CN112979219A - 兼具光热和焦耳热精油控释功能的多孔炭纤维材料及其制备方法 - Google Patents

兼具光热和焦耳热精油控释功能的多孔炭纤维材料及其制备方法 Download PDF

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CN112979219A
CN112979219A CN202110281822.1A CN202110281822A CN112979219A CN 112979219 A CN112979219 A CN 112979219A CN 202110281822 A CN202110281822 A CN 202110281822A CN 112979219 A CN112979219 A CN 112979219A
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essential oil
carbon fiber
porous carbon
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thermal
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CN112979219B (zh
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王邓峰
吴铭榜
龚文丽
叶昊
马璐琳
魏莉莉
姚菊明
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Zhejiang University of Technology ZJUT
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Abstract

本发明公开了一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料和制备方法。将纤维原料在碱液中预处理，而后浸渍在复配活化溶液中充分活化，分别在空气氛围和氮气氛围中进行预氧化炭化，制备多孔炭纤维材料；将多孔炭纤维研磨呈粉体，在粉末表面喷覆高分子溶液，升温交联后赋予炭纤维压片塑性性能；将制备多孔炭纤维炭片浸没于精油溶液中并充分震荡吸附，制取载香的多孔炭纤维/高分子复合材料。本发明利用多孔炭纤维材料高比表面积结构特征和材料自身光电热属性制备一种具有控释性能的精油载体；具有制备工艺简单，原料来源广泛，材料结构可控性强工艺特点，体具有精油吸附容量大、吸附稳定性和功能集成度高特点。

Description

兼具光热和焦耳热精油控释功能的多孔炭纤维材料及其制备 方法
技术领域
本发明涉及了一种多孔炭纤维材料的制备方法，具体涉及一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料及其制备方法。
背景技术
香熏精油是指从植物花、叶、水果皮、树皮等组织中所提出的一种缓释性油，它有植物特有的芳香以及多种药理效果，广泛应用于化妆、保健以及医疗等领域。但液体精油稳定性较差，在贮藏过程中对光、热、氧的敏感，导致气味缓释以及药理成分变质，从而失去使用价值。因此，液体精油在商用化过程中往往需要载体实现精油吸附固定与缓释，提升精油稳定性。
目前，植物精油缓释载体材料众多，其大多依赖高比表面积的多孔材料实现对精油的吸附、缓释。如中国专利CN103933597A以膨润土为原料制备多孔囊体，对精油中有机成分具有较好吸附固定作用，但该技术制备材料在精油释放过程中可控性较差，易于出现爆释。而随着微胶囊技术在精油包装领域应用，精油缓释成为可能，如中国专利CN111481450A通过将环糊精作为胶囊内壳，壳聚糖作为胶囊外壳制备一种植物精油微胶囊，通过摩擦使胶囊破裂达到缓慢释香效果。尽管微胶囊可以保护精油不受腐蚀、失活和氧化，但其工艺较为繁琐，仅实现精油缓释，对释放过程可控化程度仍然较低。近年来，利用介孔纳米材料作为精油的载体是提高精油应用品质、安全性和功能性的一种极具前景的方法。其中以介孔二氧化硅应用最为广泛，如中国专利CN201611111376.5报道的介孔二氧化硅能够对精油实现良好包裹，增加精油稳定性并延长功效。进一步的，将具有光电热效应的功能粒子掺入纳米材料载体中，即可通过光照、通电及加热方式实现精油可控释放，但功能粒子添加从一定程度上增加精油缓释载体制造成本和技术难度。
多孔多孔炭纤维材料是有纤维经活化炭化后制备的纤维状碳材料，表面形成了丰富纳米空间，具有极大比表面积和多级孔隙结构分布，同时表面分布活性基团，对有机化合物具有吸附化学亲和性。利用上述特点，多孔炭纤维对于精油这样小分子有机化合物具有高吸附活性和容量。值得注意的是，多孔炭纤维在聚集态结构上呈类石墨态，材料自身具有良好光热电效应，理论上，无需功能粒子添加即可实现精油可控化释放。
发明内容
为了解决背景技术中存在的问题，本发明提供了一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料及其制备方法，其目的克服目前精油微胶囊稳定性差，缓释性能可控性差及留香时间短的性能缺陷，又避免引入昂贵功能粒子造成制造成本和制造难度的增加。
本发明所采用的技术方案是：
1)制备复配前处理碱剂体系：将渗透剂、稳定剂及氢氧化钠在纯水中进行搅拌溶解制备第一溶液；
2)按一定浴比将纤维素原料置于第一溶液中，常温下搅拌并静置6小时，而后取出纤维充分洗净并在40℃烘干至恒重，获得预处理纤维；
3)制备活化体系：取渗透剂及化学活化剂在纯水中，充分搅拌制备第二溶液；
4)将步骤2)制备的预处理纤维加入到步骤3)制备的第二溶液中，浴比为5-10:1(预处理纤维：第二溶液，w/w)，常温下浸渍24h后取出，并在25-40℃烘除多余水分，得到活化纤维；
5)将步骤4)所得活化纤维在置于管式马弗炉中，在200℃条件下，空气氛围中加热2h，然后以5-10℃/min速率升温至一定温度，并调节为氮气氛围炭化一定时间，得到炭化纤维；
6)将步骤5)所得炭化纤维置于盐酸水溶液中，洗涤1h，然后用纯水充分冲洗，烘干多孔炭纤维；
7)取步骤6)中制备的多孔炭纤维研磨小于200目尺寸粉末，并喷覆一定浓度的高分子溶液，加热交联，并取0.5g交联多孔炭纤维置于直径为1cm圆柱形模具中，并在一定压力下挤压成型；
8)将步骤7)中制备的多孔炭纤维压片加入到一定浓度精油乙醇溶液中，待吸附稳定后，制得具有光电热控释性能的载香多孔炭纤维材料。
所述的步骤1)中：所述的渗透剂浓度1-2wt％，稳定剂浓度为0.5-1.5wt％，氢氧化钠浓度为4-8wt％。
所述步骤1)中，所述的渗透剂为硫酸化蓖麻油、烷基磺酸钠、烷基苯磺酸钠、烷基硫酸酯钠、仲烷基磺酸钠、仲烷基硫酸酯钠、一烯基磺酸钠、烷基萘磺酸钠、琥珀酸烷基酯磺酸钠、胰加漂T、氨基磺酸钠、脂肪醇聚氧乙烯醚、烷基酚聚氧乙烯醚、聚醚、磷酸酯类化合物中的至少一种，优选的是烷基磺酸钠、烷基苯磺酸钠、烷基硫酸酯钠。
所述步骤1)中稳定剂为羧甲基纤维素、三乙醇胺、椰子油酸、二乙醇胺、乙醇、丙三醇、十二醇、聚丙烯酞胺、聚乙烯醇中的至少一种，优选的是羧甲基纤维素。
3、根据权利要求1所述的一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料的制备方法，其特征在于：
所述的步骤(2)中：所述的浴比为10-20:1(第一溶液：纤维原料，w/w)。
所述步骤(2)中，所述的纤维素原料为棉、竹纤维、大麻、亚麻、汉麻、木棉、萝藦绒、黏胶、剑麻、苎麻其各类纤维素纤维及衍生纤维素制品中的至少一种，优选的是木棉、棉、萝藦绒、竹及衍生纺织品。
所述的步骤3)中：所述的渗透剂浓度为1-2wt％，化学活化剂浓度为10-50wt％。
所述步骤3)中，所述的渗透剂为硫酸化蓖麻油、烷基磺酸钠、烷基苯磺酸钠、烷基硫酸酯钠、仲烷基磺酸钠、仲烷基硫酸酯钠、一烯基磺酸钠、烷基萘磺酸钠、琥珀酸烷基酯磺酸钠、胰加漂T、氨基磺酸钠、脂肪醇聚氧乙烯醚、烷基酚聚氧乙烯醚、聚醚、磷酸酯类化合物中的至少一种。步骤3)中所述的渗透剂优选的是烷基磺酸钠、烷基苯磺酸钠、烷基硫酸酯钠。
所述步骤3)中的化学活化剂为KOH、NaOH、ZnCl2、H3PO4、NH4H2PO4、(NH4)2HPO4、K2S、CaCl2、K2CO3、Na2CO3、H2SO4、C6H18O24P6(植酸)中至少一种。所述的化学活化剂优选的是H3PO4、NH4H2PO4、(NH4)2HPO4。
所述的步骤5)中：氮气氛围加热温度450-900℃，氮气氛围加热时间为50-100min。
所述的步骤6)中，盐酸摩尔浓度为0.01～1mol/L。
步骤(6)中优选的是洗涤方式是超声震荡洗涤、真空循环抽滤洗涤、水浴震荡洗涤。
优选的是干燥方式包括鼓风烘箱干燥，真空烘箱干燥，冷冻干燥，超临界二氧化碳干燥。
所述的步骤7)中：所述的高分子溶液浓度为1-2wt％，交联温度50-70℃，挤压成型的压力0.5-1Mpa。
所述步骤7)中，所述的高分子溶液的溶质为淀粉、动物皮胶、骨胶、聚乙烯醇、天然橡胶、环氧树脂、酚醛树脂、脲醛树脂、聚氨酯、过氯乙烯树脂、氯丁橡胶、丁腈橡胶、硅酸盐、磷酸盐中的中至少一种，优选的是淀粉、聚乙烯醇；溶剂为水、乙醇、正丁醇、异丙醇、N-N二甲基甲酰胺中至少一种，优选的是水和乙醇。
所述的步骤8)中，精油乙醇溶液中的精油浓度范围1-30wt％，搅拌浸渍时间为1-12h。
所述的步骤8)中，所述的精油为玫瑰精油、杜鹃花精油、万寿菊精油、月桂精油、洋甘菊精油、茉莉精油、金银花精油、紫罗兰精油、白玉兰精油、天竺葵精油、依兰精油、薰衣草精油、牡丹精油、薄荷精油、橙花精油、松脂精油、丁香精油、榄香脂精油、豆蔻精油、柠檬精油、甜橙精油、葡萄柚精油、红柑精油、广藿香精油、留兰香精油、欧白芷精油、香根精油、藏回香精油、龙艾精油、檀香精油、沉香精油、香蜂草精油、月见草精油、茶树精油、杏仁精油、石榴精油中的至少一种。
本发明包括将纤维原料在碱液中预处理，以去除原料可溶性杂质，而后浸渍在复配活化溶液中充分活化，分别在空气氛围和氮气氛围中进行预氧化炭化，制备多孔炭纤维材料；将多孔炭纤维研磨呈粉体，并在粉末表面喷覆高分子溶液，升温交联后赋予炭纤维压片塑性性能；将制备多孔炭纤维炭片浸没于精油溶液中并充分震荡吸附，制取载香的多孔炭纤维/高分子复合材料。本发明利用多孔炭纤维材料高比表面积结构特征和材料自身光电热属性制备一种具有控释性能的精油载体。
利用本发明通过控制活化剂种类、活化炭化温度以及炭化时间进而实现多孔炭纤维结构性能调控，进而调节其对不同种类精油吸附容量；此外，通过调控光照、电压、温度等因素调节多孔炭纤维对精油缓释速度。
本发明具有有益效果如下：
本发明的高比表面积多孔炭纤维材料，实现精油负载和控释，具有以下突出有益效果：
(1)以天然纤维素基材料为原料，具有价格低廉，来源广泛以及环保可再生优势，同时制备介孔多孔炭纤维无味、无毒，适用于不同精油控释以及不同应用场景；
(2)多孔炭纤维材料载体材料制备工艺简单便捷，而多孔炭纤维载体具有比表面积、孔径可控、精油负载量大等突出优势；
(3)传统光电热控释材料是通过向精油载体基材中添加功能粒子(石墨烯、MXene)等材料实现，其工艺较为复杂，成本较高，本发明中设计多孔炭纤维材料因达比表面积和多孔优势即可作为精油载体，同时其作为碳材料固有属性赋予自身光热和焦耳热控释效应，具有功能集成化优势，且成本较低。
附图说明
表1不同制备工艺条件材料比表面积及孔径分布；
图1不同活化剂活化的材料黑暗条件下的精油吸附量及释放速率图；
图2不同活化温度条件下材料黑暗条件下的精油吸附量及释放速率图；
图3不同活化时间条件下材料黑暗条件下的精油吸附量及释放速率图；
图4不同压片压力条件下材料黑暗条件下的精油吸附量及释放速率图；
图5材料对于不同种类精油的吸附量及释放速率图；
图6不同光照强度下材料的精油吸附量及释放速率图；
图7不同电压条件下材料的精油吸附量及释放速率图；
图8不同温度条件下材料的精油吸附量及释放速率图。
具体实施方式
通过以下实施例对本发明做更详细的描述，但所述实施例不构成对本发明的限制。
本发明所制备的材料用于储存及释放精油，精油吸附量和释放速度是评价该材料性能的两个重要参数。
吸附量的定义：在一定温度条件下，单位质量的多孔炭纤维压片所能吸附的精油的质量，其单位为mg/g，公式为：
Figure BDA0002978852200000051
其中，Qe为精油吸附量，单位为mg/g；m0表示挤出粒子初始干重，单位为g；m1表示挤出粒子吸附精油后的干重，单位为g。
释放速度的定义：在一定温度条件下，单位时间内释放的精油的质量，单位为μg/min，公式为：
Figure BDA0002978852200000052
其中，S表示精油的释放速度，单位为mg/min；m2表示吸附精油的挤出粒经过t时间后的质量，单位为mg；m1为挤出粒子吸附精油后的干重，单位为mg；t为释放精油的时间，单位为min。
下面结合实施例对本发明做进一步说明。
本发明的实施例如下：
实施案例1：
1)、将1wt％十二烷基苯磺酸钠、5wt％氢氧化钠溶于水，搅拌溶解，再加入稳定剂组分1wt％羧甲基纤维素，搅拌混匀，即得复配预处理溶液；
2)、将10g棉纤维加入制备的100mL复配预处理溶液中，低速搅拌溶12h，取出洗净并于40℃烘干至恒重；
3)、制备活化体系：将1wt％十二烷基苯磺酸钠、30wt％磷酸溶液溶于水，搅拌溶解，即得活化溶液；
4)、取5g步骤2)制备的预处理棉纤维加入到步骤3)制备的30mL活化体系中，完全浸没24h后取出，并置于25～40℃烘干；
5)、将步骤4)所得纤维在置于管式马弗炉中，通空气条件，通空气条件下以5℃/min速率加热至200℃，预氧化2h，后在真空条件下，并以上述加热速率升温至500℃，炭化70min后，得到炭化纤维；
6)将步骤5)所得炭化纤维置于1mol/L盐酸中，超声洗涤1h，而后用纯水充分冲洗，烘干得多孔炭纤维。
7)取步骤6)中制备的多孔炭纤维研磨小于200目尺寸粉末，并喷覆2wt％的PVA高分子溶液，60℃交联，并取0.5g交联多孔炭纤维置于直径为1cm圆柱形模具中，在0.5Mpa压力下挤压成型；
8)将步骤7)中制备的多孔炭纤维压片加入到10wt％玫瑰精油/乙醇溶液中，待其吸附稳定后(12h)，制得兼具有光热和焦耳热控释性能的载香多孔炭纤维材料。
本实例中，精油缓释速度统计在黑暗、室温(25℃)和无外接电压条件下进行的。
实施例2-5：将实施例1中活化剂更换成KOH、ZnCl2、NH4H2PO4、(NH4)2HPO4，其余条件同实施例1。结果表明，KOH活化的多孔炭纤维具有最大精油吸附量，达351.8mg/g，而磷酸活化多孔炭纤维对于精油存贮效果最好，缓释速度最慢，达41.24μg/min。(见图1)
Figure BDA0002978852200000061
实施例6-13：将实施例1中炭化温度条件改为550、600、650、700、750、800、850、900℃，其余条件同案例1。结果表明，随着炭化温度上升，多孔炭纤维精油吸附量呈现先增大后降低趋势，当炭化温度为600℃时，样品精油吸附达达到最大，可达395.6mg/g。(见图2)
Figure BDA0002978852200000071
实施例14-18：将实施例1中炭化时间条件改为50、60、80、90和100min，其余条件同案例1。结果表明，最优炭化时间对多孔炭纤维精油吸附量及缓释速度均产生影响，其中当炭化时间为70min，样品精油吸附量达最大值，而从50-100min内，随着炭化时间延长，样品对精油缓释速度逐渐升高。(见图3)
Figure BDA0002978852200000072
实施例19-23：将实施例1中挤压压力改为0.6、0.7、0.8、0.9和1.0Mpa，其余条件同案例1。结果表明，随着压片压力的提升，粉末状多孔炭纤维逐渐被压紧实，故其对精油吸附量不断降低，但该因素对精油缓释速度影响不大。(见图4)
Figure BDA0002978852200000073
实施例24-33：将实施例1中所吸附精油更改为杜鹃花精油、万寿菊精油、月桂精油、薰衣草精油、茉莉精油、金银花精油、紫罗兰精油、白玉兰精油、柠檬精油和沉香精油，其余条件同案例1。结果表明多孔炭纤维载体对于不同精油具有良好吸附性能，其吸附量在300～400mg/g区间内，缓释速度大多集中在40μg/min左右。(见图5)
精油种类 实施例 吸附量(mg/g) 缓释速度(μg/min)
杜鹃花精油 实施例24 345.8 40.89
万寿菊精油 实施例25 364.5 41.06
月桂精油 实施例26 354.0 40.56
薰衣草精油 实施例27 348.4 40.75
茉莉精油 实施例28 361.6 39.41
金银花精油 实施例29 359.9 38.98
紫罗兰精油 实施例30 357.8 41.65
白玉兰精油 实施例31 360.1 43.64
柠檬精油 实施例32 362.6 39.87
沉香精油 实施例33 358.7 39.16
实施例34-40：在精油释放过程中，依次将实施例1中精油缓释测试中黑暗条件更改为光强为0.05、0.10、0.20、0.25、0.30、0.35、0.40W/cm2的直射光源。结果表明，随着光源强度增加，多孔炭纤维单位时间吸收能量增加，并大量转化热能，导致缓释速度显著增加。(见图6)
Figure BDA0002978852200000081
实施例41-48：在精油释放过程中，依次将实施例1中精油缓释测试中缓释温度更改为10、20、30、40、50、60、70、80℃，其余条件同为实施例1。结果表明，升温能明显提升精油的缓释速度，当温度达到80℃时，其缓释速度将达到85.41μg/min，这表明可通过温度调控进而控制多孔炭纤维的精油释放速度。(见图7)
Figure BDA0002978852200000091
实施例49-56：在精油释放过程中，依次将实施例1中精油缓释测试中多孔炭纤维压片施加外界电压5、10、15、20、25、30、35、40V，其余条件同为实施例1。结果表明多孔炭纤维具有明显电热效应，其通过加压能够显著提高精油缓释速度，且缓释速度跟电压呈一定线性关系，这表明本发明材料具有电控缓释能力。(见图8)
Figure BDA0002978852200000092
由上述实施可见，本发明在制备方法操作简单，可控性强，可以通过控制活化剂种类、炭化温度和炭化时间等多个工艺参数实现产品的比表面积和孔径的调控，进而影响其精油释放性能；此外，产品在黑暗条件下精油香气释放速度缓慢而稳定，从光(光强)、热(温度)和电(电压)三个维度均可实现精油缓释速度调节，进而控制其缓释进程。
不同条件下制取多孔炭纤维的比表面积和孔径特征如表1，其中实施例1-5、6-13和14-18分别对应活化剂种类、炭化温度和炭化时间对应多孔炭纤维结构影响规律。
表1不同样品的比表面积和孔容特征
Figure BDA0002978852200000101
由表1数据可见，上述参数均对多孔炭纤维比表面积、孔径以及孔容造成明显影响，其中KOH活化的多孔炭纤维比表面最高，达2143m2/g，对应孔径和孔容分别为1.74nm和2.04cm3/g，此外，以磷酸活化为例，600℃炭化温度和70min炭化时间为最优制备工艺。
由此实施可见，本发明具有制备工艺简单，原料来源广泛，材料结构可控性强工艺特点，所制备多孔炭纤维精油载体具有精油吸附容量大、吸附稳定性和功能集成度高特点，便于存储运输，可以通过外界光、热、电条件控制实现精油释放速率的调控，是一种便于规模化生产。

Claims (10)

1.一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料的制备方法，其特征在于：包括以下步骤：
1)制备复配前处理碱剂体系：将渗透剂、稳定剂及氢氧化钠在纯水中进行搅拌溶解制备第一溶液；
2)按一定浴比将纤维素原料置于第一溶液中，常温下搅拌并静置6小时，而后取出纤维充分洗净并在40℃烘干至恒重，获得预处理纤维；
3)制备活化体系：取渗透剂及化学活化剂在纯水中，充分搅拌制备第二溶液；
4)将步骤2)制备的预处理纤维加入到步骤3)制备的第二溶液中，浴比为5-10:1，常温下浸渍24h后取出，并在25-40℃烘除多余水分，得到活化纤维；
5)将步骤4)所得活化纤维在置于管式马弗炉中，在200℃条件下，空气氛围中加热2h，然后以5-10℃/min速率升温至一定温度，并调节为氮气氛围炭化一定时间，得到炭化纤维；
6)将步骤5)所得炭化纤维置于盐酸水溶液中，洗涤1h，然后用纯水充分冲洗，烘干多孔炭纤维；
7)取步骤6)中制备的多孔炭纤维研磨小于200目尺寸粉末，并喷覆一定浓度的高分子溶液，加热交联，并取0.5g交联多孔炭纤维置于直径为1cm圆柱形模具中，并在一定压力下挤压成型；
8)将步骤7)中制备的多孔炭纤维压片加入到一定浓度精油乙醇溶液中，待吸附稳定后，制得具有光电热控释性能的载香多孔炭纤维材料。
2.根据权利要求1所述的一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料的制备方法，其特征在于：所述的步骤1)中：所述的渗透剂浓度1-2wt％，稳定剂浓度为0.5-1.5wt％，氢氧化钠浓度为4-8wt％。
3.根据权利要求1所述的一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料的制备方法，其特征在于：所述的步骤(2)中：所述的浴比为10-20:1。
4.根据权利要求1所述的一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料的制备方法，其特征在于：所述的步骤3)中：所述的渗透剂浓度为1-2wt％，化学活化剂浓度为10-50wt％。
5.根据权利要求1一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料的制备方法，其特征在于：所述的步骤5)中：氮气氛围加热温度450-900℃，氮气氛围加热时间为50-100min。
6.根据权利要求1所述的一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料的制备方法，其特征在于：所述的步骤6)中，盐酸摩尔浓度为0.01～1mol/L。
7.根据权利要求1所述的一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料的制备方法，其特征在于：所述的步骤7)中：所述的高分子溶液浓度为1-2wt％，交联温度50-70℃，挤压成型的压力0.5-1Mpa。
8.根据权利要求1所述的一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料的制备方法，其特征在于：所述步骤7)中，所述的高分子溶液的溶质为淀粉、动物皮胶、骨胶、聚乙烯醇、天然橡胶、环氧树脂、酚醛树脂、脲醛树脂、聚氨酯、过氯乙烯树脂、氯丁橡胶、丁腈橡胶、硅酸盐、磷酸盐中的中至少一种；溶剂为水、乙醇、正丁醇、异丙醇、N-N二甲基甲酰胺中至少一种。
9.根据权利要求1所述的一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料的制备方法，其特征在于：所述的步骤8)中，精油乙醇溶液中的精油浓度范围1-30wt％，搅拌浸渍时间为1-12h。
10.一种兼具光热和焦耳热精油控释功能的多孔炭纤维材料，其特征在于：由权利要求1～9任一项所述的制备方法制得。
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