A kind of non-volatile solubilizing diluent and its preparation method and application
A diluent and non-volatile technology, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. It can solve safety issues, personal health, environmental issues, etc., and achieve improved compatibility, high boiling point, The effect of reducing the viscosity of the system
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[0029] The preparation process of this solubilizing diluent comprises the following steps:
[0030] Dry the three-neck flask, condenser tube and other instruments at 120°C for 1.5h, take them out and cool them in a desiccator before installing them. Get 0.2mol phthalic anhydride and add in a three-necked flask, add 0.2-0.3mol fatty alcohol with more than four carbons; the fatty alcohol with more than four carbons is any one of n-butanol, n-octanol or lauryl alcohol, Heating to 110-140°C, stirring while heating until completely dissolved to form mixture A. Cool mixture A to room temperature, add 100-300mL toluene, measure the acid value and record; then add 0.3-0.5mol of dihydric alcohol and 1.5-3g of p-toluenesulfonic acid to prepare mixture B; dibasic alcohol includes ethylene glycol, Diethylene glycol, hexanediol and propylene glycol, measure the initial acid value of mixture B and record it. Put the mixture B in the water separator, heat up to 110°C and reflux, use the wa...
Embodiment 1
[0033] Dry the three-necked flask, condenser tube and other instruments at 120°C for 1.5h, take them out and cool them in a desiccator and install them; take 0.2mol of phthalic anhydride into the three-necked flask, add 0.22mol of n-butanol, heat to 140°C, and stir until completely dissolved. Cool to room temperature, add 100mL toluene, measure the acid value; then add 0.3mol diethylene glycol and 1.5g p-toluenesulfonic acid, measure the initial acid value; The water formed was separated off and the acid value was monitored during the reaction. Stop the reaction until the acid value is lower than 5; after the reaction, a yellow liquid is obtained, and the toluene is removed by rotary evaporation, then dissolved in dichloromethane, washed with 5% sodium bicarbonate until neutral, washed twice with saturated saline and evaporated The solvent was removed to obtain a pale yellow solubilizing diluent.
[0034] Utilize the solubilizing diluent prepared in this embodiment to prepar...
Embodiment 2
[0036] Dry the three-neck flask, condenser tube and other instruments at 120°C for 1.5h, take them out and cool them in a desiccator before installing them. Take 0.2mol of phthalic anhydride into a three-necked flask, add 0.22mol of n-octanol, heat to 110°C, and stir until completely dissolved. Cool to room temperature, add 200mL of toluene, measure the acid value; then add 0.3mol ethylene glycol and 1.5g p-toluenesulfonic acid, measure the initial acid value. Add a water separator, heat up to 110°C and reflux, use a water separator to continuously separate the generated water, monitor the acid value during the reaction, until the acid value is lower than 5, the reaction ends. A yellow liquid was obtained, and the toluene was distilled off under reduced pressure, then dissolved in dichloromethane, washed with 5% sodium bicarbonate until neutral, washed twice with saturated brine, and the solvent was distilled off to obtain a light yellow solubilizing diluent.
[0037] Utilize...
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