之间不会发生聚合,使得纳米颗粒可以保持稳定性进而保证其使用效果。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅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。
实施一:
1)取3~5份的聚四氢呋喃醚二醇、2,2-二羟甲基丙酸和含双聚硅氧烷支链的二醇置于三口烧瓶中搅拌后,在120℃下,减压脱水2h,冷却至室温。
2)按顺序向步骤一中制得的混合溶液中加入1~2份的4,4-二环己基甲烷二异氰酸酯后,再加入二月桂酸二丁基锡在85~90℃下反应。
3)向步骤二制得的混合溶液中加入丙酮后,再加入1~2份的三乙胺反应。
4)向步骤三中加入蒸馏水,然后高速分散后,再加入1~2份的异佛尔酮二胺反应15min。
5)在60℃下,减压除去丙酮,即可得到含聚硅氧烷侧链的聚氨酯。
6)将纳米二氧化钛粉末与蒸馏水混合后再与步骤五制得的溶液通入差速反应器中,启动反应器,在离心力的作用下,二者混合,并且成品纳米晶粒会从反应器的出口离开。
实施二:
1)取3~5份的聚四氢呋喃醚二醇、2,2-二羟甲基丙酸和含双聚硅氧烷支链的二醇置于三口烧瓶中搅拌后,在120℃下,减压脱水2h,冷却至室温。
2)按顺序向步骤一中制得的混合溶液中加入6~8份的4,4-二环己基甲烷二异氰酸酯后,再加入二月桂酸二丁基锡在85~90℃下反应。
3)向步骤二制得的混合溶液中加入丙酮后,再加入1~2份的三乙胺反应。
4)向步骤三中加入蒸馏水,然后高速分散后,再加入1~2份的异佛尔酮二胺反应15min。
5)在60℃下,减压除去丙酮,即可得到含聚硅氧烷侧链的聚氨酯。
6)将纳米二氧化钛粉末与蒸馏水混合后再与步骤五制得的溶液通入差速反应器中,启动反应器,在离心力的作用下,二者混合,并且成品纳米晶粒会从反应器的出口离开。
实施三:
1)取3~5份的聚四氢呋喃醚二醇、2,2-二羟甲基丙酸和含双聚硅氧烷支链的二醇置于三口烧瓶中搅拌后,在120℃下,减压脱水2h,冷却至室温。
2)按顺序向步骤一中制得的混合溶液中加入1~2份的4,4-二环己基甲烷二异氰酸酯后,再加入二月桂酸二丁基锡在85~90℃下反应。
3)向步骤二制得的混合溶液中加入丙酮后,再加入5~7份的三乙胺反应。
4)向步骤三中加入蒸馏水,然后高速分散后,再加入1~2份的异佛尔酮二胺反应15min。
5)在60℃下,减压除去丙酮,即可得到含聚硅氧烷侧链的聚氨酯。
6)将纳米二氧化钛粉末与蒸馏水混合后再与步骤五制得的溶液通入差速反应器中,启动反应器,在离心力的作用下,二者混合,并且成品纳米晶粒会从反应器的出口离开。
尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (6)
1.一种水性聚合物无机复合纳米颗粒及应用,其特征在于,具体操作步骤包括:
1)取3~5份的聚四氢呋喃醚二醇、2,2-二羟甲基丙酸和含双聚硅氧烷支链的二醇置于三口烧瓶中搅拌后,在120℃下,减压脱水2h,冷却至室温。
2)按顺序向步骤一中制得的混合溶液中加入1~2份的4,4-二环己基甲烷二异氰酸酯后,再加入二月桂酸二丁基锡在85~90℃下反应。
3)向步骤二制得的混合溶液中加入丙酮后,再加入1~2份的三乙胺反应。
4)向步骤三中加入蒸馏水,然后高速分散后,再加入1~2份的异佛尔酮二胺反应15min。
5)在60℃下,减压除去丙酮,即可得到含聚硅氧烷侧链的聚氨酯。
6)将纳米二氧化钛粉末与蒸馏水混合后再与步骤五制得的溶液通入差速反应器中,启动反应器,在离心力的作用下,二者混合,并且成品纳米晶粒会从反应器的出口离开。
2.根据权利要求1所述的一种水性聚合物无机复合纳米颗粒及应用,其特征在于:所述步骤一中聚四氢呋喃醚二醇的相对分子质量为2000,所述2,2-二羟甲基丙酸中的—COOH的质量分数为1%且相对分子质量为396、1156、1773和2215。
3.根据权利要求1所述的一种水性聚合物无机复合纳米颗粒及应用,其特征在于:所述步骤二中反应的时间为2.5~3h,所述步骤三的反应时间为0.5h。
4.根据权利要求1所述的一种水性聚合物无机复合纳米颗粒及应用,其特征在于:所述步骤五制得的含聚硅氧烷侧链的聚氨酯反含固量为35%,所述n(—NCO):n(—OH)=1.3:1。
5.根据权利要求1所述的一种水性的聚合物/无机纳米粒子复合纳米颗粒及应用,其特征在于:所述步骤六中蒸馏水:二氧化钛=4~6:1。
6.根据权利要求1所述的一种水性的聚合物/无机纳米粒子复合纳米颗粒及应用,其特征在于:所述步骤六离心时间为3h,所述离心的温度为80~110℃。
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