Hydrolysis of Cellulose in a Small Amount of Concentrated Sulfuric Acid

1960 ◽  
Vol 24 (5) ◽  
pp. 443-449 ◽  
Author(s):  
Tatsuyoshi Kobayashi ◽  
Yoshio Sakai ◽  
Kazuaki Iizuka
2021 ◽  
Author(s):  
Bo Deng ◽  
Ya-xiong Wang ◽  
Li Huo ◽  
Ying Wang ◽  
Li’e Jin

Abstract In this paper, tannic acid, a polyphenolic substance rich in plants, is modified by the glutamic acid and cross-linked with formaldehyde to prepare a high acid density tannin-glutamate acid resin-based imitation enzyme solid acid catalyst (T-Glu-R), which is completely different from traditionally carbon-based solid acid synthesized by concentrated sulfuric acid and carbonized matter. The solid acid catalyst was characterized by Fourier transform infrared spectroscopy, scanning electron microscope, thermogravimetry, and X-ray photoelectron spectroscopy. The catalytic activity and cycle performance of T-Glu-R in the cellulose hydrolysis reaction were evaluated. The results show that the acid density of T-Glu-R reached 7.28 mmol/g, which is much higher than that of the highest acid density of carbon-based solid acid. Microcrystalline cellulose was hydrolyzed in distilled water at 180 °C for 2 h, the yield of total reducing sugars reached 72.15%. After four cycles of hydrolysis, the yield was only reduced by 4.32%, showing excellent cycle performance and stability. The study provides a new strategy with the synthesis of solid acid catalyst for hydrolysis of cellulose converted into platform compounds without concentrated sulfuric acid.


Author(s):  
И.А. Щурова ◽  
Н.А. Алексеева ◽  
С.В. Сысолятин ◽  
В.В. Малыхин

Статья посвящена усовершенствованию способа получения 2,4,6-тригидрокситолуола, востребованного химического реагента в синтезе азокрасителей и пигментов, а также химико-фармацевтических препаратов и различных полимеров. Основным сырьем для его получения является 2,4,6-тринитротолуол, который подвергают каталитическому гидрированию с последующим гидролизом образовавшегося 2,4,6-триаминотолуола. В данной работе предложены условия многоциклового использования палладиевого катализатора гидрирования 2,4,6-тринитротолуола, позволяющие сохранять активность катализатора и повысить выход 2,4,6-триаминотолуола выше 98 %. Аминопроизводное выделяется в виде дисульфата действием концентрированной серной кислоты. Кроме того, изучено влияние соотношения вода/дисульфат 2,4,6-триаминотолуола на выход 2,4,6-тригидрокситолуола; найдены условия, в которых выход на стадии гидролиза увеличен до 83-84 %. Проведен сравнительный анализ различных способов выделения 2,4,6-тригидрокситолуола из реакционной массы. The paper is concerned with upgrading the synthetic method for 2,4,6-trihydroxytoluene, an in-demand chemical reactant in the synthesis of azo-dyes and pigments, as well as chemical pharmaceuticals and various polymers. The basic feedstock for the synthesis thereof is 2,4,6-trinitrotoluene, which is subjected to catalytic hydrogenation followed by hydrolysis of the resulting 2,4,6-triaminotoluene. Here we suggest conditions for the multicycle use of Pd catalyst employed for the hydrogenation of 2,4,6-trinitrotoluene, which allow the catalyst activity to be retained and the yield of 2,4,6-triaminotoluene to be enhanced above 98%. The amino derivative is liberated as the disulfate by concentrated sulfuric acid. Moreover, we examined how the ratio of water / 2,4,6-triaminotoluene disulfate influences the yield of 2,4,6-trihydroxytoluene. Conditions were found in which the yield from hydrolysis is 83-84 %. Different methods for the isolation of 2,4,6-trihydroxytoluene from the reaction mixture were comparatively analyzed.


2019 ◽  
Vol 9 (3) ◽  
pp. 609-616 ◽  
Author(s):  
Yongjun Xu ◽  
Guiheng Liu ◽  
Jinxia Fu ◽  
Shimin Kang ◽  
Yukui Xiao ◽  
...  

1989 ◽  
Vol 185 (2) ◽  
pp. 249-260 ◽  
Author(s):  
Richard F. Helm ◽  
Raymond A. Young ◽  
Anthony H. Conner

1987 ◽  
Vol 40 (10) ◽  
pp. 1675 ◽  
Author(s):  
NR Browne ◽  
RFC Brown ◽  
FW Eastwood ◽  
GD Fallon

The title diester , Ph2C=C=C=C( COOEt )2 (2), has been prepared by a Wittig reaction between (2-bromo-3,3-diphenylprop-2-en-1-yl) triphenylphosphonium bromide and diethyl 2-oxopropane-1,3-dioate ( mesoxalic ester). The diester (2) undergoes cyclization reactions in concentrated sulfuric acid to give diethyl 2-(3'-phenyl-1H-inden-1'-y1idene)propane-l,3-dioate (4) and triethyl 3-oxo-3',9-diphenyl-2,3-dihydrospiro[lH-fluorene-1,l'-[1H]indene]-2,2,4-tricarboxylate (6), the structure of which was determined by X-ray crystallography. The title diester (2)adds cyclopentadiene across the 2,3-C=C bond to give diethyl 3-(2',2'-diphenylethenylidene)bicyclo[2.2.l]hept-5-ene-2,2-dicarboxylate (10). Alkaline hydrolysis of diester (10) gives an unstable colourless acid and a stable yellow crypto acid shown by X-ray crystallography to be 3-(2',2'-diphenylethenyl)bicyclo[2.2.l]hepta-2,5-diene-2-carboxylic acid (12). Attempts to convert diesters (2) and acid (12) into derivatives suitable for pyrolytic generation of Ph2C=C=C=C=C=O failed; The mono-acid chloride (14) yielded a small phenylazulene fraction on pyrolysis at 780-800°/0.02 mm.


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