CN105531224A - 多孔碳、调湿吸附材料、吸附式热泵和燃料电池 - Google Patents
多孔碳、调湿吸附材料、吸附式热泵和燃料电池 Download PDFInfo
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Abstract
本发明的目的在于提供一种能够在高湿度侧充分吸附水蒸气的多孔碳。该多孔碳的特征在于:具备中孔和微孔,下述(1)式所示的水蒸气吸附量比率为1.8以上,特别优选下述(1)式所示的水蒸气吸附量比率为2.0以上。或者,优选相对湿度为70%时的水蒸气吸附量为50mg/g以上。水蒸气吸附量比率=相对湿度为90%时的水蒸气吸附量/相对湿度为70%时的水蒸气吸附量…(1)。
Description
技术领域
本发明涉及多孔碳等,特别涉及能够在高湿度侧充分吸附水蒸气的多孔碳等。
背景技术
在以汽车用吸附式冷冻机为代表的热泵等中,要求溶剂的吸附量大、吸附脱附速度快、对施加压力的响应性高。另外,由于暴露于高温,因此也要求一定的化学稳定性。然而,如下述非专利文献1~3所示,作为一般吸附材料进行评价的活性碳、硅胶等中,没有充分满足现状所需要的吸附性能(吸附量、吸附脱附速度)的材料。特别是没有能够在高湿度侧充分吸附水蒸气的材料。
另外,提出了一种调湿材料用碳材料,其特征在于:通过将石油焦炭在650~800℃进行干馏而得到,在20容量%以上、30容量%以下的范围具有气孔(下述专利文献1)。
现有技术文献
专利文献
专利文献1:日本特开2007-209844号公报
非专利文献
非专利文献1:DensoTechnicalReview(デンソーテクニカルレビュー),Vol.11No.12006
非专利文献2:AdsorptionNewsVol.10,NO.3,p12-16(July1996)(日本吸附学会)
非专利文献3:化学工学论文集15(1),p38-43
发明内容
发明所要解决的课题
然而,在使用上述专利文献1所示的调湿材料用碳材料时,也存在无法在高湿度侧充分吸附水蒸气这样的课题。
因此,本发明的目的在于提供一种能够在高湿度侧充分吸附水蒸气的多孔碳等。
用于解决课题的方法
用于实现上述目的的本发明的多孔碳的特征在于:具备中孔和微孔,下述(1)式所示的水蒸气吸附量比率为1.8以上。
水蒸气吸附量比率=相对湿度为90%时的水蒸气吸附量/相对湿度为70%时的水蒸气吸附量…(1)
发明的效果
根据本发明,发挥了能够提供能够在高湿度侧充分吸附水蒸气的多孔碳等这样的优异效果。
附图说明
图1是表示本发明的制造工序的图,该图(a)是表示混合有聚酰胺酸树脂和氧化镁的状态的说明图,该图(b)是表示对混合物进行了热处理的状态的说明图,该图(c)是表示多孔碳的说明图。
图2是表示碳A1~A3、Z1~Z5中的相对湿度与水蒸气吸附量的关系的曲线图。
具体实施方式
为了实现上述目的,本发明的多孔碳的特征在于:具备中孔和微孔,下述(1)式所示的水蒸气吸附量比率为1.8以上。
水蒸气吸附量比率=相对湿度为90%时的水蒸气吸附量/相对湿度为70%时的水蒸气吸附量…(1)
上述水蒸气吸附量比率低于1.8时,在相对湿度为70%时,成为几乎没有多孔碳的水蒸气吸附余力的状态(具体而言,多孔碳的细孔中基本充满水的状态)。因此,相对湿度超过70%时,几乎无法吸附其以上的水蒸气,难以控制水蒸气吸附量。相对于此,在上述水蒸气吸附量比率为1.8以上时,在相对湿度为70%时,成为多孔碳的水蒸气吸附余力充分的状态(具体而言,多孔碳的细孔中没有充满水的状态)。因此,在相对湿度超过70%时,也能够吸附其以上的水蒸气,能够充分进行水蒸气吸附量的控制。
期望上述水蒸气吸附量比率为2.0以上。
水蒸气吸附量比率为2.0以上时,能够在高湿度气氛下进一步吸附水蒸气,因此,能够更加发挥作为吸附材料的功能。
期望上述相对湿度为70%时的水蒸气吸附量为50mg/g以上。
相对湿度为70%时的水蒸气吸附量低于50mg/g时,能够吸附的水蒸气量变少。因此,有时无法充分发挥作为吸附材料的功能,能够利用的领域受到限制。
期望上述相对湿度为90%时的水蒸气吸附量为300mg/g以上700mg/g以下。
相对湿度为90%时的水蒸气吸附量低于300mg/g时,有时作为吸附材料的功能低,能够利用的领域受到限制。另一方面,相对湿度为90%时的水蒸气吸附量超过700mg/g时,成为主要发生吸附现象的微孔几乎全部被水蒸气占满的状态,因此,有时难以控制吸附动作。
另外,如上所述,主要发生水蒸气的吸附现象的是微孔,但是高湿度侧的水蒸气的吸附量受到中孔容量影响。
期望上述中孔的孔径为3nm以上50nm以下,上述中孔的容量为0.9ml/g以上2.0ml/g以下,特别期望上述中孔的孔径为4.5nm以上50nm以下。
将上述中孔的孔径规定为3nm以上(特别是4.5nm以上)是由于制作孔径更小的中孔有时候是困难的。另外,将中孔的容量规定为0.9ml/g以上2.0ml/g以下是由于以下所示的理由。中孔的容量低于0.9ml/g时,有时比表面积小,在高湿度侧无法充分吸附水蒸气。另一方面,中孔的容量超过2.0ml/g时,总细孔中的微孔的容量(比例)非常小,因此有时难以确保用于吸附水蒸气的充分的比表面积。
另外,总细孔容量、微孔容量、中孔容量的关系如下述(2)式所示。
微孔容量=总细孔容量-中孔容量…(2)
期望上述微孔容量为0.3ml/g以上0.7ml/g以下。
微孔容量低于0.3ml/g时,有时难以确保比表面积,无法充分吸附水蒸气。另一方面,微孔容量超过0.7ml/g时,由于微孔容量对水蒸气向微孔的扩散速度产生影响,有时作为吸附材料的响答速度(吸附速度)降低。
特征在于将上述的多孔碳作为调湿吸附材料的吸附材料使用。另外,特征在于将上述的多孔碳作为吸附式热泵的吸附材料使用。另外,特征在于将上述的多孔碳作为燃料电池用电极的碳系载体使用。
以下,在以下说明具体实施方式。
上述多孔碳例如能够按照以下操作进行制造。首先,关于本发明的多孔碳,将含有有机质树脂的流动性材料和氧化物(模板颗粒)以溶液或者粉末状态进行湿式或者干式混合,制作混合物。接着,将该混合物在非氧化气氛或减压气氛下、例如以500℃以上的温度碳化。最后,通过清洗处理除去模板颗粒,由此,能够制作多孔碳。这样操作制作的多孔碳具有大量的细孔(中孔和微孔)。其中,细孔的配置不是规则的,成为随机配置的结构。
这里,通过改变模板颗粒的直径和有机树脂的种类,能够调整细孔径、多孔碳的细孔分布和碳质壁的厚度。因此,通过适当选择模板颗粒的直径和有机质树脂的种类,能够制作具有更大细孔容量的多孔碳。
具体而言,作为上述有机质树脂,优选使用在单位结构中含有至少一个以上的氮或氟原子的聚酰亚胺。该聚酰亚胺能够通过酸成分和二胺成分的缩聚得到。其中,在该情况下,在酸成分和二胺成分的任一方或双方,需要含有一个以上的氮原子或氟原子。
具体而言,将作为聚酰亚胺的前体的聚酰胺酸进行成膜,通过加热除去溶剂,得到聚酰胺酸膜。接着,将所得到的聚酰胺酸膜在200℃以上进行热酰亚胺化,能够制造聚酰亚胺。
作为上述二胺,能够例示2,2-双(4-氨基苯基)六氟丙烷〔2,2-Bis(4-aminophenyl)hexafluoropropane〕、2,2-双(三氟甲基)-联苯胺〔2,2’-Bis(trifluoromethyl)-benzidine〕、4,4’-二氨基八氟联苯、3,3’-二氟-4,4’-二氨基二苯基甲烷,3,3’-二氟-4,4’-二氨基二苯基醚、3,3’-二(三氟甲基)-4,4’-二氨基二苯基醚、3,3’-二氟-4,4’-二氨基二苯基丙烷、3,3’-二氟-4,4’-二氨基二苯基六氟丙烷、3,3’-二氟-4,4’-二氨基苯甲酮、3,3’,5,5’-四氟-4,4’-二氨基二苯基甲烷、3,3’,5,5’-四(三氟甲基)-4,4’-二氨基二苯基甲烷、3,3’,5,5’-四氟-4,4’-二氨基二苯基丙烷、3,3’,5,5’-四(三氟甲基)-4,4’-二氨基二苯基丙烷、3,3’,5,5’-四氟-4,4-二氨基二苯基六氟丙烷、1,3-二氨基-5-(全氟壬烯氧基)苯、1,3-二氨基-4-甲基-5-(全氟壬烯氧基)苯、1,3-二氨基-4-甲氧基-5-(全氟壬烯氧基)苯、1,3-二氨基-2,4,6-三氟-5-(全氟壬烯氧基)苯、1,3-二氨基-4-氯-5-(全氟壬烯氧基)苯、1,3-二氨基-4-溴-5-(全氟壬烯氧基)苯、1,2-二氨基-4-(全氟壬烯氧基)苯、1,2-二氨基-4-甲基-5-(全氟壬烯氧基)苯、1,2-二氨基-4-甲氧基-5-(全氟壬烯氧基)苯、1,2-二氨基-3,4,6-三氟-5-(全氟壬烯氧基)苯、1,2-二氨基-4-氯-5-(全氟壬烯氧基)苯、1,2一二氨基-4-溴-5-(全氟壬烯氧基)苯、1,4-二氨基-3-(全氟壬烯氧基)苯、1,4-二氨基-2-甲基-5-(全氟壬烯氧基)苯、1,4-二氨基-2-甲氧基-5-(全氟壬烯氧基)苯、1,4-二氨基-2,3,6-三氟-5-(全氟壬烯氧基)苯、1,4-二氨基-2-氯-5-(全氟壬烯氧基)苯、1,4-二氨基-2-溴-5-(全氟壬烯氧基)苯、1,3-二氨基-5-(全氟己烯氧基)苯、1,3-二氨基-4-甲基-5-(全氟己烯氧基)苯、1,3-二氨基-4-甲氧基-5-(全氟己烯氧基)苯、1,3-二氨基-2,4,6-三氟-5-(全氟己烯氧基)苯、1,3-二氨基-4-氯-5-(全氟己烯氧基)苯、1,3-二氨基-4-溴-5-(全氟己烯氧基)苯、1,2-二氨基-4-(全氟己烯氧基)苯、1,2-二氨基-4-甲基-5-(全氟己烯氧基)苯、1,2-二氨基-4-甲氧基-5-(全氟己烯氧基)苯、1,2-二氨基-3,4,6-三氟-5-(全氟己烯氧基)苯、1,2-二氨基-4-氯-5-(全氟己烯氧基)苯、1,2-二氨基-4-溴-5-(全氟己烯氧基)苯、1,4-二氨基-3-(全氟己烯氧基)苯、1,4-二氨基-2-甲基-5-(全氟己烯氧基)苯、1,4-二氨基-2-甲氧基-5-(全氟己烯氧基)苯、1,4-二氨基-2,3,6-三氟-5-(全氟己烯氧基)苯、1,4-二氨基-2-氯-5-(全氟己烯氧基)苯、1,4-二氨基-2-溴-5-(全氟己烯氧基)苯、不含氟原子的对苯二胺(PPD)、二氧二苯胺等的芳香族二胺。另外,上述二胺成分也可以组合2种以上的上述各芳香族二胺来使用。
另一方面,作为酸成分,可以列举含有氟原子的4,4-六氟异丙烯二酞酸酐(6FDA)、和不含氟原子的3,4,3’,4’-联苯四羧酸二酐(BPDA)、均苯四甲酸二酐(PMDA)等。
另外,作为聚酰亚胺前体的溶剂使用的有机溶剂,可以列举N-甲基-2-吡咯烷酮、二甲基甲酰胺等。
作为酰亚胺化的方法,可以如公知的方法〔例如,参照高分子学会编《新高分子实验学》共立出版,1996年3月28日,第3卷高分子的合成·反应(2)158页〕所示,采用加热或者化学酰亚胺化的任一种方法,本发明不受该酰亚胺化的方法影响。
另外,作为聚酰亚胺以外的树脂,能够使用石油系焦油沥青、丙烯酸树脂等。
另一方面,作为上述氧化物使用的原料,除了碱土金属氧化物(氧化镁、氧化钙等)以外,也能够使用通过热处理在热分解过程中变化为氧化镁的状态的、金属有机酸(柠檬酸镁、草酸镁、柠檬酸钙、草酸钙等)、氯化物、硝酸盐、硫酸盐。
另外,作为除去氧化物的清洗液,使用盐酸、硫酸、硝酸、柠檬酸、乙酸、甲酸等一般的无机酸,优选作为2mol/l以下的稀酸使用。另外,也能够使用80℃以上的热水。
另外,上述混合物的碳化优选在非氧化气氛或减压气氛下以500℃以上、1500℃以下的温度进行。高碳收率的树脂为高分子,因此,在低于500℃时,有时碳化不充分且细孔的发展不充分。另一方面,在1500℃以上时,由于收缩大、氧化物烧结、粗大化,因此,细孔的尺寸变小,比表面积变小。非氧化性气氛为氩气氛或氮气氛等,减压气氛为133Pa(1torr)以下的气氛。
另外,期望上述多孔碳的体积密度(bulkdensity)为0.1g/cc以上1.0g/cc以下。体积密度低于0.1g/cc时,难以确保比表面积,无法确保碳质壁的形状。另一方面,体积密度超过1.0g/cc时,有时难以形成三维网眼结构,细孔的形成不充分。
实施例
(实施例1)
首先,如图1(a)所示,将作为模板颗粒的氧化镁粉末(MgO、平均粒径为5nm)2和作为碳前体的有机物树脂(聚乙烯醇)1以3:2的重量比混合。接着,如图1(b)所示,将该混合物在不活泼气氛下以900℃进行2小时热处理,使聚乙烯醇热分解,由此,得到具备碳质壁3的烧制物。接着,如图1(c)所示,将所得到的烧制物用以1mol/l的比例添加的硫酸溶液清洗,使MgO完全溶出。由此,得到具有大量细孔4的非晶质的多孔碳5。
将这样操作制得的多孔碳材料在以下称为材料A1。
(实施例2)
作为模板颗粒,使用平均粒径为20nm的氧化镁粉末,除此以外,与上述实施例1同样操作制作多孔碳。
将这样操作制得的多孔碳材料在以下称为材料A2。
(实施例3)
作为模板颗粒使用镁盐(乙酸镁),作为碳前体使用有机物树脂(聚乙烯醇),除此以外,与上述实施例1同样操作制作多孔碳。
将这样操作制得的多孔碳在以下称为材料A3。
(比较例1)
使用市售的活性炭(和光纯药工业株式会社制活性炭(商品编号037-02115))。
将这样的活性炭在以下称为材料Z1。
(比较例2)
将由聚酰亚胺形成的膜在氮气氛下以900℃进行热处理,由此制作碳材料。
将这样操作制得的材料在以下称为材料Z2。
(比较例3)
使用市售的合成沸石系吸附材料(和光纯药工业株式会社制合成沸石A-3(商品编号269-00555)。
将这样的材料在以下称为材料Z3。
(比较例4)
使用市售的合成沸石系吸附材料(和光纯药工业株式会社制合成沸石F-9(制品号261-00635))。
将这样的材料在以下称为材料Z4。
(比较例5)
使用市售的二氧化硅(Sigma-Aldrich公司制MCM-41type643645)。
将这样的材料在以下称为材料Z5。
(实验)
对于上述材料A1~A3、Z1~Z5的BET比表面积等,以下述的方法进行研究,将这些结果示于表1中。
(1)首先,在密闭的吸附测定用玻璃小室内配置材料A1~A3、Z1~Z5之后,在真空下以300℃进行2小时的脱气处理。
(2)使用氮作为吸附气体,在77K(-196℃)进行测定,求出氮吸附等温线。该测定中,使用日本BEL株式会社制的自动气体/蒸气吸附量测定装置BELSORP-18。BET比表面积由相对压(P/P0)=0.05~2.20的范围的测定点算出。
总细孔容量从相对压(P/P0)0.95的吸附量求出,微孔的容量通过Dubinin-Radushkevitch(DR)求出。另外,中孔容量从上述总细孔容量和上述微孔的容量之差求出。
(3)中孔径和微孔径的导出
中孔径由BJH(Berret-Joyner-Halenda)法求出,微孔径由HK(Horvath-Kawazoe)法求出。
(4)水蒸气吸附测定
水蒸气吸附测定使用日本BEL株式会社制的自动气体/蒸气吸附量测定装置BELSORP-18进行。测定条件在使吸附温度为25℃、相对压(P/P0)0~0.9的范围进行。另外,作为吸附质的水,使用通过重复进行4~5次冻结和脱泡处理而高度纯化的蒸馏水。所得到的吸附等温线以横轴为水蒸气相对压(P/P0)、纵轴为每1g试样吸附的水蒸气的量(mg/g)进行描绘。将其结果示于图2。
接着,根据图2,研究25℃时的水蒸气相对压P/P0为0.70(意味着相对湿度为70%。以下,有时称为RH70)时的水蒸气吸附量、P/P0=0.90(意味着相对湿度为90%。以下,有时称为RH90)时的水蒸气吸附量,算出下述(1)式所示的水蒸气吸附量比率。
水蒸气吸附量比率=RH90时的水蒸气吸附量/RH70时的水蒸气吸附量…(1)
从表1和图2可知,关于材料Z1~Z5,RH90时的水蒸气吸附量/RH70时的水蒸气吸附量(以下,有时称为RH90/RH70)的值为1.0~1.7,相对于此,关于材料A1~A3,RH90/RH70的值为2.3~7.8。由此可知,材料A1~A3与材料Z1~Z5相比,RH90/RH70的值变大。因此,材料Z1~Z5在RH70时成为几乎没有多孔碳的水蒸气吸附余力的状态,因此,在RH90时几乎无法吸附水蒸气。相对于此,材料A1~A3在RH70时成为多孔碳的水蒸气吸附余力充分的状态,因此,即使在为RH90时也能够充分吸附水蒸气。
成为这样的结果的理由可以认为是:高湿度时的水蒸气吸附量依赖于中孔容量。即,材料A1~A3的中孔容量为0.834~1.861ml/g,非常大,相对于此,材料Z1~Z5中不存在中孔或者即使存在时其容量为0.024~0.455ml/g,非常小。因此,成为上述的实验结果。
工业上的可利用性
本发明能够作为调湿·吸附材料、吸附式热泵、燃料电池用电极载体等使用。
符号说明
1:聚酰胺酸树脂
2:氧化镁
3:碳质壁
4:细孔
5:多孔碳
Claims (10)
1.一种多孔碳,其特征在于:
具备中孔和微孔,下述(1)式所示的水蒸气吸附量比率为1.8以上,
水蒸气吸附量比率=相对湿度为90%时的水蒸气吸附量/相对湿度为70%时的水蒸气吸附量…(1)。
2.如权利要求1所述的多孔碳,其特征在于:
所述水蒸气吸附量比率为2.0以上。
3.如权利要求1或2所述的多孔碳,其特征在于:
所述相对湿度为70%时的水蒸气吸附量为50mg/g以上。
4.如权利要求1~3中任一项所述的多孔碳,其特征在于:
所述相对湿度为90%时的水蒸气吸附量为300mg/g以上700mg/g以下。
5.如权利要求1~4中任一项所述的多孔碳,其特征在于:
所述中孔的孔径为3nm以上50nm以下,所述中孔的容量为0.9ml/g以上2.0ml/g以下。
6.如权利要求5所述的多孔碳,其特征在于:
所述中孔的孔径为4.5nm以上50nm以下。
7.如权利要求1~6中任一项所述的多孔碳,其特征在于:
所述微孔容量为0.3ml/g以上0.7ml/g以下。
8.一种调湿吸附材料,其特征在于:
将权利要求1~7中任一项所述的多孔碳作为吸附材料使用。
9.一种吸附式热泵,其特征在于:
将权利要求1~7中任一项所述的多孔碳作为吸附材料使用。
10.一种燃料电池,其特征在于:
将权利要求1~7中任一项所述的多孔碳作为电极的碳系载体使用。
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EP4223415A1 (en) | 2020-09-29 | 2023-08-09 | N.E. Chemcat Corporation | Catalyst for electrodes, composition for forming gas diffusion electrode, gas diffusion electrode, membrane electrode assembly, and fuel cell stack |
FR3122585A1 (fr) * | 2021-05-04 | 2022-11-11 | Universite Claude Bernard Lyon 1 | Solide mésoporeux pour réguler l’humidité dans les espaces clos |
WO2024202884A1 (ja) * | 2023-03-31 | 2024-10-03 | 日鉄ケミカル&マテリアル株式会社 | 固体高分子型燃料電池の触媒担体用炭素材料、固体高分子型燃料電池用触媒層、燃料電池、及び固体高分子型燃料電池の触媒担体用炭素材料の製造方法 |
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TWI638771B (zh) | 2018-10-21 |
EP3042877B1 (en) | 2021-02-17 |
JP5695147B2 (ja) | 2015-04-01 |
KR20160051879A (ko) | 2016-05-11 |
TW201515993A (zh) | 2015-05-01 |
JP2015051891A (ja) | 2015-03-19 |
US10137405B2 (en) | 2018-11-27 |
KR102328148B1 (ko) | 2021-11-18 |
US20160199809A1 (en) | 2016-07-14 |
EP3042877A4 (en) | 2017-05-10 |
WO2015033643A1 (ja) | 2015-03-12 |
CN105531224B (zh) | 2018-10-16 |
CA2922942A1 (en) | 2015-03-12 |
EP3042877A1 (en) | 2016-07-13 |
MX2016001521A (es) | 2017-01-11 |
CA2922942C (en) | 2022-09-13 |
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