Method for preparing gallic acid by sulfuric acid hydrolysis
A technology for hydrolysis of gallic acid and sulfuric acid, which is applied in the preparation of carboxylate/lactone, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems such as the inability to meet the demand of gallic acid, Achieve the effect of reducing decolorization treatment time, improving yield, and avoiding excessive hydrolysis
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Embodiment 1
[0021] Grind 1kg gallnut, add it to a high-pressure reactor, add 2.5L of water, heat up to boiling, and add a compound mixture of sulfuric acid with a mass concentration of 1% and tartaric acid with a mass concentration of 3%, and mix and add it according to the ratio of 1kg of sulfuric acid and 3kg of tartaric acid , the addition amount of the mixture is 2% of the water quality, stirring while adding, after the addition is completed, seal the reaction kettle, control the temperature at 100 ° C, react for 2 hours, and heat filter to obtain the filtrate and filter residue; the filtrate is cooled and crystallized, filtered, The solid and liquid are obtained, the liquid is returned and mixed with water and added to the reactor, the solid is dissolved in hot water, decolorized by activated carbon adsorption, filtered, crystallized, and dried under a vacuum of 0.02 MPa.
[0022] The crude product yield of gallic acid is 59.6%, the crude product yield of gallic acid by the simple sul...
Embodiment 2
[0024] Grind 1kg gallnut, add it to a high-pressure reactor, add 3.5L of water, heat up to boiling, and add a compound mixture of sulfuric acid with a mass concentration of 20% and tartaric acid with a mass concentration of 3%, and mix and add it according to the ratio of 1kg of sulfuric acid and 7kg of tartaric acid , the addition of the mixture is 4% of the water quality, stirring while adding, after the addition is completed, seal the reactor, control the temperature at 130 ° C, react for 4 hours, and heat filter to obtain the filtrate and filter residue; the filtrate is cooled and crystallized, filtered, Obtain solid and liquid, return the liquid and mix it with water and add it to the reaction kettle. After the solid is dissolved in hot water, it is decolorized by activated carbon adsorption, filtered, crystallized, and dried under a vacuum of 0.08 MPa.
[0025] The crude product yield of gallic acid is 58.3%, the crude product yield of gallic acid by the simple sulfuric a...
Embodiment 3
[0027] Grind 1kg of tara, add it to a high-pressure reaction kettle, add 3L of water, heat up to boiling, and add a compound mixture of sulfuric acid with a mass concentration of 10% and tartaric acid with a mass concentration of 3%, and mix and add it according to the ratio of 1kg of sulfuric acid and 5kg of tartaric acid , the addition of the mixture is 3% of the water quality, stirring while adding, after the addition is completed, seal the reactor, control the temperature at 110 ° C, react for 3 hours, and heat filter to obtain the filtrate and filter residue; the filtrate is cooled and crystallized, filtered, The solid and liquid are obtained, the liquid is returned and mixed with water and added to the reactor, the solid is dissolved in hot water, decolorized by activated carbon adsorption, filtered, crystallized, and dried under a vacuum of 0.06 MPa.
[0028] The crude product yield of gallic acid is 58.7%, the crude product yield of gallic acid by the simple sulfuric ac...
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