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Preparation of nanostructured functionalised carbons by phosphoric acid activation method

机译:磷酸活化法制备纳米结构官能化碳

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Functionalised nanostructured carbons were obtained by template method using sucrose as carbon precursor and silica gel SG60 as structure directing agent. To introduce acid groups to carbon a different amount of phosphoric acid was added to sucrose (impregnation ratio 0-1) before filling the pores of silica gel. After carbonisation the template was removed by dissolution in HF. Carbons were characterised by SEM/EDX, nitrogen adsorption at 77 K and acid-base titration. Pore size distributions (PSD) indicated that the porous structure of carbons obtained at impregnation ratio of 0-0.75 is relatively homogeneous with mesopore mean size 3.1 nm and some microporosity. PSD significantly changes at IR= 1 showing additional larger mesopores with mean diameter of 8.2 nm. Acid-base titration showed that carbon obtained by template method without addition of phosphoric acid contains significant amount (1.75 mmol/g) of surface groups. Calculated proton affinity distributions evidence the presence of three types of surface groups that were assigned to carboxylic (pK=3.7), lactone/enol (pK= 7.6) and phenolic (pK= 10.2) groups. Addition of phosphoric acid to carbon precursor has led to 2.3-2.5 fold increase in the total amount of surface groups (up to 4.1-4.4 mmol/g). Proton affinity distribution indicates disappearance of carboxyl and lactone/enol groups and appearance of two new groups with pK= 2.2-2.4 and 6.6-6.9, which were assigned to the first and second dissociation constants of phosphate groups. It could be concluded that the functionalised nanostructured carbons can be obtained by combination of template synthesis with phosphoric acid activation.
机译:以蔗糖为碳前驱体,以硅胶SG60为结构导向剂,通过模板法获得了功能化的纳米结构碳。为了将酸基团引入碳中,在填充硅胶孔之前,向蔗糖中添加不同量的磷酸(浸渍比0-1)。碳化后,通过溶于HF除去模板。通过SEM / EDX,77 K下的氮吸附和酸碱滴定法表征碳。孔尺寸分布(PSD)表明,以0-0.75的浸渍比获得的碳的多孔结构相对均匀,中孔平均尺寸为3.1nm,并且具有一些微孔性。 PSD在IR = 1时发生显着变化,显示出其他更大的中孔,平均直径为8.2 nm。酸碱滴定表明,通过不添加磷酸的模板法获得的碳含有大量(1.75 mmol / g)的表面基团。计算出的质子亲和力分布证明存在三种类型的表面基团,分别分配为羧基(pK = 3.7),内酯/烯醇(pK = 7.6)和酚基(pK = 10.2)。向碳前体中添加磷酸已导致表面基团总量增加2.3-2.5倍(最高4.1-4.4 mmol / g)。质子亲和力分布表明羧基和内酯/烯醇基团的消失以及两个新的pK = 2.2-2.4和6.6-6.9的新基团的出现,这两个新基团被分配为磷酸酯基团的第一和第二解离常数。可以得出结论,可以通过模板合成与磷酸活化相结合获得官能化的纳米结构碳。

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