CN105693994A - 一种改性聚氨酯的制备方法 - Google Patents

一种改性聚氨酯的制备方法 Download PDF

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CN105693994A
CN105693994A CN201610243038.0A CN201610243038A CN105693994A CN 105693994 A CN105693994 A CN 105693994A CN 201610243038 A CN201610243038 A CN 201610243038A CN 105693994 A CN105693994 A CN 105693994A
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连慧琴
胡砚瓯
李月婷
常炜
崔秀国
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Beijing Institute of Petrochemical Technology
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Abstract

本发明公开了一种改性聚氨酯的制备方法，首先将石墨烯分散在熔融的多元醇中，搅拌加热并真空干燥，制得石墨烯复合多元醇；然后向所制得的石墨烯复合多元醇中加入二异氰酸酯，在惰性气体保护下充分搅拌，并加热反应，制备得到聚氨酯预聚体；再向所制得的聚氨酯预聚体中加入扩链剂，充分搅拌后浇注到模具中，反应后制备得到改性的聚氨酯。上述制备方法的工艺简单、环境友好、易于规模化生产，从而使其应用于光电器件、油料存储等多种领域。

Description

一种改性聚氨酯的制备方法
技术领域
本发明涉及材料制备技术领域，尤其涉及一种改性聚氨酯的制备方法。
背景技术
聚氨酯弹性体具有结构和性能可调性，既有橡胶的高弹性，又有塑料的高强度，其优异的耐候、耐磨、耐油等性能使其在工业、国防及高科技领域得到广泛的应用。
但现有技术中，一般的聚氨酯弹性体绝缘性高，易产生静电，严重影响了其在石油储备、光电器件等方面的应用。
发明内容
本发明的目的是提供一种改性聚氨酯的制备方法，该方法工艺简单、环境友好、易于规模化生产，从而使其应用于光电器件、油料存储等多种领域。
一种改性聚氨酯的制备方法，所述方法包括：
步骤1、将石墨烯分散在熔融的多元醇中，搅拌加热并真空干燥，制得石墨烯复合多元醇；
步骤2、向所制得的石墨烯复合多元醇中加入二异氰酸酯，在惰性气体保护下充分搅拌，并加热反应，制备得到聚氨酯预聚体；
步骤3、向所制得的聚氨酯预聚体中加入扩链剂，充分搅拌后浇注到模具中，反应后制备得到改性的聚氨酯。
在所述步骤1中：
搅拌加热的时间为2～50min，加热温度为80～110℃；
且真空干燥的时间为0.5～3h。
在所述步骤2中：
所采用的惰性气体包括氮气或氩气；
搅拌的时间为0.5～2h；
加热反应的温度为60～80℃，反应时间为2～8h。
在所述步骤3中：
反应时间为2～12h，且反应温度为30～80℃。
所述步骤1中：
所采用的石墨烯为片状结构，且所述石墨烯的边长尺寸为0.1～100mμm。
在所述步骤2中：
所采用的二异氰酸酯包括：甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、萘二异氰酸酯或异佛尔酮二异氰酸酯。
在所述步骤1中：
所采用的多元醇包括：聚醚多元醇、聚酯多元醇中的一种或几种。
在所述步骤3中：
所采用的扩链剂包括：乙二醇、丁二醇、己二醇和乙二胺中的一种或几种。
所述扩链剂中的羟基或氨基的摩尔数与所述多元醇中的羟基的摩尔数之比为：
1:0.1～1:0.9。
由上述本发明提供的技术方案可以看出，上述制备方法的工艺简单、环境友好、易于规模化生产，从而使其应用于光电器件、油料存储等多种领域。
附图说明
为了更清楚地说明本发明实施例的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域的普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他附图。
图1为本发明实施例所提供改性聚氨酯的制备方法流程示意图。
具体实施方式
下面结合本发明实施例中的附图，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，都属于本发明的保护范围。
本发明实施例所述制备方法通过石墨烯与聚氨酯弹性体的复合，制备出具有导电、阻隔性的多功能聚氨酯。下面将结合附图对本发明实施例作进一步地详细描述，如图1所示为本发明实施例所提供改性聚氨酯的制备方法流程示意图，所述方法包括：
步骤1、将石墨烯分散在熔融的多元醇中，搅拌加热并真空干燥，制得石墨烯复合多元醇；
在该步骤中，搅拌加热的时间为2～50min，加热温度为80～110℃；
且真空干燥的时间为0.5～3h。
具体实现中，所采用的石墨烯为片状结构，且所述石墨烯的边长尺寸为0.1～100mμm；这里，所用到石墨烯可以包括电化学方法、氧化还原法制备的石墨烯，长度为0.1～20μm之间。
所采用的多元醇包括：聚醚多元醇、聚酯多元醇中的一种或几种。
步骤2、向所制得的石墨烯复合多元醇中加入二异氰酸酯，在惰性气体保护下充分搅拌，并加热反应，制备得到聚氨酯预聚体；
在该步骤中，所采用的惰性气体包括氮气或氩气；搅拌的时间为0.5～2h；加热反应的温度为60～80℃，反应时间为2～8h。
所采用的二异氰酸酯包括：甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、萘二异氰酸酯或异佛尔酮二异氰酸酯。
步骤3、向所制得的聚氨酯预聚体中加入扩链剂，充分搅拌后浇注到模具中，反应后制备得到改性的聚氨酯。
在该步骤中，进行反应的时间为2～12h，且反应温度为30～80℃。
所采用的扩链剂包括：乙二醇、丁二醇、己二醇和乙二胺中的一种或几种。
上述扩链剂中的羟基或氨基的摩尔数与所述多元醇中的羟基的摩尔数之比范围为：1:0.1～1:0.9。
下面以具体的实施例对上述制备方法的过程进行详细说明：
实施例1、首先将石墨烯0.5g分散到熔融聚四氢呋喃50g中，搅拌2～50min，加热80～110℃，真空干燥0.5～2h，制得复合多元醇。
然后向复合多元醇加入二苯基甲烷二异氰酸酯9g，氮气气体保护，充分搅拌0.5～2h，加热60～80℃反应2～8h，制备聚氨酯预聚体。
再向聚氨酯预聚物中加入1,4-丁二醇2.3g，充分搅拌2～50min，浇注到模具中，于80～110℃反应2～12h，制得导电聚氨酯。
经测试，上述实施例所制得的导电聚氨酯弹性体的电导率为7.7*105Ω·cm。
实施例2、首先将石墨烯1g分散到熔融聚己二酸乙二醇二乙二醇酯50g中，搅拌2～50min，加热80～110℃，真空干燥0.5～2h，制得复合多元醇。
然后向复合多元醇加入二苯基甲烷二异氰酸酯9g，氮气气体保护，充分搅拌0.5～2h，加热60～80℃反应2～8h，制备聚氨酯预聚体。
再向聚氨酯预聚物中加入1,4-丁二醇2.3g，充分搅拌2～50min，浇注到模具中，于80～110℃反应2～12h，制得导电聚氨酯。
经测试，上述实施例2所得导电聚氨酯弹性体的电导率为8.6*104Ω·cm。
综上所述，本发明实施例所述制备方法具有如下优点和效果：
1)采用原位聚合的方法，实现了改性聚氨酯弹性体的规模化制备；
2)采用原有聚氨酯弹性体生产设备，不增加设备投资；
3)所制备的改性聚氨酯弹性体导电性可根据不同应用领域控制制备；
4)所得到的改性聚氨酯可广泛的应用于光电器件、油料储备等多种领域。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明披露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求书的保护范围为准。

Claims (9)

1.一种改性聚氨酯的制备方法，其特征在于，所述方法包括：
步骤1、将石墨烯分散在熔融的多元醇中，搅拌加热并真空干燥，制得石墨烯复合多元醇；
步骤2、向所制得的石墨烯复合多元醇中加入二异氰酸酯，在惰性气体保护下充分搅拌，并加热反应，制备得到聚氨酯预聚体；
步骤3、向所制得的聚氨酯预聚体中加入扩链剂，充分搅拌后浇注到模具中，反应后制备得到改性的聚氨酯。
2.根据权利要求1所述改性聚氨酯的制备方法，其特征在于，在所述步骤1中：
搅拌加热的时间为2～50min，加热温度为80～110℃；
且真空干燥的时间为0.5～3h。
3.根据权利要求1所述改性聚氨酯的制备方法，其特征在于，在所述步骤2中：
所采用的惰性气体包括氮气或氩气；
搅拌的时间为0.5～2h；
加热反应的温度为60～80℃，反应时间为2～8h。
4.根据权利要求1所述改性聚氨酯的制备方法，其特征在于，在所述步骤3中：
反应时间为2～12h，且反应温度为30～80℃。
5.根据权利要求1所述改性聚氨酯的制备方法，其特征在于，在所述步骤1中：
所采用的石墨烯为片状结构，且所述石墨烯的边长尺寸为0.1～100mμm。
6.根据权利要求1所述改性聚氨酯的制备方法，其特征在于，在所述步骤2中：
所采用的二异氰酸酯包括：甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、萘二异氰酸酯或异佛尔酮二异氰酸酯。
7.根据权利要求1所述改性聚氨酯的制备方法，其特征在于，在所述步骤1中：
所采用的多元醇包括：聚醚多元醇、聚酯多元醇中的一种或几种。
8.根据权利要求1所述改性聚氨酯的制备方法，其特征在于，在所述步骤3中：
所采用的扩链剂包括：乙二醇、丁二醇、己二醇和乙二胺中的一种或几种。
9.根据权利要求1所述改性聚氨酯的制备方法，其特征在于，
所述扩链剂中的羟基或氨基的摩尔数与所述多元醇中的羟基的摩尔数之比为：1:0.1～1:0.9。
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