{"title":"Nanoestructuras de sílice, con diámetro y distribución de mesoporos variable, modificadas con ácido tungstofosfórico como catalizadores en la síntesis de quinoxalinas","authors":"A. Sosa, G. Romanelli, L. R. Pizzio","doi":"10.15446/rev.colomb.quim.v49n2.84249","DOIUrl":null,"url":null,"abstract":"Tungstophosphoric acid supported on silica nanostructures (SNX#WPA) with variable diameter and mesopore size distribution were synthetized. Silica nanostructures (SNX) were prepared in octane/aqueous media using polystyrene and CTAB as organic templates. The materials were characterized by XRD, SEM, TEM and dinitrogen adsorption/desorption isotherm analysis. The octane/water ratio influenced the morphology and size of SNX prepared, as well as its pore size distribution. The SNX samples obtained using OCT/H 2 O ratios in the range 0.07-0.35 (SN4, SN5, and SN6 samples). present small (5-6 nm) and large (28-34 nm) mesopores (mainly generated by polystyrene). Large mesopores and their volume contribution were clearly higher than in the SN1, SN2, and SN3 samples. The structure and morphology of SNX#WPA samples were similar to those of the SNX. Furthermore, the characterization of all the SNX#WPA materials by FT-IR and 31 P NMR indicated the presence of undegraded [PW 12 O 40 ] 3− and [H 3-X PW 12 O 40 ] (3-X)− species. According to the potentiometric titration results, the solids presented very strong acid sites. The performance of SNX#WPA materials as catalysts in the synthesis of quinoxalines was evaluated. The yields achieved were high, without formation of by-products resulting from competitive reactions or decomposition products, so the prepared materials are highly selective and reusable catalysts.","PeriodicalId":0,"journal":{"name":"","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2020-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.15446/rev.colomb.quim.v49n2.84249","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.15446/rev.colomb.quim.v49n2.84249","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 0
摘要
合成了具有可变直径和孔径分布的二氧化硅负载的钨磷酸纳米结构(snx# WPA)。以聚苯乙烯和CTAB为有机模板,在辛烷/水介质中制备了二氧化硅纳米结构(SNX)。采用XRD、SEM、TEM和二氮吸附/脱附等温线对材料进行了表征。辛烷/水比对制备的SNX的形貌、尺寸以及孔径分布都有影响。使用OCT/ h2o比值在0.07-0.35范围内获得的SNX样品(SN4, SN5和SN6样品)。存在小孔(5-6 nm)和大孔(28-34 nm)(主要由聚苯乙烯产生)。大介孔及其体积贡献明显高于SN1、SN2和SN3样品。snx# WPA样品的结构和形态与SNX相似。此外,所有SNX#WPA材料的FT-IR和31p NMR表征表明存在未降解的[PW 12 O 40] 3-和[H 3- x PW 12 O 40] (3- x) -物质。根据电位滴定结果,固体呈现很强的酸位。对SNX#WPA材料作为催化剂合成喹诺啉的性能进行了评价。产率高,没有竞争性反应或分解产物产生副产物,因此制备的材料是高选择性和可重复使用的催化剂。
Nanoestructuras de sílice, con diámetro y distribución de mesoporos variable, modificadas con ácido tungstofosfórico como catalizadores en la síntesis de quinoxalinas
Tungstophosphoric acid supported on silica nanostructures (SNX#WPA) with variable diameter and mesopore size distribution were synthetized. Silica nanostructures (SNX) were prepared in octane/aqueous media using polystyrene and CTAB as organic templates. The materials were characterized by XRD, SEM, TEM and dinitrogen adsorption/desorption isotherm analysis. The octane/water ratio influenced the morphology and size of SNX prepared, as well as its pore size distribution. The SNX samples obtained using OCT/H 2 O ratios in the range 0.07-0.35 (SN4, SN5, and SN6 samples). present small (5-6 nm) and large (28-34 nm) mesopores (mainly generated by polystyrene). Large mesopores and their volume contribution were clearly higher than in the SN1, SN2, and SN3 samples. The structure and morphology of SNX#WPA samples were similar to those of the SNX. Furthermore, the characterization of all the SNX#WPA materials by FT-IR and 31 P NMR indicated the presence of undegraded [PW 12 O 40 ] 3− and [H 3-X PW 12 O 40 ] (3-X)− species. According to the potentiometric titration results, the solids presented very strong acid sites. The performance of SNX#WPA materials as catalysts in the synthesis of quinoxalines was evaluated. The yields achieved were high, without formation of by-products resulting from competitive reactions or decomposition products, so the prepared materials are highly selective and reusable catalysts.