CN113321817A - 一种纳米木质素制备过程关键变量的分析方法 - Google Patents
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Abstract
纳米木质素的制备过程是包含诸多变量的复杂体系。本发明提供了一种纳米木质素制备过程关键变量的分析方法。采用大数据分析中的多变量分析进行纳米木质素制备过程变量之间相互关系的确定及在诸多变量中确定对产物影响的关键变量。采用主成分分析法和偏最小二乘法进行纳米木质素制备过程数据库的分析,根据分析得到的变量关系,揭示利用绿色溶剂制备纳米木质素的机理。本发明操作简便,便于实施,分析得到的关键变量对纳米木质素的工业化大规模制备具有重要的指导意义。
Description
技术领域
本发明属于生物基纳米材料制备领域,尤其是涉及纳米木质素的制备,是一种纳米木质素的制备过程中关键变量的分析方法。
背景技术
木质纤维素类生物质是可再生的循环利用的资源,木质纤维素类生物质的三大组成成分是纤维素、半纤维素和木质素。木质素是含有芳香结构的天然高分子化合物,是广泛存在于生物质中,在植物纤维结构中具有重要的粘结作用。目前对木质素的高附加值利用是研究的热点。其中,将木质纤维素类生物质中的木质素制备成纳米尺寸范围的纳米木质素是全球的研究热点之一。纳米木质素在多个领域都展现出巨大的发展潜力。
纳米木质素的制备过程是包含诸多变量的一个复杂***的过程,各变量之间相互作用,改变一个变量则或出现牵一发而动全身的效果,因此,找到制备纳米木质素过程中的关键变量,对于高效制备纳米木质素来说具有重要意义。纳米木质素制备过程中的变量诸多,比如有生物质原料的各项物化性质参数、反应试剂的各项物化性质参数、反应条件的各项参数、制备成的纳米木质素各物化性质的参数等。因此,全面整体研究整个过程中所有变量之间的相互关系或内在关联可以剖析纳米木质素的制备原理,找到对整个制备过程起到关键作用的变量是目前亟待解决的问题。
发明内容
为了解决上述问题,本发明提供了木质纤维素类生物质制备纳米木质素过程的关键变量的分析方法。本方法操作简单、易于实现。为后续大规模工业化生产纳米木质素提供了理论指导。
为了实现上述目的,本发明采用的技术方案如下,基于大数据处理中的多变量分析进行研究,具体包括:
(1)收集制备纳米木质素的原料的各项物化性质参数;优选地,所述的原料为木质纤维素类生物质原料,如农林废弃物、餐余废弃物等,更优选地,为玉米秸秆、小麦秸秆、柳枝稷、针叶木木屑、阔叶木木屑等。
(2)收集纳米木质素制备过程所用溶剂的各项物化性质参数;优选地,溶剂为低共熔溶剂,更优选地为二元或者三元低共熔溶剂,更加优选地为氯化胆碱基的低共熔溶剂,更加优选地为氯化胆碱基的酸性的二元或者三元低共熔溶剂。
(3)收集纳米木质素制备反应条件的各项参数;优选地,反应条件为反应压力、反应时间、反应搅拌程度、反应固液比、反应剧烈程度等。更优选地,固液比为1-100,反应温度为60-180℃,反应时间为10min-300min。
(4)收集所制备的纳米木质素各物化性质的参数;优选地,纳米木质素各参数为木质素得率、粒径、纯度、分子量、基团含量、分散性等参数。
(5)进行多变量分析,剖析各变量之间的相互关系,揭示制备机理,找到具有生产指导意义的关键制备变量。优选地,多变量分析为主成分分析、偏最小二乘法分析等其中的一种或几种组合。
本发明的优点在于:
(1)采用了多变量分析,基于大数据处理,进行了纳米木质素制备过程的***研究。
(2)根据多变量分析的结果,达到在诸多变量中确定制备纳米木质素关键变量的目的。
(3)方法简单,具有普遍性,易于推广,对大规模生产纳米木质素具有重要的指导意义。
(4)明确了各变量之间的相关性,对于调整变量发生的结果可以进行初步预测。
具体实施方式
应该指出,以下详细说明都是例示性的,旨在对本发明提供进一步的说明。除非另有指明,本发明使用的所有技术和科学术语具有与本发明所属技术领域的普通技术人员通常理解的相同含义。
需要注意的是,这里所使用的术语仅是为了描述具体实施方式,而非意图限制根据本发明的示例性实施方式。如在这里所使用的,除非上下文另外明确指出,否则单数形式也意图包括复数形式,此外,还应当理解的是,当在本说明书中使用术语“包含”和/或“包括”时,其指明存在特征、步骤、操作、器件、组件和/或它们的组合。
下面结合具体的实施例,对本发明做进一步的说明,但本发明并不限于此。
实施例1
采用低共熔溶剂与木质纤维素类生物质反应,反应后进行固液分离,将液体部分进行反溶剂沉淀析出、离心分离、真空抽滤等操作获得纳米木质素产品。低共熔溶剂为基于氯化胆碱的二元和三元的酸性的低共熔溶剂。木质纤维素类生物质是玉米秸秆、小麦秸秆、柳枝稷、杨木木片、桉木木片、苹果皮、甘蔗渣、龙竹、桦木木片、芦苇、水稻秆。原料粉碎后的目数为20-60目。反应温度为80-200℃、反应时间为60min-280min,反应搅拌速度为100rpm-600rpm,固液比为5-20。经过反应所制备的纳米木质素的得率为40-60%,粒径为30-130nm,纯度为80-92%,分子量为1000-1800g/mol,多分散性为1.3-1.9。对制备过程的所有变量进行汇总生成总数据集,对数据集进行主成分分析(PCA)和偏最小二乘法分析(PLS),经过分析,得出制备纳米木质素的关键变量,按照重要程度,前三依次为反应温度、低共熔溶剂的酸度、固液比。
以上所述仅为本发明的较佳实施举例,并不用于限制本发明,凡在本发明精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
最后应该说明的是,以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述实施例所记载的技术方案进行修改,或者对其中部分进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。上述虽然对本发明的具体实施方式进行了描述,但并非对本发明保护范围的限制,所属领域技术人员应该明白,在本发明的技术方案的基础上,本领域技术人员不需要付出创造性劳动即可做出的各种修改或变形仍在本发明的保护范围以内。
Claims (9)
1.一种纳米木质素制备过程关键变量的分析方法,其特征在于,基于大数据处理中的多变量分析进行研究,具体包括如下:收集制备纳米木质素的原料的各项物化性质参数;收集纳米木质素制备过程所用溶剂的各项物化性质参数;收集纳米木质素制备反应条件的各项参数;收集所制备的纳米木质素各物化性质的参数;进行多变量分析,剖析各变量之间的相互关系,揭示制备机理,找到具有生产指导意义的关键制备变量。
2.如权利要求1所述的方法,其特征在于,所述的溶剂包括但不限于低共熔溶剂、离子液体、酸、碱等。
3.如权利要求1所述的方法,其特征在于,所述的制备纳米木质素原料为木质纤维素类生物质原料。
4.如权利要求1所述的方法,其特征在于,所述的多变量分析包括但不限于主成分分析和偏最小二乘法分析等分析方法。
5.如权利要求1所述的方法,其特征在于,所述的具有生产指导意义的关键制备变量是指对制备纳米木质素具有重要意义的变量,调节该变量将对制备的纳米木质素产品产生重大影响。
6.如权利要求1所述的方法,其特征在于,所述的原料的各项物化性质参数包括但不限于生物质原料的成分组成、粒径、硬度、含水率等参数。
7.如权利要求1所述的方法,其特征在于,所述的制备反应条件参数包括但不限于反应助剂的用量、固液比、温度、压力、搅拌情况、反应剧烈程度等参数。
8.如权利要求1所述的方法,其特征在于,所述的制备的纳米木质素各物化性质的参数包括但不限于木质素得率、粒径、纯度、分子量、基团含量、分散性等参数。
9.如权利要求1所述的方法,其特征在于,所述的纳米木质素产品是指在三维里的任何一维度上尺寸大小在100纳米之内的木质素。
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CN110546478A (zh) * | 2017-02-24 | 2019-12-06 | 卡内基梅隆大学 | 利用复杂数据处理来设计材料的配方 |
CN111576071A (zh) * | 2020-05-19 | 2020-08-25 | 青岛科技大学 | 一种木质纤维低共熔溶剂预处理机理的分析方法 |
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US20180113101A1 (en) * | 2016-10-25 | 2018-04-26 | Regeneron Pharmaceuticals, Inc. | Methods and systems for chromatography data analysis |
CN110546478A (zh) * | 2017-02-24 | 2019-12-06 | 卡内基梅隆大学 | 利用复杂数据处理来设计材料的配方 |
CN111576071A (zh) * | 2020-05-19 | 2020-08-25 | 青岛科技大学 | 一种木质纤维低共熔溶剂预处理机理的分析方法 |
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