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Studies On Preparation And Catalytic Performance Of Chaff Carbon Sulfonic Acid

Posted on:2013-11-20Degree:MasterType:Thesis
Country:ChinaCandidate:X H QuFull Text:PDF
GTID:2321330518988683Subject:Organic Chemistry
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Chemical industry is constantly looking for high activity,high stability and pollution-free solid acid catalyst to improve the environmental security of chemicals production and gradually realize"green" chemical production process.the application of solid acid instead of liquid acid catalyzed organic reactions is one of the most important ways to realize the environment friendly.solid carbon sulfonic acid as a novel catalysts have many advantages such as stable,insoluble in water and organic solvent,be reusable and pollution-free.Comply with the direction of the development of Green chemistry.In this paper,we focused on the development of a novel solid sulfonic materials in catalytic field.Chaff as raw material,through decompression carbonizing-sulfonating and sulfuric acid catalytic charring-sulfonating methods to obtain the chaff char sulfonic acid.Chaff char sulfonic acid through acid-base titration and infrared quantitative analysis methods to determine the amount of acid.Under the optimized conditions the amount of acid of the chaff char sulfonic acid is between 0.8 and 1.2 mmol g-1.The chaff char and the prepared chaff char sulfonic acid were characterized by FT-IR,TG,XRD and N2 adsorption-desorption.The results showed that the obtained char materials have polycyclic aromatic rings with a number of oxygen-groups and the prepared chaff char sulfonic acid showed an obvious C-S absorption peak in FT-IR spectrum.chaff char sulfonic acid belongs to no finalize the design macroporous materials.At the same time,this catalyst has good thermal stability of which sulfonic acid groups can remain stable at 200?.The catalytic application of chaff char sulfonic acid was investigated in conversion of cyclohexene and selectivity of cyclohexyl acetate reaetions and Biginelli reaetions.Effects of reaction time,catalyst amount,material ratio were investigated in catalyzing the esterification of acetic acid and cyclohexene;The catalytic effciency of the novel solid acid was examined by comparing the catalytic effect of the reaction with sulfuric acid,sulfonated resins,p-toluenesulfonic acid,sulfamic acid and so on.At the same time with different raw materials prepared biomass solid carbon sulfonic acid as the catalyst were used in catalyzing the esterification of acetic acid and cyclohexene.Chaff char sulfonic acid showed the same catalytic activity as solid sulfonic acid resin catalyst.The three-component Biginelli reaction of benzaldehyde methylacetoacetate and urea was examined.Separately inspected catalytic activity of catalyst in Biginelli reaction under ultrasound promote and backflow conditions.The results show that under backflow conditions conversion of benzaldehyde can be reached 86.3%.Chaff char sulfonic acid which was reused for 4 times also owned catalytic aetivity in Biginelli reaction under backflow condition.Conversion of benzaldehyde can be reached 83.8%under ultrasound promote condition.Chaff char sulfonic acid has good catalytic performance under the two conversions.Used the novel solid acid,the 3,4-Dihydropyrimidin-2(1H)-ones and thione analogs derivatives were synthesized in moderate condition and resulted to high yield.
Keywords/Search Tags:chaff, biomass char sulfonic acid, solid acid catalys, cyclohexyl acetate, Biginelli reaction
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