CN114316912A - 一种具有疏水表面的可逆温致变色相变储能微胶囊的制备方法 - Google Patents
一种具有疏水表面的可逆温致变色相变储能微胶囊的制备方法 Download PDFInfo
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Abstract
本发明提供了一种具有疏水表面的可逆温致变色相变储能微胶囊的制备方法。该方法工艺简单,产品疏水、储能调温性能稳定、成本低廉,适用范围广泛。其包括以下步骤:(1)可逆温致变色相变储能微胶囊的制备,(2)将步骤1制备的微胶囊置于无水环境,然后加入一定用量的异氰酸酯反应获得具有疏水表面的可逆温致变色相变储能微胶囊。该制备方法获得的微胶囊在保持良好的储热调温性能并伴随色彩变化监控能量储存和释放状态,同时具有疏水性能,使用安全,用途广泛。
Description
技术领域
本发明涉及一种微胶囊的制备方法,具体为一种具有疏水性能的可逆温致变色相变储能微胶囊及其制备方法。
背景技术
相变材料是一种高储热密度的材料,利用相变潜热储存能量和释放潜热,在近似恒定的温度下实现潜热储能和温度调节。有机相变材料因其优异的化学稳定性。合适的相变温度和较小的体积变化而吸引了广泛的研究兴趣并呈现出巨大的应用价值。温致变色相变材料由温致变色染料、显色剂和助溶剂组成,能够吸收和释放潜热,并在相变过程中伴随着明显的颜色变化。可逆温致变色相变材料微胶囊是将温致变色相变材料封装在微小的容器内,起到保护和支撑等作用。微胶囊化可使热致变色相变材料与外界环境相隔离,形成微室,避免储能、释放过程中的泄漏,防止外界环境腐蚀,便于使用、储存和运输,同时增加传热比表面积,明显增强传热效果。因其适用范围十分广泛,已经引起了越来越多的关注。
疏水性能在自清洁、防冰、防腐蚀、防结垢等领域具有广泛的应用价值。具有疏水性能的可逆温致变色相变储能微胶囊的发明不仅可以提高微胶囊的应用性能,还可以进一步拓宽其应用领域。
具有疏水表面的可逆温致变色相变储能微胶囊不仅可以实现储热调温性能,而且伴随颜色的外观变化来指示能量吸收和释放的状态,同时具有疏水性能。储热调温是利用相变微胶囊在相变过程中释放或吸收潜热的同时保持温度不变来应对局部环境的变化,具有双向自动调温的功能。具有疏水表面的可逆温致变色相变储能微胶囊作为一种新型材料,在智能纺织品、建筑、医学等领域具有广泛的应用前景。
目前大多数的方法仅是用于制备具有单一相变微胶囊,同时具备疏水性能以及可逆温致变色储能调温相变微胶囊及其制备方法很少被报道。
发明内容
针对现有技术的不足,本发明提供了一种具有疏水性的可逆温致变色储热调温相变微胶囊及其制备方法。该制备方法工艺简单,多种方式可实施,疏水性能以及储热调温性能稳定,成本低廉,适于工业化应用。该制备方法制备的微胶囊不仅可以保持良好的储热调温性能,而且伴随颜色外观的变化监测能量存储和释放状态,同时具有稳定的疏水性能,使用安全,用途十分广泛。
本发明制备具有疏水表面的可逆温致变色相变储能微胶囊具体步骤如下:
(1)可逆温致变色相变储能微胶囊的制备:取1~5份温致变色染料中加入1~15份显色剂,在60~300份相变材料在200摄氏度下溶解获得澄清透明的芯材;将50~100份的芯材加入到200~2000份浓度为0.1~20wt%的乳化剂水溶液,剪切乳化得到水包油型乳液;将得到的水包油乳液转移到三口烧瓶中,向三口烧瓶中加入壁材料,在持续搅拌下升温熟化最终得到微胶囊。
(2)将步骤2制备的可逆温致变色微胶囊洗涤过滤干燥后的粉末置于有机溶剂中,然后向体系中加入异氰酸酯反应30min后终止。洗涤过滤干燥后获得具有疏水表面的可逆温致变色相变储能微胶囊。
所述的异氰酸酯包括甲苯二异氰酸酯、异氟尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、二环己基甲烷二异氰酸酯、赖氨酸二异氰酸酯等中的任意一种。
所述的温致变色染料包括2-苯氨基-3-甲基-6-二丁氨基荧烷、3,3-二(2-二乙氧基-4-N,N-二乙氨基苯基)-4-氮杂苯酞、3,3’-双(1-正辛基-2-甲基吲哚-3-基)苯酞、6-二甲氨基-3,3-双(4-二甲基氨基苯基)苯酞、4,4’-[(9-丁基-9H-咔唑-3-基)亚甲基]双[N-甲基-N-苯基苯胺]、CD-1(N,N-二乙基对苯二胺盐酸盐)、FT-2、热敏红、热敏绿等中的任意一种。
所述的显色剂包括无机类和有机类。其中无机类为酸性白土、活性白土、高领土和铝镁硅酸盐类等中的任意一种。有机类显色剂为酚类、羧酸盐类、磺酸类以及酸式磷酸酯类等中任意一种。
所述的乳化剂为烷基酚聚氧乙烯醚聚氧丙烯、月桂醇聚氧乙烯醚、苯乙基酚聚氧乙烯醚聚氧丙烯醚、脂肪酰胺聚氧乙烯醚、甘油聚氧乙烯醚聚氧丙烯醚脂肪酸酯、十二烷基苯磺酸钠、单、双甲基萘磺酸钠、羟基烷基磺酸钠、烷基聚氧乙烯醚丁二酸酯磺酸盐、芳烷基酚聚氧乙烯醚硫酸盐、脂肪酸聚氧乙烯酯磷酸盐、芳烷基酚聚氧乙烯醚甲醛缩合物、聚丙烯酰胺、烷基二甲基苄基铵盐型、甜菜碱型等中任意一种。
所述的相变材料为醇类,硫酸、酮、醚、磷酸酯、碳酸酯、亚硫酸酯、羟酸酯、脂肪酸酯中的任意一种物质。其中醇类为正辛醇、正十二醇、正十四醇、正十六醇、正十八醇等中任意一种或几种任意比的混合物;所述脂肪酸酯为肉豆蔻酸甲酯、棕榈酸甲酯、硬脂酸甲酯中的任意一种或几种以任意比的混合物。
所述的壁材料为葡萄糖、淀粉、海藻酸钠、羧甲基纤维素、聚脲、聚乳酸、聚乙烯醇、聚乙二醇、聚甲基丙烯酸甲酯、聚甲基丙烯酸烯丙酯、聚乙烯吡咯烷酮、密胺树脂、酚醛树脂、聚丙烯酸酯等中任意一种。
所述的有机溶剂为环己烷、异戊烷、正戊烷、异辛烷、环戊烷、庚烷等中任意一种。
本发明将异氰酸酯与微胶囊壁材表面的羟基反应以获得疏水表面。这种制备方法工艺简单,能耗低,应用范围广泛,适于工业化生产。
附图说明
图1是实施例1所制备的具有疏水表面的可逆温致变色相变储能微胶囊的形貌图(扫描电子显微图片),图2是实施例1所制备的微胶囊的局部放大图以及水接触角(扫描电子显微图片)。
具体实施方式
以下通过具体实施例进一步说明本发明描述的方法,但是并不意味着本发明局限于这些实施例。
实施例1:
(1)可逆温致变色相变储能微胶囊的制备:取1g 6-二甲氨基-3,3-双(4-二甲基氨基苯基)苯酞中加入3g双酚A,在200摄氏度下溶解于60g正十四醇中获得澄清透明的芯材;将50g的芯材加入到210g苯乙烯马来酸酐共聚物钠盐浓度为20wt%的水溶液中,剪切乳化得到水包油型乳液;将得到的水包油乳液转移到三口烧瓶中,向三口烧瓶中加入密胺树脂,在持续搅拌下升温熟化最终得到微胶囊。
(2)将步骤2制备的可逆温致变色微胶囊洗涤过滤干燥后的粉末置于环己烷中,然后向体系中加入甲苯二异氰酸酯反应30min后终止。洗涤过滤干燥后获得具有疏水表面的可逆温致变色相变储能微胶囊。
本实施例制得的具有疏水表面的可逆温致变色相变储能微胶囊的形貌图,局部放大图以及水接触角如图1、图2所示,从图中可知,本实施例制得的微胶囊表面具有疏水性。
实施例2:
(1)可逆温致变色相变储能微胶囊的制备:取1g 3,3’-双(1-正辛基-2-甲基吲哚-3-基)苯酞中加入1g双酚S,在200摄氏度下溶解于100g正十二醇中获得澄清透明的芯材;将50g的芯材加入到200g十二烷基苯磺酸钠浓度为15wt%的水溶液中,剪切乳化得到水包油型乳液;将得到的水包油乳液转移到三口烧瓶中,向三口烧瓶中加入酚醛树脂,在持续搅拌下升温熟化最终得到微胶囊。
(2)将步骤2制备的可逆温致变色微胶囊洗涤过滤干燥后的粉末置于环戊烷中,然后向体系中加入异氟尔酮二异氰酸酯反应30min后终止。洗涤过滤干燥后获得具有疏水表面的可逆温致变色相变储能微胶囊。
实施例3:
(1)可逆温致变色相变储能微胶囊的制备:取1g 4,4’-[(9-丁基-9H-咔唑-3-基)亚甲基]双[N-甲基-N-苯基苯胺]中加入1g双酚A,在200摄氏度下溶解于100g肉豆蔻酸甲酯中获得澄清透明的芯材;将50g的芯材加入到200g聚丙烯酰胺为10wt%的水溶液中,剪切乳化得到水包油型乳液;将得到的水包油乳液转移到三口烧瓶中,向三口烧瓶中加入密胺树脂,在持续搅拌下升温熟化最终得到微胶囊。
(2)将步骤2制备的可逆温致变色微胶囊洗涤过滤干燥后的粉末置于环己烷中,然后向体系中加入二苯基甲烷二异氰酸酯反应30min后终止。洗涤过滤干燥后获得具有疏水表面的可逆温致变色相变储能微胶囊。
实施例4:
(1)可逆温致变色相变储能微胶囊的制备:取3g热敏红中加入3g双酚F,在200摄氏度下溶解于60g正十六醇中获得澄清透明的芯材;将50g的芯材加入到210g羟基烷基磺酸钠浓度为10wt%的水溶液中,剪切乳化得到水包油型乳液;将得到的水包油乳液转移到三口烧瓶中,向三口烧瓶中加入密胺树脂,在持续搅拌下升温熟化最终得到微胶囊。
(2)将步骤2制备的可逆温致变色微胶囊洗涤过滤干燥后的粉末置于庚烷中,然后向体系中加入二环己基甲烷二异氰酸酯反应30min后终止。洗涤过滤干燥后获得具有疏水表面的可逆温致变色相变储能微胶囊。
Claims (8)
1.一种具有疏水表面的可逆温致变色相变储能微胶囊的制备方法,其包括如下步骤:
(1)可逆温致变色相变储能微胶囊的制备:取1~5份温致变色染料中加入1~15份显色剂,在60~300份相变材料在200摄氏度下溶解获得澄清透明的芯材;将50~100份的芯材加入到200~2000份浓度为0.1~20wt%的乳化剂水溶液,剪切乳化得到水包油型乳液;将得到的水包油乳液转移到三口烧瓶中,向三口烧瓶中加入壁材料,在持续搅拌下升温熟化最终得到微胶囊。
(2)将步骤2制备的可逆温致变色微胶囊洗涤过滤干燥后的粉末置于有机溶剂中,然后向体系中加入异氰酸酯反应30min后终止。洗涤过滤干燥后获得具有疏水表面的可逆温致变色相变储能微胶囊。
2.如权利要求1所述的制备方法,其特征在于:所述的异氰酸酯包括甲苯二异氰酸酯、异氟尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、二环己基甲烷二异氰酸酯、赖氨酸二异氰酸酯等中的任意一种。
3.如权利要求1所述的制备方法,其特征在于:所述的温致变色染料包括2-苯氨基-3-甲基-6-二丁氨基荧烷、3,3-二(2-二乙氧基-4-N,N-二乙氨基苯基)-4-氮杂苯酞、3,3’-双(1-正辛基-2-甲基吲哚-3-基)苯酞、6-二甲氨基-3,3-双(4-二甲基氨基苯基)苯酞、4,4’-[(9-丁基-9H-咔唑-3-基)亚甲基]双[N-甲基-N-苯基苯胺]、CD-1(N,N-二乙基对苯二胺盐酸盐)、FT-2、热敏红、热敏绿等中的任意一种。
4.如权利要求1所述的制备方法,其特征在于:所述的显色剂包括无机类和有机类。其中无机类为酸性白土、活性白土、高领土和铝镁硅酸盐类等中的任意一种。有机类显色剂为酚类、羧酸盐类、磺酸类以及酸式磷酸酯类等中任意一种。
5.如权利要求1所述的制备方法,其特征在于:所述的乳化剂为烷基酚聚氧乙烯醚聚氧丙烯、月桂醇聚氧乙烯醚、苯乙基酚聚氧乙烯醚聚氧丙烯醚、脂肪酰胺聚氧乙烯醚、甘油聚氧乙烯醚聚氧丙烯醚脂肪酸酯、十二烷基苯磺酸钠、单、双甲基萘磺酸钠、羟基烷基磺酸钠、烷基聚氧乙烯醚丁二酸酯磺酸盐、芳烷基酚聚氧乙烯醚硫酸盐、脂肪酸聚氧乙烯酯磷酸盐、芳烷基酚聚氧乙烯醚甲醛缩合物、聚丙烯酰胺、烷基二甲基苄基铵盐型、甜菜碱型等中任意一种。
6.如权利要求1所述的制备方法,其特征在于:所述的相变材料为醇类,硫酸、酮、醚、磷酸酯、碳酸酯、亚硫酸酯、羟酸酯、脂肪酸酯中的任意一种物质。其中醇类为正辛醇、正十二醇、正十四醇、正十六醇、正十八醇等中任意一种或几种任意比的混合物;所述脂肪酸酯为肉豆蔻酸甲酯、棕榈酸甲酯、硬脂酸甲酯中的任意一种或几种任意比的混合物。
7.如权利要求1所述的制备方法,其特征在于:所述的壁材材料为葡萄糖、淀粉、海藻酸钠、羧甲基纤维素、聚脲、聚乳酸、聚乙烯醇、聚乙二醇、聚甲基丙烯酸甲酯、聚甲基丙烯酸烯丙酯、聚乙烯吡咯烷酮、密胺树脂、酚醛树脂、聚丙烯酸酯等中任意一种。
8.如权利要求1所述的制备方法,其特征在于:所述的有机溶剂为环己烷、异戊烷、正戊烷、异辛烷、环戊烷、庚烷等中任意一种。
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CN116377720A (zh) * | 2023-04-06 | 2023-07-04 | 江苏瑞洋安泰新材料科技有限公司 | 一种温致变色防水面料及其制备方法 |
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CN115785599B (zh) * | 2023-01-09 | 2023-11-17 | 中国科学技术大学 | 一种用于高光谱伪装的仿生热致变色材料的制备方法 |
CN116377720A (zh) * | 2023-04-06 | 2023-07-04 | 江苏瑞洋安泰新材料科技有限公司 | 一种温致变色防水面料及其制备方法 |
CN116377720B (zh) * | 2023-04-06 | 2023-10-17 | 江苏瑞洋安泰新材料科技有限公司 | 一种温致变色防水面料及其制备方法 |
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