CN111663335A - 一种柔性光/电-热双响应相变布制备方法 - Google Patents
一种柔性光/电-热双响应相变布制备方法 Download PDFInfo
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- CN111663335A CN111663335A CN202010557823.XA CN202010557823A CN111663335A CN 111663335 A CN111663335 A CN 111663335A CN 202010557823 A CN202010557823 A CN 202010557823A CN 111663335 A CN111663335 A CN 111663335A
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
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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
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
本发明公开了一种柔性光/电‑热双响应相变布，其以碳纤维布为基底，包括生长在碳纤维上的金属有机骨架材料，以及吸附在所述金属有机骨架材料中的相变储能材料。本发明还公开了制备方法，主要包括（1）在碳纤维布上原位合成金属有机骨架，得到碳纤维布@MOFs载体；（2）溶液浸渍法吸附相变材料，获得柔性光/电‑热双响应相变布。本发明柔性光/电‑热双响应相变布通过基底布、相变芯材和MOFs的有机结合，有效的改善有机相变材料无法实现光/电响应及其热致变形和高温泄露的缺点，具有高光/电‑热转换能力、强结构完整性、高循环稳定性和优异抗剪切性能的优势，具有广阔的应用前景。
Description
技术领域
本发明属于纳米复合材料和复合相变材料领域，具体涉及一种柔性光/电-热双响应相变布的制备方法。
背景技术
可再生能源在替代化石燃料的过度开发与使用方面发挥重要的作用。其中，太阳能作为一种丰富而持久的可再生能源在光电转换与光催化领域取得了显著的应用效果。但是，上述太阳能系统仍受限于能源转换效率低的问题。如果把可以同时储存与释放热能的相变材料应用到光热转换领域上将有效的提升太阳能的利用率。然而，大多数相变材料对光的吸收能力差，并且，存在热致变形的问题。此外，阳光的间歇性问题导致了热量的间断性。因此，在保障光热体系良好力学性能的同时实现热能的持续供应仍是一个挑战，开发具有优异力学性能的光/电-热双响应相变材料具有重要意义。
碳布作为一种具有优异光吸收与导电性能的柔性材料因其可以为体系提供连续的电子传输通道并促进热量的持续供应。但是，不能将碳布直接用为光/电-热双响应相变材料，这主要受限于碳布无法负载具有蓄传热性能的相变芯材。
发明内容
本发明的目的在于针对现有技术的不足，提供一种柔性光/电-热双响应相变布，其以碳纤维布为基底，包括生长在碳纤维上的金属有机骨架材料，以及吸附在所述金属有机骨架材料中的相变材料。一方面，MOFs孔道的表面张力、毛细作用力或者氢键作用力可将相变芯材有效地封装于孔道中，进而实现复合相变材料的高芯材负载量与高相变焓值。另一方面，碳布@MOFs的多级孔结构促进太阳光在碳布表面的聚集，增强对光源的捕获，进而提升光-热转换效率。与此同时，柔性的碳布基底为体系提供连续的电子传输通道，实现相变材料在低激发电压下由电能向热能的快速转换。此外，MOFs增加载体材料的浸润性，PCM与碳布通过MOFs实现链锁效应，增强材料的抗剪切性能。
适用于本申请的相变材料可多元醇类、脂肪酸类、直链烷烃中的一种或多种任意组合。其中，所述多元醇类包括但不限于聚乙二醇(平均分子量为1000-20000)，新戊二醇、季戊四醇等；所述脂肪酸类包括但不限于硬脂酸、肉豆蔻酸、棕榈酸、月桂酸、十五烷酸、癸酸、癸二酸等；所述直链烷烃包括但不限于正十六烷、正十烷、正十四烷、正十八烷等。
本发明的另一目的在于提供上述柔性光/电-热双响应相变布的制备方法，包括以下步骤：
(1)在碳纤维布上原位合成金属有机骨架，得到碳纤维布@MOFs载体；
(2)将步骤1制备的碳纤维布@MOFs载体在40～200℃条件下抽真空2～10h，然后置于相变材料的溶液中，其中碳纤维布@MOFs载体的质量与溶液中相变材料的质量之比在1：9以上，然后在高于相变材料相变温度的条件下干燥，得到碳布@MOFs基复合相变材料。
在某些实施例中，采用如下方法进行原位合成：将碳纤维布浸泡于30mL浓HNO3溶液中，100℃下反应3h后，真空干燥24h得到活化的碳纤维布；将活化的碳纤维布浸渍于含有可溶性金属盐与有机羧酸配体的DMF或水溶液中，其中可溶性金属盐与有机羧酸配体的摩尔比为2:1；在100-200℃下的50mL反应釜中反应12～48h，用N,N-二甲基甲酰胺(DMF) 过滤洗涤三次，去除副产物及杂质，在60～150℃下干燥4～48h，得到碳布@MOFs载体材料。
适用于本发明金属有机骨架合成的可溶性金属盐包括但不限于：硝酸锌、氯化锌、硫酸锌、醋酸锌、硝酸铁、氯化铁、硫酸铁、醋酸铁、硝酸钴、氯化钴、硫酸钴、醋酸钴、硝酸铜、氯化铜、硫酸铜、醋酸铜、硝酸铬、氯化铬、硫酸铬、醋酸铬、硝酸锆、氯化锆、硫酸锆、醋酸锆、硝酸镍、硫酸镍、醋酸镍、氯化镍、硝酸铝、硫酸铝、醋酸铝、氯化铝、硝酸锰、氯化锰、硫酸锰、醋酸锰、硫酸钛硝酸钛、氯化钛、等其中的一种或几种；有机羧酸配体包括但不限于：对苯二甲酸、2-硝基对苯二甲酸、2-磺酸基对苯二甲酸、2-氨基对苯二甲酸等其中的一种或几种。
本发明的有益效果在于：
本发明的优点在于：柔性光/电-热双响应相变布通过基底布、相变芯材和MOF的有机结合，有效的改善有机相变材料的吸光能力差、电导率能低、热致变形、容易泄露的缺点，具有高光/电热转换能力、强结构完整性、高循环稳定性和优异抗剪切性能的优势，具有广阔的应用前景。
1)碳布@MOFs的多级孔结构促进太阳光直接在碳布表面的聚集，增强对光源的捕获，进而有效提升材料的光-热转换效率；
2)碳布作为电子传输通道，可以实现电能向热能的快速转换，同时碳布柔性基底保障了材料的连续性与结构完整性，扩展了光/电-热双响应相变材料的应用范围；
3)多级孔结构MOFs作为储能单元，利用孔道的表面张力，毛细作用力或氢键作用力将相变芯材有效地封装于孔道中，有效解决碳布材料无法储能的核心问题；
4)本发明提供的制备方法简单、光/电热性能好、结构完整性强、芯材选择多样化、循环稳定性好、适合规模化生产。
附图说明
图1为本发明实施案例1得到的碳布@MOFs载体的SEM图谱。
图2为本发明实施案例1得到的碳布@MOFs载体的XRD图谱。
图3为本发明实施案例1得到的碳布@MOFs载体负载PEG2000的XRD图谱。
图4为本发明实施案例1得到的碳布@MOFs载体负载PEG2000的DSC图谱。
图5为本发明实施案例1得到的碳布@MOFs载体负载PEG2000的光热温度变化曲线。
图6为本发明实施案例1得到的碳布@MOFs载体负载PEG2000的电热温度变化曲线。
图7为本发明实施案例1得到的碳布@MOFs载体负载PEG2000的抗剪切性能对比图。
具体实施方式
下面结合具体的实施方式对本发明的技术方案做进一步说明。
实施案例1
(1)碳布@MOF-5载体材料的制备：
将2cm*3cm的碳布浸泡于30mL浓HNO3溶液中，100℃下反应3h后，真空干燥24h 得到活化的碳布；将活化的碳布(2cm*3cm)置于含有0.743g六水合硝酸锌和0.207g对苯二甲酸的25mL DMF溶剂中，并将其置入50mL反应釜中。在120℃下反应10h后，用DMF 过滤洗涤3次，在80℃下干燥24h，得到碳布@MOF-5载体材料。
(2)复合相变材料的制备：
将上述制备的碳布@MOF-5(2cm*3cm)载体材料在120℃条件下抽真空8h，将基体的孔道完全打开。将0.18g PEG2000溶解在20mL乙醇中，得到均匀的相变材料溶液。然后将载体材料置入准备好的相变材料溶液中，然后置于80℃烘箱中干燥24h，得到PEG2000/ 碳布@MOF-5光/电-热双响应相变材料。
从图1的SEM图中可以观察到，MOF-5均匀的生长在碳纤维的表面，因此该多孔结构在吸附芯材分子方面拥有较强的潜力。从图2的XRD结果中可以观测到MOF-5的所有特征峰，结合图1的SEM扫描电镜结果，证实了采用本方案可以成果制备碳布@MOF-5载体材料，碳布@MOF-5载体将PEG2000吸附至其多级孔道内，同时在吸附饱和后，其表面继续吸附部分PEG2000，因此从图3柔性相变布的XRD结果中可以观测到PEG2000的显著特征峰，证实了采用本实验方案成功获得了具有优异结晶性能的柔性相变布。图4所示的DSC测试结果表明，柔性相变布的的融化温度为61.6℃，熔融焓为116.5J/g，融化温度为31.5℃，熔融焓为112.3 J/g。图5光热性能测试结果表明，该柔性相变布可以在1Sun(模拟标准太阳光)的光强下于300s内升温至138℃，图6电热性能测试结果表明，该柔性相变布可以在2.0V的低激发电压下于42s内迅速实现热量的存储与转换，同时图7的剪切强度测试结果表明，该柔性导电相变布的剪切强度比纯碳布提升了61.5％，以上结果有力的证明本发明制备的柔性光/电-热双响应相变布具有优异的光/电热转换与存储特性以及良好的力学性能，有效解决了碳布材料无法储能以及相变材料的吸光能力差、电导率能低、热致变形、容易泄露的核心问题，同时提供的制备方法简单，适合规模化生产。
实施案例2
(1)碳布@IRMOF-3载体材料的制备：
将2cm*3cm的碳布浸泡于30mL浓HNO3溶液中，100℃下反应3h后，真空干燥24h 得到活化的碳布；将活化的碳布(2cm*3cm)置于含有0.892g六水合硝酸锌、0.181g 2-氨基对苯二甲酸的30mL DMF溶剂中，并将其置入50mL反应釜中。在100℃下反应24h后，用DMF过滤洗涤3次，在80℃下干燥24h，得到碳布@IRMOF-3载体材料。
(2)复合相变材料的制备：
将0.25g上述制备的碳布@IRMOF-3(2cm*3cm)载体材料在120℃条件下抽真空8h，将基体的孔道完全打开。将0.25g十八酸溶解在20mL乙醇中，得到均匀的相变材料溶液。然后将载体材料置入准备好的相变材料溶液中，然后置于80℃烘箱中干燥24h，得到十八酸 /碳布@IRMOF-3光/电-热双响应相变材料。
测试结果表明，该柔性导电相变布可以在1Sun(模拟标准太阳光)的光强下于300s内升温至102℃，并且在3.2V的激发电压下于58s内实现热量的存储与转换，同时其剪切强度比纯碳布提升了46.2％。
实施案例3
(1)碳布@MIL-101(Cr)-NH2载体材料的制备：
将2cm*3cm的碳布浸泡于30mL浓HNO3溶液中，100℃下反应3h后，真空干燥24h 得到活化的碳布；将活化的碳布(2cm*3cm)置于含有1.6g九水合硝酸铬和0.72g 2-氨基对苯二甲酸和0.4g NaOH的30mL去离子水中，并将其置入50mL反应釜中。在150℃下反应 12h后，用DMF过滤洗涤3次，在80℃下干燥24h，得到碳布@MIL-101(Cr)-NH2载体材料。
(2)复合相变材料的制备：
将上述制备的碳布@MIL-101(Cr)-NH2(2cm*3cm)载体材料在120℃条件下抽真空8h，将基体的孔道完全打开。将0.20g十八酸溶解在20mL乙醇中，得到均匀的相变材料溶液。然后将载体材料分散入准备好的相变材料溶液中，然后置于80℃烘箱中干燥24h，得到十八酸/碳布@MIL-101(Cr)-NH2光/电-热双响应相变材料。
测试结果表明，该柔性导电相变布可以在1Sun(模拟标准太阳光)的光强下于300s内升温至116℃，并且在2.8V的激发电压下于69s内实现热量的存储与转换，同时其剪切强度比纯碳布提升了52.6％。
Claims (5)
1.一种柔性光/电-热双响应相变布，其特征在于，包括碳纤维布，生长在碳纤维上的金属有机骨架材料，以及吸附在所述金属有机骨架材料中的相变材料。
2.根据权利要求1所述的柔性光/电-热双响应相变布，其特征在于，相变材料选自多元醇类、脂肪酸类、直链烷烃中的一种或多种任意组合。
3.根据权利要求2所述的柔性光/电-热双响应相变布，其特征在于，所述多元醇类包括聚乙二醇(平均分子量为1000-20000)，新戊二醇、季戊四醇等；所述脂肪酸类包括硬脂酸、肉豆蔻酸、棕榈酸、月桂酸、十五烷酸、癸酸、癸二酸等；所述直链烷烃包括：正十六烷、正十烷、正十四烷、正十八烷等。
4.如权利要求1所述的柔性光/电-热双响应相变布的制备方法，其特征在于，包括以下步骤：
（1）在碳纤维布上原位合成金属有机骨架，得到碳纤维布@MOFs载体；
（2）将步骤1制备的碳纤维布@MOFs载体在40~200 ℃条件下抽真空2～10 h，然后置于相变材料的溶液中，其中碳纤维布@MOFs载体的质量与溶液中相变材料的质量之比在1：9以上，然后在高于相变材料相变温度的条件下干燥，得到碳布@MOFs基复合相变材料。
5.根据权利要求4所述的制备方法，其特征在于，所述步骤（1）具体为：
将碳纤维布浸泡于30 mL浓HNO3溶液中，100 ℃下反应3 h后，真空干燥24 h得到活化的碳纤维布；将活化的碳纤维布浸渍于含有可溶性金属盐与有机羧酸配体的DMF或水溶液中，其中可溶性金属盐与有机羧酸配体的摩尔比为2:1；在100-200 ℃下的50 mL反应釜中反应12~48 h，用N,N-二甲基甲酰胺（DMF）过滤洗涤三次，去除副产物及杂质，在60~150℃下干燥4~48 h，得到碳布@MOFs载体材料。
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