CN101684403B - 一种天然微管包封的相变微胶囊及其制备方法 - Google Patents
一种天然微管包封的相变微胶囊及其制备方法 Download PDFInfo
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
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Abstract
本发明公开了一种微管包封的相变材料的微胶囊及其制备方法。该相变材料的微胶囊由相变材料、切短的微管和聚合物组成;所述切短的微管是将中空管状天然纤维切成长度为0.1mm-5cm得到的纤维段;所述中空管状天然纤维直径为0.1-1000μm;所述相变材料封装在所述切短的微管中,所述切短的微管包覆于所述聚合物中。本发明采用的包封管是廉价易得的天然微管,由于微管的大中空度使其储能密度大,封闭结构使能量输出稳定,极细的微米级管状结构使传热迅速,热及化学稳定性有利于长期使用。
Description
技术领域
本发明涉及一种天然微管包封的相变微胶囊及其制备方法。
背景技术
相变材料(Phase change materials,PCM),又称为潜热储能材料(Latent thermalenergy storage,LTES)是指物质发生相变时能够吸收或放出热量而该物质本身温度不变或变化不大的一类材料。相变材料作为储能载体,由于其具有贮热密度高、设备体积小、热效率高以及吸放热为恒温过程等优点,可以有效提高能源的利用率、缓解能源紧张的难题。目前,已被广泛运用于冰箱和空调的制冷和蓄冷、智能建筑物的自动恒温、太阳能应用中的能量储存和交换技术、电力的“移峰填谷”、废热和余热的回收利用以及日用品中。由于它使用简便、不耗能,具有很大的应用前景和广阔市场。
从材料的相态变化过程,相变材料主要分为固-液相变、固-固相变、固-气相变及液-气相变,后两者在相变过程中伴随有大量的气体存在,使材料体积变化较大,在实际应用中很少被选用。固-液相变由于体积变化小,潜热较大,储能好,相变温度范围广,在实际中得到了广泛的应用。但由于该材料在相变过程中有液相产生,因此必须用容器密封盛装,以防止泄漏污染环境,并且容器对相变材料而言必须是惰性的。这一缺点极大地束缚了固-液相变储能材料在实际中的应用。近年来,随着技术的发展和应用场合的要求,人们试图对其进行形状稳定处理使其转变成形式上的“固-固”相变,但实际上仍发生固-液相变,解决了相变材料的熔融问题,大大方便了实际应用。目前对相变材料进行形状稳定的方法主要有定型化和微胶囊化两种方法。
定型化相变材料实质上是一类复合相变储能材料,是指将相变材料与载体物质相结合,形成一种外形上可保持固体形状、具有不流动性的相变材料,其可代替固-固相变材料。这类相变材料的主要组成有两种:其一是工作物质成分,即相变材料,利用其相变来进行储能、放能,工作物质包括各种相变材料,但用的较多的主要是固-液相变材料。其二是载体物质,其作用是保持相变材料的不流动性和可加工性,载体物质的熔化温度要求高于相变材料的相变温度,使工作物质的相变范围内保持其固体的形状和材料性能。从近年定型复合相变材料的合成发展状况看,主要制备方法可大致归为:共混法,接枝法,烧结法,原位插层法和溶胶-凝胶法。但由于定型化相变材料的物理作用相对较小,材料经多次使用时易发生固-液相变材料在载体上的脱附,泄漏渗出以及宏观的两相分离等现象。
微胶囊化相变材料是利用微胶囊技术将固液相变材料微粒表面包覆一层性能稳定的高分子膜或无机材料而构成的具有核壳结构的复合相变材料。微胶囊化相变材料在相变过程中,内核发生固-液相变,而其外层的高分子膜保持为固态,因此该类相变材料在宏观上表现为固态颗粒。相变微胶囊的化学制备方法主要有原位聚合法、界面聚合法、反应相分离法以及复凝聚法等类,不同的制备方法所得到的外壳性能有所差别。随着聚合物科学的发展,微胶囊化技术逐渐成熟,因此,相变储能微胶囊材料由于其特殊的性能和用途受到了广泛的关注和研究。相变微胶囊的吸热、放热的储热原理相当于一种“热电池”,微容器的封装使用相变材料转变成无数微小的工作单元,因此,大大扩展了相变材料的使用领域和场合。掺混了相变微胶囊的制品会在所改性的物品周围建立起围绕所采用相变物质熔点范围的微气候环境,从而满足对舒适度的要求。微胶囊化相变材料可以很好地解决固-液相变过程中极易熔融流动、渗透迁移、相分离、腐蚀等严重问题,经壳层材料包封保护后,相变材料与外界环境相分离而得以稳定,同时,聚合物壳层材料或经改性的壳层材料大大增加了相变材料与基体材料的相容性,从而大大增加了相变材料的实用性。然而,对于微胶囊的囊壁的强度、渗透性以及耐热性还有待于提高,而且主要是成本较高。
发明内容
本发明的目的是提供一种利用切短的天然微管包封相变材料的相变微胶囊及其制备方法。
本发明所提供的相变微胶囊,由相变材料、切短的微管和聚合物组成;
所述切短的微管是将中空管状天然纤维切成长度为0.1mm-5cm得到的纤维段;所述中空管状天然纤维直径为0.1-1000μm,相变材料封装在所述切短的微管中,切短的微管包覆于所述聚合物中。
所述天然纤维来源于木棉纤维、乳草纤维、丝瓜纤维、竹纤维、天竹纤维、亚麻纤维、羊毛或羽绒。
所述相变材料可为下述1)和2)中的至少一种:1)为固-液相变材料,2)为固-固相变材料;
所述固液相变材料可为下述a)和b)中的至少一种:a)为无机相变材料,b)为有机相变材料;
其中,所述无机相变材料为结晶水合盐和/或熔融盐。所述结晶水合盐可为碱金属或碱土金属的卤化物、硫酸盐、磷酸盐、硝酸盐、醋酸盐或碳酸盐中的一种或其任意组合,如Na2SO4·10H2O、Na2HPO4·12H2O、CaCl2·6H2O、SnCl·6H2O等;所述熔融盐具体可为K2WO4或K2MoO4等。
所述有机相变材料可为下述物质中的任意一种:高级脂肪烃、高级脂肪酸、高级脂肪酸酯、高级脂肪酸或酯的盐、高级脂肪醇、芳香烃、芳香酮、芳香酰胺、氟氯烷、多羰基碳酸和结晶高分子。
高级脂肪烃通常是含6~8个以上碳原子的脂肪烃的统称。高级脂肪酸通常指含C6~C26的一元羧酸。
所述高级脂肪烃为下述十六种物质中的一种或其任意组合:正二十八烷、正二十七烷、正二十六烷、正二十五烷、正二十四烷、正二十三烷、正二十二烷、正二十一烷、正二十烷、正十九烷、正十八烷、正十七烷、正十六烷、正十五烷、正十四烷和正十三烷;所述结晶高分子为密度高于0.94g/cm3的高密度聚乙烯、聚乙二烯或结晶聚氯乙烯。
所述固-固相变材料为无机盐、多元醇或高分子交联树脂。
其中,所述无机盐为Li2SO4和/或KHF2;所述多元醇可为下述六种物质中的一种或其任意组合:季戊四醇(PE)、2,2-二羟甲基丙醇(PG)、新戊二醇(NPG)、2-氨基-2-甲基-1,3-丙二醇、三羟甲基乙烷和三羟甲基氨基甲烷;所述高分子交联树脂为交联聚烯烃、交联聚缩醛、交联聚烯烃和交联聚缩醛的共聚物或交联聚烯烃和交联聚缩醛的共混物。
所述聚合物层中的聚合物为下述十种聚合物中的任意一种或其任意共聚物或其任意共混物:脲醛树脂、三聚氰胺-甲醛树脂、三聚氰胺脲醛树脂、聚氨酯、聚甲基丙烯酸甲酯、聚甲基丙烯酸乙酯、酚醛树脂、环氧树脂、聚丙烯腈或醋酸纤维素。
本发明所提供的制备切短微管包封的相变材料的微胶囊的方法,包括以下步骤:
1)芯材相变材料的液化
将相变材料加热到熔点以上或用溶剂溶解得到液态的相变材料;
2)液态相变材料填充切短的天然微管
将切短的天然微管分散于步骤1)的液态相变材料中,浸泡,通过毛细吸收使所述天然微管内充满液态的相变材料;
3)微胶囊化相变材料的包封
用聚合物包覆步骤2)中填充了相变材料的微管,得到了所述的相变材料的微胶囊。
所述方法还包括洗去得到的相变材料的微胶囊表面吸附的相变材料的步骤。
所述溶剂可为下述十种溶剂中的任意一种:去离子水、N,N’-二甲基甲酰胺、N,N’-二甲基乙酰胺、四氢呋喃、二氯甲烷、三氯甲烷、环己烷、甲醇、乙醇和丙酮。
本发明与现有的微胶囊化相变材料包封技术相比有如下有益效果:
1、本发明采用的包封管是廉价易得的天然微管。如其中的木棉纤维是一种具有大比表面积、大中空度结构的天然纤维素纤维,中空度高达80~90%,是现有的人工制备方法难以达到的,用于制造相变储能材料比现有的任何纤维都更有优势;且木棉纤维热稳定性好,在250℃下基本不发生热降解。同时,木棉纤维的化学稳定性较好,只在高浓度的强酸中才可溶解。
2、利用切短的具有大比表面积微孔结构的天然微管作为支撑材料,通过微孔的毛细作用力,将液态的有机物或无机物相变储热材料(高于相变温度条件下)吸入到微孔内,形成有机和无机、有机或无机复合相变储热材料。这种复合相变储热材料,当有机或无机相变储热材料在微孔内发生固-液相变时,由于毛细管力的作用,液态的相变储热材料很难从微孔中溢出。
3、虽然毛细力作用在一定程度上解决了固-液相变材料的流动性问题,但其仍为一个“开放”的包裹体系,所以可进一步用聚合物对微胶囊化的已吸附了相变材料的微管封壁、封端。
4、由于微管的大中空度使其储能密度大,封闭结构使能量输出稳定,极细的微米级管状结构使传热迅速,热及化学稳定性有利于长期使用,特殊的亲油疏水的浸润性能在加工过程中可被利用。
5、微胶囊化的相变材料形态在实际工艺过程中能更好地分散在基体材料中。与基体材料混合后,微米级的胶囊化相变材料尺寸可以保持制品的外观不受影响。
附图说明
图1为实施例1制备的相变微胶囊在循环升降温下的DSC曲线图。
图2为实施例1制备的相变微胶囊扫描电镜照片,其中a)切短的天然木棉纤维管;b)和c)装填了石蜡的胶囊化木棉纤维微管;d)脲醛树脂进一步包封后的胶囊化石蜡填充木棉纤维管。
具体实施方式
实施例1、制备天然木棉纤维管封装石蜡并用脲醛树脂包封的相变微胶囊
(1)芯材相变材料的液化
将有机相变材料石蜡加热到熔点60℃以上获得液态的石蜡相变材料;
(2)液态相变材料填充切短的天然微管
将1g长度为10-50μm的天然木棉纤维(切短的微管)分散于10mL步骤(1)的液态相变材料中,浸泡使毛细吸收达到平衡,使木棉纤维管内充满液态的相变材料;
(3)微胶囊化相变材料的包封
直接在步骤(2)填充了相变材料的天然木棉纤维的熔体中滴加2g尿素甲醛预聚物(将2ml体积分数为36%的甲醛水溶液加1g尿素搅拌到全溶解,升温到60℃,保温15min得到的),提高熔体温度到97~98℃,反应1小时。生成的脲醛树脂聚合物在木棉纤维周围界面相分离沉积,使微胶囊化的相变材料包封脲醛树脂层;
(4)微胶囊化相变材料的提纯
将步骤(3)中包封脲醛树脂层的吸满了相变材料的微管捞出,再放入热水中洗去管间吸附的相变材料后晾干,即形成微胶囊化相变材料。
相变材料在循环升降温下的DSC曲线如图1所示,扫描电镜照片如图2所示。
由图1可知相变微胶囊在循环升降温下具有很好的可循环相变储能效果。
由图2可知装填了石蜡的胶囊化木棉纤维微管经过脲醛树脂包封后形成了胶囊化相变材料。
实施例2、制备天然乳草纤维封装季戊四醇并用醋酸纤维素包封的相变微胶囊
(1)芯材相变材料的液化
将有机相变材料季戊四醇(PE)溶解到少量乙醇中获得液态的季戊四醇(PE)溶液相变材料;
(2)液态相变材料填充切短的天然微管
将1g长度为0.5-10μm的天然乳草纤维分散于10mL步骤(1)得到的液态相变材料中,浸泡使毛细吸收达到平衡,使乳草纤维管内充满液态的相变材料;
(3)微胶囊化相变材料的包封
将步骤(2)得到的含有乙醇溶剂的相变材料微胶囊中的乙醇挥发掉,使相变材料季戊四醇(PE)溶液浓缩固化后浸渍于5mL浓度为5%(质量百分含量)的醋酸纤维素的二氯甲烷溶液中,利用界面沉积反应使微胶囊化的相变材料包封醋酸纤维素层;
(4)微胶囊化相变材料的提纯
将步骤(3)中包封了醋酸纤维素层的填充了相变材料的乳草纤维,捞起后晾干,即形成微胶囊化相变材料。
此方法制备的相变微胶囊在循环升降温下具有很好的可循环相变储能效果,并且装填了季戊四醇(PE)的胶囊化乳草纤维微管经过醋酸纤维素包封后形成分散性较好的胶囊化相变材料。
实施例3、制备天然竹纤维封装CaCl2·6H2O并用醋酸纤维素包封的相变微胶囊
(1)芯材相变材料的液化
将1g无机相变材料CaCl2·6H2O溶解到10mL去离子水中获得液态的CaCl2·6H2O溶液相变材料;
(2)液态相变材料填充切短的天然微管
将1g长度为500-1000μm的天然竹纤维分散于10mL(1)得到的液态相变材料中,浸泡使毛细吸收达到平衡,使竹纤维管内充满液态的相变材料;
(3)微胶囊化相变材料的包封
将步骤(2)得到的含有去离子水的相变材料微胶囊中的去离子水挥发掉,使相变材料CaCl2·6H2O溶液浓缩固化后浸渍于10mL浓度为5%(质量百分含量)的醋酸纤维素的二氯甲烷溶液中,利用界面沉积反应使微胶囊化的相变材料包封醋酸纤维素层;
(4)微胶囊化相变材料的提纯
将步骤(3)中包封了醋酸纤维素层的填充了相变材料的竹纤维,捞起后晾干,即形成微胶囊化相变材料。
此方法制备的相变微胶囊在循环升降温下具有很好的可循环相变储能效果,并且装填了无机相变材料CaCl2·6H2O的胶囊化竹纤维微管经过醋酸纤维素包封后形成分散性较好的胶囊化相变材料。
实施例4、制备天然亚麻纤维封装季戊四醇和Li2SO4并用聚丙烯腈包封的相变微胶囊
(1)芯材相变材料的液化
将10g有机相变材料季戊四醇(PE)和10g无机相变材料Li2SO4溶解到10mL去离子水和酒精的等体积混合溶液中获得液态的有机/无机混合相变材料;
(2)液态相变材料填充切短的天然微管
将5g长度为100-500μm的天然亚麻纤维分散于10mL步骤(1)的液态相变材料中,浸泡使毛细吸收达到平衡,使亚麻纤维管内充满液态的相变材料;
(3)微胶囊化相变材料的包封
将步骤(2)得到的含有去离子水和酒精溶剂的相变材料微胶囊中的去离子水和酒精挥发掉,使相变材料季戊四醇(PE)和Li2SO4的混合溶液浓缩固化后浸渍于5mL浓度为5%(质量百分含量)的聚丙烯腈的N,N’-二甲基甲酰胺溶液中,利用界面沉积反应,使微胶囊化的相变材料包封聚丙烯腈层;
(4)微胶囊化相变材料的提纯
将步骤(3)中包封了聚丙烯腈层的填充了相变材料的亚麻纤维,捞起后浸入去离子水凝固浴中使聚丙烯腈层固化,然后晾干。
此方法制备的相变微胶囊在循环升降温下具有很好的可循环相变储能效果,并且装填了相变材料季戊四醇(PE)和Li2SO4的胶囊化天然亚麻纤维微管经过聚丙烯腈包封后形成分散性较好的胶囊化相变材料。
Claims (5)
1.一种相变材料的微胶囊,由相变材料、切短的微管和聚合物组成;所述切短的微管是将中空管状天然纤维切成长度为0.1mm-5cm得到的纤维段;所述中空管状天然纤维直径为0.1-1000μm;所述相变材料封装在所述切短的微管中,所述切短的微管包覆于所述聚合物中;
所述天然纤维来源于下述4种天然纤维中的至少一种:木棉纤维、乳草纤维、竹纤维和亚麻纤维;
所述聚合物为下述三种聚合物中的任意一种或其任意共聚物或其任意共混物:脲醛树脂、聚丙烯腈和醋酸纤维素;
所述相变材料为下述1)和2)中的至少一种:1)为固-液相变材料,2)为固-固相变材料;
所述固液相变材料为下述a)和b)中的至少一种:a)为无机相变材料,b)为有机相变材料;
所述无机相变材料为结晶水合盐;
所述有机相变材料为高级脂肪烃;
所述固-固相变材料为无机盐或多元醇。
2.根据权利要求1所述的微胶囊,其特征在于:
所述结晶水合盐为碱金属或碱土金属的卤化物、硫酸盐、磷酸盐、硝酸盐或碳酸盐中的一种或其任意组合;
所述无机盐为KHF2;
所述高级脂肪烃为下述十六种物质中的一种或其任意组合:正二十八烷、正二十七烷、正二十六烷、正二十五烷、正二十四烷、正二十三烷、正二十二烷、正二十一烷、正二十烷、正十九烷、正十八烷、正十七烷、正十六烷、正十五烷、正十四烷和正十三烷;所述结晶高分子为密度高于0.94g/cm3的高密度聚乙烯、聚乙二烯或结晶聚氯乙烯;
所述多元醇为下述五种物质中的一种及其任意组合:季戊四醇、新戊二醇、2-氨基-2-甲基-1,3-丙二醇、三羟甲基乙烷和三羟甲基氨基甲烷。
3.一种制备权利要求1-2中任一所述的相变材料的微胶囊的方法,包括以下步骤:
1)将权利要求1-2中任一所述相变材料的微胶囊中的相变材料加热到熔点以上或用溶剂溶解得到液态的相变材料;
2)将权利要求1-2中任一所述相变材料的微胶囊中切短的微管分散于步骤1)的液态相变材料中,浸泡,通过毛细吸收使所述微管内充满液态的相变材料;
3)利用权利要求1-2中任一所述相变材料的微胶囊中的聚合物包覆步骤2)中填充了相变材料的切短的微管,得到权利要求1-2中任一所述的相变材料的微胶囊。
4.根据权利要求3所述的方法,其特征在于:所述方法还包括洗去得到的相变材料的微胶囊表面吸附的相变材料的步骤。
5.根据权利要求4所述的方法,其特征在于:所述溶剂为下述十种溶剂中的任意一种:去离子水、N,N’-二甲基甲酰胺、N,N’-二甲基乙酰胺、四氢呋喃、二氯甲烷、三氯甲烷、环己烷、甲醇、乙醇和丙酮。
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