CN105778121A - 一种纳米尺度磁电杂化粒子的分散方法 - Google Patents
一种纳米尺度磁电杂化粒子的分散方法 Download PDFInfo
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- CN105778121A CN105778121A CN201610211003.9A CN201610211003A CN105778121A CN 105778121 A CN105778121 A CN 105778121A CN 201610211003 A CN201610211003 A CN 201610211003A CN 105778121 A CN105778121 A CN 105778121A
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Abstract
本发明公开了一种纳米尺度磁电杂化粒子的分散方法，属于杂化粒子制备技术领域。本发明采用反相细乳液聚合的方法制备纳米尺度磁电杂化粒子分散液。采用导电聚合物溶液和单体水溶液混合，通过超声波破碎乳化，形成稳定的纳米固体颗粒，以稳定液滴和或聚合物乳胶粒子；少量固体颗粒即可形成乳胶粒子表面保护层，避免了使用常用的高分子乳化剂；采用内溶碱性物质的反相细乳液聚合物乳胶和可形成磁性物质的盐溶液分散液混合，可以得到乳胶粒子内部尺寸在50纳米以下的磁性氧化物；采用乙烯基水溶性单体聚合成为杂化粒子载体，增加了纳米尺度磁电杂化粒子分散液稳定性。
Description
技术领域：
本发明涉及的纳米尺度磁电材料的分散方法采用导电性能高分子材料和磁性氧化物前驱体分散在聚合物基体中，分散后的磁电材料至少有一维方向的尺寸在100纳米以下，属于杂化粒子制备技术领域。
背景技术：
聚合物为基体的杂化粒子通常可以使用原位法、核/壳结构法和分散共混法来制备。原位法是指把单体和纳米二氧化硅先混合均匀，在适当的条件下，引发单体自由基聚合，制备纳米复合乳液。由于单体粒子直径较小，粘度比较低，进行纳米粒子表面效改性后可以得到均匀的分散液，既保证了体系的均匀性，同时又提高了乳液的物理性能。核/壳结构法一般分为包埋法或单体聚合法，其中包埋法是指将无机纳米粒子通过一定操作分散在高分子溶液中，通过一系列操作得到聚合物无机纳米复合微球。单体聚合法是以无机纳米粒子存在为条件，引发单体聚合而形成的具有核/壳结构的聚合物无机纳米复合微球的方法。可以用单体聚合法来制备单分散性、多层结构以及带有功能基团的杂化复合材料。包埋法得到的核/壳结构微球，因为无机粒子表面的金属离子同高分子壳层功能基团之间是通过核/壳之间的范德华力来连接的，所以所得杂化复合材料的粒径不太容易控制。单体聚合法制备杂化复合微球可采用悬浮聚合、分散聚合、乳液聚合(包括无皂乳液聚合、核/壳乳液聚合)反胶束聚合等聚合体系。分散共混法分散共混法指先制备出纳米粒子，之后在用制备的纳米粒子与有机聚合物分散混合的方法，这种方法是制备聚合物/纳米粒子复合材料最直接的方法，适用于各种形态的粒子。纳米粒子与材料的合成是分开来进行的，纳米粒子的形态、尺寸容易控制。但是由于纳米粒子存在很大的界面自由能，粒子很容易发生自身团聚，利用常规的共混方法不能缩小纳米粒子与聚合物基体之间的高界面能差。
由于采用分散共混法有一定的缺陷，因此通过反相细乳液（聚合）的方法制备纳米尺度磁电杂化粒子。由于在纳米尺度，纳米结构的材料如具有比表面积大和表面能高的特点，这会使其显示出它独有的小尺寸效应，宏观量子隧道效应以及表面效应，给予了功能复合材料许多特殊性能，使其在磁电领域有特别的作用。
发明内容:
本发明的目的是利用反相细乳液（聚合）方法得到稳定的纳米尺度磁电杂化粒子分散液。
一种纳米尺度磁电杂化粒子的分散方法，按照下述步骤进行：
（1）反相细乳液稳定混合溶液的制备：
将导电聚合物溶解在A组分和B组分中；
A组分为氯仿、二甲基甲酰胺、乙腈、丙酮和二氯甲烷中的一种或几种。
B组分为环己烷、正庚烷、煤油、液体石蜡或苯基硅油中一种或几种的溶剂的混合。
步骤（1）中导电聚合物为聚噻吩、聚吡咯和聚苯胺等中的一种或几种；
步骤（1）中A组分和B组分的质量比例为20-100:100；导电聚合物在A组分中的质量比例为1-5:100。
（2）反相细乳液预乳液的制备：
将适量的水溶性单体水溶液，加入一定质量的盐溶液（反相细乳液聚合的助稳定剂）和碱性化合物后和步骤（1）溶液混合；用一定的方法将以上混合物分散，分散过程用冰水冷却，避免在分散过程发生聚合反应。
步骤（2）所述方法中的单体可以是带有乙烯基的一种或者是几种水溶性单体的混合，如采用丙烯酰胺、丙烯酸的中和物、甲基丙烯酸-2-羟乙酯、甲基丙烯酸-2-羟丙酯，N-乙烯基甲酰胺、4-乙烯基吡啶、N,N-亚甲基双丙烯酰胺或二甲基丙烯酸乙二醇酯等；单体水溶液的质量浓度为5-25%。
盐可以为氯化钠，盐加入单体水溶液后质量浓度为0.5-2.5%。
碱性化合物为氢氧化钠、氢氧化钾、氨水、氢氧化钙、乙酸钠和丙酸钠等能在水溶液中形成氢氧根离子的无机或有机化合物，用量为碱性化合物占单体水溶液质量的0.5-2.5%。
步骤（2）单体水溶液和步骤（1）得到的混合溶剂混合质量比为10-50:100；混合物分散的方法可以采用磁力预乳化和超声波破碎乳化等方式，时间可以为10-40分钟。
（3）反相细乳液的聚合：
将由步骤（2）制备的预乳液置于反应釜中，开动搅拌，搅拌速率为90r/min。采用导气管通入惰性气体将反应釜中空气置换后，反应釜加热，到达指定温度后加入引发剂。聚合反应2小时后保温1小时，得到反相细乳液聚合物乳胶。
步骤（3）所述的引发剂为水溶性过氧化物，如过硫酸钾、过硫酸铵、偶氮二异丁基脒盐酸盐、偶氮二异丁咪唑啉盐酸盐、偶氮二氰基戊酸和偶氮二异丙基咪唑啉等；或是水溶性过氧化物和还原剂组成的氧化还原引发体系，如过硫酸钾-亚铁盐、亚硫酸钠、过硫酸铵-亚铁盐、亚硫酸钠。也可以是油溶性过氧化物，如过氧化苯甲酰、过氧化月桂酰等，或是偶氮类引发剂，如偶氮二异丁腈、偶氮二异庚腈；引发剂用量为步骤（2）制备的水溶性单体质量比例的0.1-3.0%。
（4）纳米尺度磁电杂化粒子分散液的制备：
将可以形成磁性物质的水溶性盐溶液和步骤（1）的混合溶液按照预乳液和超声波破碎乳化后，得到盐溶液分散液；将此分散液迅速和步骤（3）得到的细乳液聚合物乳液在一定温度下混合，搅拌120分钟后，形成稳定的纳米尺度磁电杂化粒子分散液。
步骤（4）可以形成磁性物质的水溶性盐溶液可以为任意一种或多种铁、铬、镉、镍、钴等具有一定水溶性的金属盐；用量和步骤（2）使用的碱性化合物为等摩尔量；步骤（4）盐溶液和步骤（1）得到的混合溶剂的混合质量比为10-50:100。
本发明的优点在于本发明采用反相细乳液聚合的方法制备纳米尺度磁电杂化粒子分散液。1、采用导电聚合物溶液和单体水溶液混合，通过超声波破碎乳化，形成稳定的纳米固体颗粒，以稳定液滴和或聚合物乳胶粒子；少量固体颗粒即可形成乳胶粒子表面保护层，避免了使用常用的高分子乳化剂；2、采用内溶碱性物质的反相细乳液聚合物乳胶和可形成磁性物质的盐溶液分散液混合，可以得到乳胶粒子内部尺寸在50纳米以下的磁性氧化物；3、采用乙烯基水溶性单体聚合成为杂化粒子载体，增加了纳米尺度磁电杂化粒子分散液稳定性。
附图说明
图1为实施例1步骤（3）乳胶粒子电子透射电镜图片；
图2为实施例1步骤（4）杂化粒子电子透射电镜图片。
具体实施方式
下面结合实例，对本发明作进一步的详细说明。
实施例1
（1）反相细乳液稳定溶液的制备：
将1克聚苯胺溶解在99克二氯甲烷中，然后和100克环己烷混合。形成反相细乳液聚合稳定溶液。
（2）反相细乳液预乳液的制备：
将2.5克丙烯酰胺溶解在47.5克水中形成5%质量浓度单体溶液，加入0.25克氯化钠和0.25克氢氧化钠，然后和步骤（1）形成的溶液混合；用磁力搅拌方法预乳化20分钟，然后采用超声波破碎乳化细乳化方法将以上混合物分散，破碎时间20分钟，分散过程用冰水冷却，避免在分散过程发生聚合反应。
（3）反相细乳液的聚合：
将由步骤（2）制备的超声破碎后的预乳液置于反应釜中，开动搅拌，搅拌速率为90r/min。采用导气管通入惰性气体将反应釜中空气置换后，反应釜加热，到达80摄氏度后加入0.05克过硫酸钾引发聚合。反应2小时后保温1小时，得到反相细乳液聚合物乳胶粒子，粒径采用马尔文激光粒径分析仪得到的Z均粒径为210纳米。图1为聚合物粒子电子透射电镜观测图片，从图中可以看出粒子周围明显存在固体颗粒，起到了稳定乳胶粒子的作用。
（4）纳米尺度磁电杂化粒子分散液的制备：
将可以形成磁性物质的0.217克六水硝酸亚铁和0.631克九水硝酸铁盐溶解成10克水溶液，然后和步骤（1）100克的混合溶液按照预乳液和超声波破碎乳化后，得到盐溶液分散液，此分散液20分钟后即会发生分层现象；因此将制备好的分散液迅速和步骤（3）得到的细乳液聚合物乳液在一定温度下混合，搅拌120分钟后，形成稳定的纳米尺度磁电杂化粒子分散液。此分散体的Z均粒径为240纳米。图2为杂化粒子的电子透射电镜图片，从图中可以看到，磁性化合物呈点状（黑点）分布，尺寸在50纳米以下，聚苯胺在外层呈点状分布。分散体可以稳定时间（不发生分层和沉淀现象）为三个月以上。
实施例2
（1）反相细乳液稳定溶液的制备：
将1克聚苯胺溶解在19克二氯甲烷中，然后和100克环己烷混合。形成反相细乳液聚合稳定溶液。
（2）反相细乳液预乳液的制备：
将2.5克丙烯酸钠溶解在7.5克水中形成25%质量浓度水溶性单体溶液，加入0.25克氯化钠和0.25克氢氧化钠，然后和步骤（1）形成的100克溶液混合；用磁力搅拌方法预乳化20分钟，然后采用超声波破碎乳化细乳化方法将以上混合物分散，破碎时间20分钟，分散过程用冰水冷却，避免在分散过程发生聚合反应。
（3）反相细乳液的聚合：
将由步骤（2）制备的超声破碎后的预乳液置于反应釜中，开动搅拌，搅拌速率为90r/min。采用导气管通入惰性气体将反应釜中空气置换后，反应釜加热，到达70摄氏度后加入0.3克偶氮二异丁腈引发聚合。反应2小时后保温1小时，得到反相细乳液聚合物乳胶粒子，粒径采用马尔文激光粒径分析仪得到的Z均粒径为140纳米。
（4）纳米尺度磁电杂化粒子分散液的制备：
将可以形成磁性物质的0.217克六水硝酸亚铁和0.631克九水硝酸铁盐溶解成10克水溶液，然后和取步骤（1）20克的混合溶液按照预乳液和超声波破碎乳化后，得到盐溶液分散液；将此分散液迅速和步骤（3）得到的细乳液聚合物乳液在一定温度下混合，搅拌120分钟后，形成稳定的纳米尺度磁电杂化粒子分散液。此分散体的Z均粒径为150纳米。可以稳定时间（不发生分层和沉淀现象）为三个月以上。
实施例3
聚合步骤如下：
（1）反相细乳液稳定溶液的制备：
将2.5克聚吡咯和2.5克聚苯胺溶解在95克二氯甲烷中，然后和100克环己烷混合。形成反相细乳液聚合稳定溶液。
（2）反相细乳液预乳液的制备：
将2.5克N-乙烯基甲酰胺溶解在47.5克水中形成5%质量浓度单体溶液，加入0.15克氯化钠和0.25克氢氧化钠，然后和步骤（1）形成的溶液混合；用磁力搅拌方法预乳化20分钟，然后采用超声波破碎乳化细乳化方法将以上混合物分散，破碎时间20分钟，分散过程用冰水冷却，避免在分散过程发生聚合反应。
（3）反相细乳液的聚合：
将由步骤（2）制备的超声破碎后的预乳液置于反应釜中，开动搅拌，搅拌速率为90r/min。采用导气管通入惰性气体将反应釜中空气置换后，反应釜加热，到达80摄氏度后加入0.10克过硫酸钾引发聚合。反应2小时后保温1小时，得到反相细乳液聚合物乳胶粒子，粒径采用马尔文激光粒径分析仪得到的Z均粒径为200纳米。
（4）纳米尺度磁电杂化粒子分散液的制备：
将可以形成磁性物质的0.822克六水硫酸镍盐溶解成10克水溶液，然后和步骤（1）100克的混合溶液按照预乳液和超声波破碎乳化后，得到盐溶液分散液；将此分散液迅速和步骤（3）得到的细乳液聚合物乳液在一定温度下混合，搅拌120分钟后，形成稳定的纳米尺度磁电杂化粒子分散液。此分散体的Z均粒径为220纳米。可以稳定时间（不发生分层和沉淀现象）为三个月以上。
上述对实施例的描述是为便于该技术领域的普通技术人员能理解和应用本发明。熟悉本领域的人员显然可以容易地对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于这里的实施例，本领域技术人员根据本发明的揭示，对于本发明做出的修改都应该在本发明的保护范围之内。
Claims (5)
1.一种纳米尺度磁电杂化粒子的分散方法，其特征在于按照下述步骤进行：
（1）反相细乳液稳定混合溶液的制备：
将导电聚合物溶解在A组分和B组分中；
（2）反相细乳液预乳液的制备：
将适量的水溶性单体水溶液，加入一定质量的盐溶液（反相细乳液聚合的助稳定剂）和碱性化合物后和步骤（1）溶液混合；用一定的方法将以上混合物分散，分散过程用冰水冷却，避免在分散过程发生聚合反应；
（3）反相细乳液的聚合：
将由步骤（2）制备的预乳液置于反应釜中，开动搅拌，搅拌速率为90r/min；采用导气管通入惰性气体将反应釜中空气置换后，反应釜加热，到达指定温度后加入引发剂；聚合反应2小时后保温1小时，得到反相细乳液聚合物乳胶；
（4）纳米尺度磁电杂化粒子分散液的制备：
将可以形成磁性物质的水溶性盐溶液和步骤（1）的混合溶液按照预乳液和超声波破碎乳化后，得到盐溶液分散液；将此分散液迅速和步骤（3）得到的细乳液聚合物乳液在一定温度下混合，搅拌120分钟后，形成稳定的纳米尺度磁电杂化粒子分散液。
2.根据权利要求1所述的一种纳米尺度磁电杂化粒子的分散方法，其特征在于步骤（1）中A组分为氯仿、二甲基甲酰胺、乙腈、丙酮和二氯甲烷中的一种或几种；步骤（1）中B组分为环己烷、正庚烷、煤油、液体石蜡或苯基硅油中一种或几种的溶剂的混合；步骤（1）中导电聚合物为聚噻吩、聚吡咯和聚苯胺等中的一种或几种；步骤（1）中A组分和B组分的质量比例为20-100:100；导电聚合物在A组分中的质量比例为1-5:100。
3.根据权利要求1所述的一种纳米尺度磁电杂化粒子的分散方法，其特征在于步骤（2）所述方法中的单体可以是带有乙烯基的一种或者是几种水溶性单体的混合，如采用丙烯酰胺、丙烯酸的中和物、甲基丙烯酸-2-羟乙酯、甲基丙烯酸-2-羟丙酯，N-乙烯基甲酰胺、4-乙烯基吡啶、N,N-亚甲基双丙烯酰胺或二甲基丙烯酸乙二醇酯等；单体水溶液的质量浓度为5-25%；盐可以为氯化钠，盐加入单体水溶液后质量浓度为0.5-2.5%；碱性化合物为氢氧化钠、氢氧化钾、氨水、氢氧化钙、乙酸钠和丙酸钠等能在水溶液中形成氢氧根离子的无机或有机化合物，用量为碱性化合物占单体水溶液质量的0.5-2.5%；步骤（2）单体水溶液和步骤（1）得到的混合溶剂混合质量比为10-50:100；混合物分散的方法可以采用磁力预乳化和超声波破碎乳化等方式，时间可以为10-40分钟。
4.根据权利要求1所述的一种纳米尺度磁电杂化粒子的分散方法，其特征在于步骤（3）所述的引发剂为水溶性过氧化物，如过硫酸钾、过硫酸铵、偶氮二异丁基脒盐酸盐、偶氮二异丁咪唑啉盐酸盐、偶氮二氰基戊酸和偶氮二异丙基咪唑啉等；或是水溶性过氧化物和还原剂组成的氧化还原引发体系，如过硫酸钾-亚铁盐、亚硫酸钠、过硫酸铵-亚铁盐、亚硫酸钠；也可以是油溶性过氧化物，如过氧化苯甲酰、过氧化月桂酰等，或是偶氮类引发剂，如偶氮二异丁腈、偶氮二异庚腈；引发剂用量为步骤（2）制备的水溶性单体质量比例的0.1-3.0%。
5.根据权利要求1所述的一种纳米尺度磁电杂化粒子的分散方法，其特征在于步骤（4）可以形成磁性物质的水溶性盐溶液可以为任意一种或多种铁、铬、镉、镍、钴等具有一定水溶性的金属盐；用量和步骤（2）使用的碱性化合物为等摩尔量；步骤（4）盐溶液和步骤（1）得到的混合溶剂的混合质量比为10-50:100。
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