CN104311774A - 一种空心微珠填充环氧自交联改性聚氨酯的制备方法 - Google Patents

一种空心微珠填充环氧自交联改性聚氨酯的制备方法 Download PDF

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CN104311774A
CN104311774A CN201410488840.7A CN201410488840A CN104311774A CN 104311774 A CN104311774 A CN 104311774A CN 201410488840 A CN201410488840 A CN 201410488840A CN 104311774 A CN104311774 A CN 104311774A
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Abstract

一种空心陶瓷微珠填充环氧自交联改性聚氨酯的制备方法，包括空心陶瓷微珠的预处理，环氧自交联改性聚氨酯乳液的制备，空心陶瓷微珠填充环氧自交联改性聚氨酯复合材料的制备三个过程。本发明得到的空心陶瓷微珠填充环氧自交联改性聚氨酯成膜后具有低密度、强耐水性及耐溶剂性。

Description

一种空心微珠填充环氧自交联改性聚氨酯的制备方法
技术领域
本发明涉及一种空心微珠填充环氧自交联改性聚氨酯的制备方法，属化工领域。
技术背景        
空心陶瓷微珠填充环氧树脂复合材料具有较低的密度，广泛应用于航空隔热材料和深海浮力材料中，，另外由于环氧树脂具有高模量、高强度和耐化学性好、热稳定性好等优点，而且可直接参与水性聚氨酯的合成反应，从而提高聚氨酯的耐水、耐溶剂、耐热蠕变性能及拉伸强度等。本发明利用了环氧树脂的环氧基和羟基参与反应，形成多重交联，制得环氧树脂改性的水性聚氨酯，具有良好的稳定性、耐水性及耐溶剂性。
发明内容
本发明的目的是提供一种空心微珠填充环氧自交联改性聚氨酯的制备方法，具有低密度、强耐水性及耐溶剂性。
为实现以上目的，本发明的一种空心微珠填充环氧自交联改性聚氨酯的制备方法为： 
(1) 空心陶瓷微珠的预处理：取干燥后的空心陶瓷微珠加入到硅烷偶联剂KH-550与无水乙醇的混合溶液中，于70℃水浴中充分搅拌1h，进行减压抽滤去除溶剂，烘干备用；
(2) 环氧自交联改性聚氨酯乳液的制备：以2,6-甲苯二异氰酸酯(TDI)、聚四氢呋喃二醇(PTMG)、1,4-丁二醇(BDO)、聚醚二元醇磺酸盐(SPPG)，环氧树脂(E-128)为原料制备预聚体，加入3-[二-(2-羟乙基)]胺基-N(1,1-二甲基-3丁酮)丙酰胺(DHPA)对预聚体交联扩链，DHPA的用量为预聚体质量的3%，加入三羟甲基丙烷(TMP)进行交联扩链，反应1h，降温至40℃，加入三乙胺进行中和反应生成盐，反应3-4min，加入水进行乳化60min，得到环氧自交联改性聚氨酯乳液；
(3) 空心陶瓷微珠填充环氧自交联改性聚氨酯复合材料的制备：在上述环氧自交联改性聚氨酯乳液中加入固化剂，于70℃下充分搅拌混合后，进行真空脱泡，加入经硅烷偶联剂处理的空心陶瓷微珠，加入量为聚氨酯乳液质量的20%，充分搅拌混合后，进行模压成型，得到空心陶瓷微珠填充的环氧自交联改性聚氨酯复合材料。
所述的步骤(1)中硅烷偶联剂KH-550与无水乙醇的质量比为1:6-1:8。
所述的步骤(2)中预聚体原料的配比为：TDI与PTMG、SPPG、BDO、E-128的摩尔比为1.2:1-1.3:1，BDO占预聚体质量的2%-3%，SPPG占预聚体质量的4%-5%，E-128占预聚体质量的5%-6%；TMP占预聚体质量的0.2%；三乙胺的物质的量与SPPG的物质的量相同；水的用量为预聚体总质量的2倍。
本发明产生的有益效果为，本专利采用环氧树脂改性水性聚氨酯，充分利用环氧树脂的环氧基和羟基参与反应，形成多重交联，提高水性聚氨酯的耐化学性和力学性能，在其中加入空心陶瓷微珠可降低复合材料的密度，增强压缩强度及弯曲强度。
实施例
实施例1：
一种空心微珠填充环氧自交联改性聚氨酯的制备方法为： 
(1) 空心陶瓷微珠的预处理：取干燥后的空心陶瓷微珠加入到质量比为1:6的硅烷偶联剂KH-550与无水乙醇的混合溶液中，于70℃水浴中充分搅拌1h，进行减压抽滤去除溶剂，烘干备用；
(2) 环氧自交联改性聚氨酯乳液的制备：以TDI、PTMG、BDO、SPPG、E-128为原料制备预聚体，加入TMP进行交联扩链，反应1h；加入3-[二-(2-羟乙基)]胺基-N(1,1-二甲基-3丁酮)丙酰胺(DHPA)对预聚体交联扩链，DHPA的用量为预聚体质量的3%，降温至40℃，加入三乙胺进行中和反应生成盐，反应3-4min，加入水进行乳化60min，得到环氧自交联改性聚氨酯乳液；其中预聚体原料的配比为：TDI与PTMG、SPPG、BDO、E-128的摩尔比为1.2:1，BDO占预聚体质量的2%，SPPG占预聚体质量的4%，E-128占预聚体质量的5%；TMP占预聚体质量的0.2%；三乙胺的物质的量与SPPG的物质的量相同；水的用量为预聚体总质量的2倍；
(3) 空心陶瓷微珠填充环氧自交联改性聚氨酯复合材料的制备：在上述环氧自交联改性聚氨酯乳液中加入固化剂，于70℃下充分搅拌混合后，进行真空脱泡，加入经硅烷偶联剂处理的空心陶瓷微珠，加入量为乳液质量的20%，充分搅拌混合后，进行模压成型，得到空心陶瓷微珠填充的环氧自交联改性聚氨酯复合材料。
实施例2：
一种空心微珠填充环氧自交联改性聚氨酯的制备方法为： 
(1) 空心陶瓷微珠的预处理：取干燥后的空心陶瓷微珠加入到质量比为1:7的硅烷偶联剂KH-550与无水乙醇的混合溶液中，于70℃水浴中充分搅拌1h，进行减压抽滤去除溶剂，烘干备用；
(2) 环氧自交联改性聚氨酯乳液的制备：以TDI、PTMG、BDO、SPPG、E-128为原料制备预聚体，加入TMP进行交联扩链，反应1h；加入3-[二-(2-羟乙基)]胺基-N(1,1-二甲基-3丁酮)丙酰胺(DHPA)对预聚体交联扩链，DHPA的用量为预聚体质量的3%，降温至40℃，加入三乙胺进行中和反应生成盐，反应3-4min，加入水进行乳化60min，得到环氧自交联改性聚氨酯乳液；其中预聚体原料的配比为：TDI与PTMG、SPPG、BDO、E-128的摩尔比为1.2:1，BDO占预聚体质量的2%，SPPG占预聚体质量的4%，E-128占预聚体质量的5%；TMP占预聚体质量的0.2%；三乙胺的物质的量与SPPG的物质的量相同；水的用量为预聚体总质量的2倍；
(3) 空心陶瓷微珠填充环氧自交联改性聚氨酯复合材料的制备：在上述环氧自交联改性聚氨酯乳液中加入固化剂，于70℃下充分搅拌混合后，进行真空脱泡，加入经硅烷偶联剂处理的空心陶瓷微珠，加入量为乳液质量的20%，充分搅拌混合后，进行模压成型，得到空心陶瓷微珠填充的环氧自交联改性聚氨酯复合材料。
实施例3：
一种空心微珠填充环氧自交联改性聚氨酯的制备方法为： 
(1) 空心陶瓷微珠的预处理：取干燥后的空心陶瓷微珠加入到质量比为1:8的硅烷偶联剂KH-550与无水乙醇的混合溶液中，于70℃水浴中充分搅拌1h，进行减压抽滤去除溶剂，烘干备用；
(2) 环氧自交联改性聚氨酯乳液的制备：以TDI、PTMG、BDO、SPPG、E-128为原料制备预聚体，加入TMP进行交联扩链，反应1h；加入3-[二-(2-羟乙基)]胺基-N(1,1-二甲基-3丁酮)丙酰胺(DHPA)对预聚体交联扩链，DHPA的用量为预聚体质量的3%，降温至40℃，加入三乙胺进行中和反应生成盐，反应3-4min，加入水进行乳化60min，得到环氧自交联改性聚氨酯乳液；其中预聚体原料的配比为：TDI与PTMG、SPPG、BDO、E-128的摩尔比为1.3:1，BDO占预聚体质量的3%，SPPG占预聚体质量的5%，E-128占预聚体质量的6%；TMP占预聚体质量的0.2%；三乙胺的物质的量与SPPG的物质的量相同；水的用量为预聚体总质量的2倍；
(3) 空心陶瓷微珠填充环氧自交联改性聚氨酯复合材料的制备：在上述环氧自交联改性聚氨酯乳液中加入固化剂，于70℃下充分搅拌混合后，进行真空脱泡，加入经硅烷偶联剂处理的空心陶瓷微珠，加入量为乳液质量的20%，充分搅拌混合后，进行模压成型，得到空心陶瓷微珠填充的环氧自交联改性聚氨酯复合材料。

Claims (6)

1.一种空心微珠填充环氧自交联改性聚氨酯的制备方法，其特征在于：制备方法为：
(1) 空心陶瓷微珠的预处理：取干燥后的空心陶瓷微珠加入到硅烷偶联剂KH-550与无水乙醇的混合溶液中，于70℃水浴中充分搅拌1h，进行减压抽滤去除溶剂，烘干备用；
(2) 环氧自交联改性聚氨酯乳液的制备：以TDI、PTMG、BDO、SPPG、E-128为原料制备预聚体，加入TMP进行交联扩链，反应1h，加入3-[二-(2-羟乙基)]胺基-N(1,1-二甲基-3丁酮)丙酰胺(DHPA)对预聚体交联扩链，DHPA的用量为预聚体质量的3%，降温至40℃，加入三乙胺进行中和反应生成盐，反应3-4min，加入水进行乳化60min，得到环氧自交联改性聚氨酯乳液；
(3) 空心陶瓷微珠填充环氧自交联改性聚氨酯复合材料的制备：在上述环氧自交联改性聚氨酯乳液中加入固化剂，于70℃下充分搅拌混合后，进行真空脱泡，加入经硅烷偶联剂处理的空心陶瓷微珠，加入量为聚氨酯乳液质量的20%，充分搅拌混合后，进行模压成型，得到空心陶瓷微珠填充的环氧自交联改性聚氨酯复合材料。
2.如权利要求1所述的一种空心微珠填充环氧自交联改性聚氨酯的制备方法，其特征在于：所述的步骤(1)中硅烷偶联剂KH-550与无水乙醇的质量比为1:6-8。
3.如权利要求1所述的一种空心微珠填充环氧自交联改性聚氨酯的制备方法，其特征在于：所述的步骤(2)中预聚体原料的配比为：TDI与PTMG、SPPG、BDO、E-128的摩尔比为1.2-1.3:1，BDO占预聚体质量的2%-3%，SPPG占预聚体质量的4%-5%，E-128占预聚体质量的5%-6%。
4.如权利要求1所述的一种空心微珠填充环氧自交联改性聚氨酯的制备方法，其特征在于：所述的步骤(2)中TMP占预聚体质量的0.2%。
5.如权利要求1所述的一种空心微珠填充环氧自交联改性聚氨酯的制备方法，其特征在于：所述的步骤(2)中三乙胺的物质的量与SPPG的物质的量相同。
6.如权利要求1所述的一种空心微珠填充环氧自交联改性聚氨酯的制备方法，其特征在于：所述的步骤(2)中水的用量为预聚体总质量的2倍。
CN201410488840.7A 2014-09-23 2014-09-23 一种空心微珠填充环氧自交联改性聚氨酯的制备方法 Pending CN104311774A (zh)

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CN108314808A (zh) * 2017-01-16 2018-07-24 中国海洋大学 一种深海柔性浮力材料及其制备方法
CN109401280A (zh) * 2018-10-10 2019-03-01 苏州市雄林新材料科技有限公司 一种tpu幻彩膜及其制备方法

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Application publication date: 20150128