Method for preparing 2,5-dihydroxy p-benzene dicarboxylic acid
A technology of hydroxyterephthalic acid and hydroquinone, which is applied in the field of catalytic preparation 2, can solve the problems of unseen and high solvent toxicity, and achieve the effect of high yield and high purity
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example 1
[0018] In a 0.5L autoclave with heating, stirring and temperature control system, add 13.75g hydroquinone, 35g potassium hydroxide, 150ml n-octane and 5% Pd(II) / C catalyst. Introduce carbon dioxide gas, raise the temperature to 200°C, make the pressure of the kettle reach 9.5MPa, and react for 4 hours. Cool the reacted mixture, suction filter, recover the filtrate, dissolve the filter cake in 500ml of 0.1% sodium bisulfite aqueous solution, heat and boil to remove the residual solvent, and suction filter while the mixture is fully dissolved Remove a little impurity and catalyst, cool the filtrate in an ice-water bath to below 8°C to crystallize, and wash the filter cake with a small amount of ice water. After the obtained filter cake was dissolved in 300ml of hot water, concentrated hydrochloric acid was added to adjust the pH to less than 2, and after stirring, it was allowed to stand for 1 hour, then suction filtered, the filter cake was washed, and the filter cake was vacu...
example 2
[0020] In a 0.5L autoclave with heating, stirring and temperature control system, add 13.75g hydroquinone, 35g potassium hydroxide, 150ml n-octane and 5% Pd(II) / C catalyst. Introduce carbon dioxide gas, raise the temperature to 200°C, make the pressure of the kettle reach 11.5MPa, and react for 4 hours. Cool the reacted mixture, suction filter, recover the filtrate, dissolve the filter cake in 500ml of 0.1% sodium bisulfite aqueous solution, heat and boil to remove the residual solvent, and suction filter while the mixture is fully dissolved Remove a little impurity and catalyst, cool the filtrate in an ice-water bath to below 8°C to crystallize, and wash the filter cake with a small amount of ice water. After the obtained filter cake was dissolved in 300ml of hot water, concentrated hydrochloric acid was added to adjust the pH to less than 2, and after stirring, it was allowed to stand for 1 hour, then suction filtered, the filter cake was washed, and the filter cake was vac...
example 3
[0022] In a 0.5L autoclave with heating, stirring and temperature control system, add 13.75g hydroquinone, 35g potassium hydroxide, 150ml n-octane and 5% Pd(II) / C catalyst. Introduce carbon dioxide gas, raise the temperature to 220°C, make the pressure of the kettle reach 9.5MPa, and react for 4 hours. Cool the reacted mixture, suction filter, recover the filtrate, dissolve the filter cake in 500ml of 0.1% sodium bisulfite aqueous solution, heat and boil to remove the residual solvent, and suction filter while the mixture is fully dissolved Remove a little impurity and catalyst, cool the filtrate in an ice-water bath to below 8°C to crystallize, and wash the filter cake with a small amount of ice water. After the obtained filter cake was dissolved in 300ml of hot water, concentrated hydrochloric acid was added to adjust the pH to less than 2, and after stirring, it was allowed to stand for 1 hour, then suction filtered, the filter cake was washed, and the filter cake was vacu...
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