A novel solid acid catalyst synthesized from ZnAl2O4 spinel and its application in the esterification of acetic acid and n-butyl alcohol

RSC Advances ◽  
2015 ◽  
Vol 5 (25) ◽  
pp. 19652-19658 ◽  
Author(s):  
An-Qi Wang ◽  
Xiu-Ling Wu ◽  
Jun-Xia Wang ◽  
Hui Pan ◽  
Xiao-Yun Tian ◽  
...  

A new spinel-style S2O82−/ZnAl2O4 catalyst with the mesoporous structure exhibited the well catalytic activity and structural stability.

2019 ◽  
Vol 7 (1) ◽  
pp. 55-80 ◽  
Author(s):  
Fatemeh Ghorbani ◽  
Seied Ali Pourmousavi ◽  
Hamzeh Kiyani

Background: Much attention has been focused on heterogeneous catalysts. Reactions with these recoverable and reusable catalysts are clean, selective with high efficiency. Among the heterogeneous solid acid catalyst in organic synthesis, Carbon-Based Solid Acids (CBSAs), which are important solid acid with many practical and research applications have been extensively studied. In this work, green Pistachio peel, a biomass waste, was converted into a novel carbon-based solid acid catalyst (Pis-SO3H). Objective: The aim of this work is to synthesize highly sulfonated carbon as an efficient, recyclable, nontoxic solid acid catalyst by simultaneous sulfonation, dehydration and carbonization of green Pistachio peel as biomass and investigate the catalytic activity of Pis-SO3H in acetalization, thioacetalization, acylation of aldehydes and synthesis of 3,3'-Arylmethylene-bis(4-hydroxycoumarin) derivatives. Method: Pis-SO3H was synthesized by an integrated fast one-step hydrothermal carbonization and sulfonation process in the presence of sulfuric acid. The characterization of the physicochemical properties of Pis-SO3H was achieved by XRD, FT-IR, FE-SEM, and elemental analysis. Results: The result of acid-base titration showed that the total acidity of the catalyst was 7.75 mmol H+g−1. This new heterogeneous catalyst has been efficiently used for the chemoselective thioacetalization, acetalization and acylation of aldehyde and the synthesis of biscoumarins under solvent-free conditions. All the reactions work easily in high yields. The antimicrobial activity of some of the biscoumarins was evaluated in screening by disk diffusion assay for the zone of inhibition. Conclusion: The catalytic activity of the Pis-SO3H was investigated during acetalization, thioacetalization, acylation and synthesis of biscoumarins. The results of protection of carbonyl groups and synthesis of biscoumarins in the present work offer effective alternatives for environmentally friendly utilization of abundant biomass waste.


2011 ◽  
Vol 383-390 ◽  
pp. 1144-1149 ◽  
Author(s):  
Yue Ling Gu ◽  
Guo Hui Xu ◽  
Zuo Gang Guo ◽  
Shu Rong Wang

Solid acid catalyst has high catalytic esterification activity but with a free acid excess problem. In this paper, washing pretreatments were adopted in the catalyst preparation processes and their influences on catalytic activity and residual free acid amount were investigated. Residual free acid amount can be reduced by 33% with both washing before calcinations and washing after calcinations pretreatments. But their influences on catalyst activities were different. Washing before calcinations pretreatment reduced the catalytic activity from 80.29% to 57.72% while the other washing pretreatment had little influence on the catalyst activity. In order to describe the influence mechanism of washing pretreatments, catalysts were characterized by FT-IR and XRD. Finally, typical compounds in bio-oil were selected to form a bio-oil model compounds system. The catalyst pretreated by washing after calcinations was used on the esterification research of this bio-oil model system. The volume ratio of propanol to bio-oil model compound was 3:1. The reaction temperature was 90 °C and the amount of catalyst was 2wt% of total liquid mass. Combined with the GC-MS qualitative and quantitative results, carboxylic acids, such as formic acid, acetic acid, propionic acid were converted to esters effectively.


2015 ◽  
Vol 41 (9) ◽  
pp. 12186-12191 ◽  
Author(s):  
Qiang Zhao ◽  
Shuangming Meng ◽  
Junli Wang ◽  
Yongsheng Qiao ◽  
Zuopeng Li ◽  
...  

2010 ◽  
Vol 96 ◽  
pp. 183-187 ◽  
Author(s):  
Pan Wang ◽  
Si Hui Zhan ◽  
Hong Bing Yu

Using solid acid catalyst for the levulinic acid (LA) production from cellulose is one of the promising methods for utilization of biomass. An environmentally friendly solid acid catalyst, sulfated TiO2 was prepared by precipitation-impregnation method and used to catalyze the production of levulinic acid from cellulose. The concentration of sulphuric acid had a remarkable influence on the construction and catalytic activity of sulfated TiO2. The influence of reaction temperature and catalyst dosage on levulinic acid yield was also investigated with the aim to obtain the highest yield of LA. The optimum condition for the highest yield of levulinic acid (27.2%) was achieved at 240 °C, 0.7g of sulfated TiO2 and reaction time of 15 min. The recycling test indicated that the catalytic activity of the catalyst had a slight decrease after being used two times.


2020 ◽  
Author(s):  
Iryanti F. Nata ◽  
Chairul Irawan ◽  
Meilana D. Putra ◽  
Cheng-Kang Lee

Abstract The sulfonated carbon solid acid catalyst (C-SO3H) was successfully generated from palm empty fruit bunch (PEFB) carbon via hydrothermal sulfonation by addition of hydroxyethylsulfonic acid and citric acid. The C-SO3H was identified contain of 1.75 mmol/g of acidity and 40.2% of sulphur. The surface morphology of C-SO3H showed pores with diameters of 3-6 µm and crystalline index (CrI) of material was decreased to 63.8% due to changed structure become carbon. The surface area of carbon was increased significantly from 11.5 to 239.65 m2 g- 1 after hydrothermal treatment. The identification of functional groups of -SO3H, COOH and -OH were detected by Fourier Transform Infra-Red (FT-IR). The optimum catalytic activity of C-SO3H was achieved via hydrolysis reaction with 60.4% of total reducing sugar (TRS) yield. The both concentrations of C-SO3H and cassava peel starch are 5% (w v- 1) at 100 oC for 1 h. Stability of C-SO3H showed good performance for 4th repeated used; it showed insignificant of activity that decreased only of 6%. Thus, the C-SO3H is a candidate for green and potential sulfonated solid acid catalyst for wide range applications.


2021 ◽  
Vol 17 (1) ◽  
pp. 13-21
Author(s):  
Shofiyya Julaika ◽  
Agus Farid Fadli ◽  
Widiyastuti Widiyastuti ◽  
Heru Setyawan

Solid acid catalyst is a promising alternative to the counterpart homogeneous acid for esterification reaction from the viewpoint of reusability and environmental concerns. This work aims to develop sulfonated mesoporous silica-carbon composite as solid acid catalyst for the esterification. The catalyst was synthesized from sodium silicate as the silica precursor and polyethylene glycol (PEG) as both carbon precursor and template via a sol-gel route in an aqueous system. Then, it was carbonized to produce mesoporous silica-carbon composite. Using the proposed method, the surface area of the silica-carbon composite could reach as high as 1074.21 m2/g. Although the surface area decreased to 614.02 m²/g when it was functionalized with sulfonate groups, the composite had a high ionic capacity of 5.3 mEq/g and exhibited high catalytic activity for esterification reaction of acetic acid with ethanol. At a reaction temperature of 80 °C, the acetic acid conversion reached 76.55% in 4 h. In addition, the catalyst had good reusability, which can be comparable with the commercial catalyst Foltrol F-007. It appears that the sulfonated silica-carbon composite prepared from sodium silicate using PEG as the carbon source a promising candidate as catalyst for esterification and the related area. Copyright © 2021 by Authors, Published by BCREC Group. This is an open access article under the CC BY-SA License (https://creativecommons.org/licenses/by-sa/4.0). 


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