A method of using PTA residue to prepare mixed benzene acid two -shrimply glycerin
A technology of diglycidyl ester and mixed phthalic acid, applied in the field of preparation of glycidyl ester, can solve the problems of high product cost, restricting wide application, restricting production efficiency and application, etc. The effect of avoiding recycling and promoting widespread application
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Embodiment 1
[0019] In the 100ml four-necked flask, add successively 10.1g of PTA secondary residues with an acid value of 617mgKOH / g, the catalyst triphenylphosphine is 0.5% of the quality of the PTA residues, i.e. 0.05g, and the solvent butyl acetate is 0.05g of the PTA secondary residues. 2 times, that is 20g. Stir, heat to reflux, weigh 15.5g of epichlorohydrin with the molar ratio of carboxylic acid and epichlorohydrin in the PTA secondary residue of 1.0:1.5, add it dropwise to the reaction solution, and reflux for 0.5h , stop heating, add 0.5g of activated carbon, continue to stir and cool for 1h, remove the activated carbon by suction filtration, remove the solvent by rotary evaporation of the filtrate, weigh, add an appropriate amount of solvent dichloromethane, and weigh NaOH with a molar ratio of 1:2.0 Solid 4.1g, prepare 50% NaOH aqueous solution, slowly add NaOH aqueous solution dropwise under stirring state, to the reaction filtrate, stir and react at room temperature for 3 ho...
Embodiment 2
[0021] Add 10.1 g of PTA secondary residues with an acid value of 617 mgKOH / g to a 100 ml four-necked flask, the catalyst triphenylphosphine is 1% of the mass of the PTA residues, i.e. 0.1 g, and the solvent toluene is 2.5 times of the PTA secondary residues , ie 25g. Stir, heat to reflux, weigh 20.2 g of epichlorohydrin with the molar ratio of the carboxylic acid in the PTA secondary residue to epichlorohydrin at a ratio of 1.0:2.0, add it dropwise to the reaction solution, and reflux for 3 hours. Stop heating, add 0.5g of activated carbon, continue to stir and cool for 1h, remove the activated carbon by suction filtration, weigh 4.4g of NaOH solid at a molar ratio of 1:2.5, prepare a 50% NaOH aqueous solution, and slowly add it dropwise under stirring NaOH aqueous solution was added to the reaction filtrate, stirred at room temperature for 4 hours, washed with water until neutral, separated into layers, the lower layer was removed, and rotary evaporated to obtain 4.2 g of a ...
Embodiment 3
[0023] In the 100ml four-necked flask, add successively the PTA secondary residue 10.1g of acid number 617mgKOH / g, catalyst triphenylphosphine is 3% of the quality of PTA residue, i.e. 0.3g, solvent butyl acetate PTA secondary residue 3% times, that is 30g. Stir, heat to reflux, weigh 25.8g of epichlorohydrin with the molar ratio of carboxylic acid and epichlorohydrin in the PTA secondary residue of 1.0:2.5, add it dropwise to the reaction solution, and reflux for 0.5h , stop heating, add 0.5g of activated carbon, continue to stir and cool for 1h, remove the activated carbon by suction filtration, remove the solvent by rotary evaporation of the filtrate, weigh, add an appropriate amount of dichloromethane, and weigh the NaOH solid with a molar ratio of 1:3 5.2g, prepare 50% NaOH aqueous solution, slowly add NaOH aqueous solution dropwise under stirring state, after stirring for 5h, wash with water until neutral, separate layers, remove the lower layer, and rotary steam to obta...
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