The manufacture method of bis(2-ethylhexyl) terephthalate
A technology of terephthalic acid and terephthalic acid is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., to achieve the effects of increasing the reaction rate, reducing the reaction time, and improving the filtration rate.
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Embodiment 1
[0028]In a 3L autoclave equipped with stirrer, thermometer, back pressure valve manometer, oil-water separator, return line, nitrogen flow controller, condenser and 30cm filling fractionation column, 1333.2g (10.24mole) Isooctyl alcohol (also known as 2-ethylhexanol, 2-EH), 531.5g (3.20mole) of pure terephthalic acid (PTA), 3.07g (relative to the total weight of the reaction system alcohol and acid reactants TyzorPC-64 (phosphate titanate chelate, Ti=5.0%, purchased from DORFKETALCO.) catalyst equivalent to Ti=82ppm) was put into the reaction kettle. The reaction kettle was fully stirred under nitrogen flow and pressurized to a gauge pressure of 4.0kg / cm 2 , make the temperature rise to 232°C within 1 hour (starting esterification distillation temperature), the water and alcohol mixture brought out by the nitrogen flow begins to condense in the oil-water separator after filling the fractionation column and the condenser, and the upper alcohol mixture is refluxed The pipe is l...
Embodiment 2
[0030] Use the same reactor and reaction compound as in Example 1, but replace the packed fractionation column with a 30cm single tube, and the catalyst system uses TyzorTE (bis(triethanolamine) diisopropyl titanate chelate), Ti=8.2 %, purchased from DORFKETALCO. products). 1333.2 g (10.24 mole) of 2-EH, 531.5 g (3.20 mole) of PTA, and 1.87 g of TyzorTE (Ti=82 ppm) were put into the reactor. The reaction kettle is fully stirred under nitrogen flow and pressurized to a gauge pressure of .4.0kg / cm 2 , and heated up to 233°C in 1 hour, the water and alcohol mixture brought out by the nitrogen flow began to pass through the single tube (meaning the column without filler) and the condenser, and then condensed in the oil-water separator, and the upper alcohol mixture was led by the return pipe Return to the reactor to ensure that the reaction 2-EH / PTA is maintained at a fixed molar ratio of 3.2 / 1, and the water in the lower layer is continuously distilled out of the oil-water separ...
Embodiment 3
[0032] A reactor was used as in Implementation 1, but the catalyst used was TyzorIAM (trialkoxyphosphate butyl titanate dimer, Ti=8.8%, purchased from DORFKETALCO.). 1333.2 g (10.24 mole) of 2-EH, 531.5 g (3.20 mole) of PTA and 1.68 g of TyzorIAM (Ti=82 ppm) were put into the reactor. The reaction kettle was fully stirred under nitrogen flow and pressurized to a gauge pressure of 3.0kg / cm 2 , and heated up to 227°C within 1 hour, the water and alcohol mixture brought out by the nitrogen flow began to condense in the oil-water separator after filling the fractionation column and condenser, and the upper alcohol mixture was led back to the reactor through the return pipe to ensure the reaction 2 -EH / PTA is maintained at a fixed molar ratio of 3.2 / 1, and the water in the lower layer is continuously distilled out of the oil-water separator and taken out for metering. The reaction continues to heat up to 250°C, and after 3.7 hours, remove water from the separator and measure 116 m...
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