Method for refining tri-n-hexyl trimellitate and used refining agent thereof
A technology of tri-n-hexyl trimellitate and trimellitic acid, which is applied in the field of organic compound preparation, can solve problems such as unfavorable economic benefits, difficulty in reducing costs, and low production efficiency, so as to reduce production costs, improve production efficiency, and operate convenient effect
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Embodiment 1
[0018] Preparation of refined preparation: mix (100) g calcium oxide, (100) g magnesium oxide, (200) g activated carbon, and (100) g silicon dioxide evenly.
[0019] (1) Esterification step: drop into successively 100 kilograms of trimellitic acid, 256 kilograms of n-hexanols, 0.3 kilograms of concentrated sulfuric acid in a 500-liter reactor with a heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator. Kilogram, under stirring, slight vacuum, heating to boiling reaction at the same time, keep boiling reflux state, continuously separate water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is terminated.
[0020] (2) Water washing step: add 250 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand for stratification, and remove the water layer therein.
[0021] (3) Dealcoholization step: dealcoholizing the washe...
Embodiment 2
[0025] Preparation of refined preparation: (120) g calcium oxide, (120) g magnesium oxide, (240) g gac, (120) g silicon dioxide are mixed evenly.
[0026] (1) Esterification reaction step: drop into successively 100 kilograms of trimellitic acid, 256 kilograms of n-hexanols, 0.3 kilograms of concentrated sulfuric acid in a 500-liter reactor with a heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator. Kilogram, under stirring, slight vacuum, heating to boiling reaction at the same time, keep boiling reflux state, continuously separate water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is terminated.
[0027] (2) Water washing step: add 250 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand for stratification, and remove the water layer therein.
[0028] (3) Dealcoholization step: dealcoholizing the washed ...
Embodiment 3
[0032] Preparation of refined preparation: (140) g calcium oxide, (140) g magnesium oxide, (280) g gac, (140) g silicon dioxide are mixed evenly.
[0033] (1) Esterification reaction step: drop into successively 100 kilograms of trimellitic acid, 256 kilograms of n-hexanols, 0.3 kilograms of concentrated sulfuric acid in a 500-liter reactor with a heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator. Kilogram, under stirring, slight vacuum, heating to boiling reaction at the same time, keep boiling reflux state, continuously separate water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is terminated.
[0034] (2) Water washing step: add 50 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand for stratification, and remove the water layer therein.
[0035] (3) Dealcoholization step: dealcoholizing the washed m...
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