Methyl esterification recycling method of alkali decrement wastewater solid residue
A technology for alkali reduction of waste water and solid residues, applied in chemical instruments and methods, organic chemistry, carboxylate preparation and other directions, can solve the problems of low quality, low solid purity of terephthalic acid, and low utilization value, etc. The effect of recovery
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Embodiment 1
[0051] The alkali reduction solid residue of the methyl esterification treatment in this embodiment comes from the alkali reduction wastewater treatment unit of a large textile company. The main composition of the residue is shown in Table 2. Drying pretreatment is required before the reaction to ensure the residue raw material The water content is less than 0.5%.
[0052] Table 2. Composition of solid residues in alkali reduction wastewater for methyl esterification treatment
[0053]
[0054] A 1.0L high-pressure reactor is used for methyl esterification reaction of PTA oxidation residue. The high-pressure reactor is equipped with electric heating and PID temperature control system. The gas phase outlet of the reactor is equipped with a stop valve, condenser, back pressure valve, etc., and the condensate It is not directly refluxed, but can be recovered from a solvent tank. First quantitatively weigh 200.0g of dry alkali weight reduction residue and 600.0g of methanol in...
Embodiment 2
[0058] Carry out the methyl esterification reaction of the residue similarly to Example 1, the difference is that the residue methanol feed ratio is 1:2, the reactor feed is 250.0g residue and 500.0g methanol, the esterification temperature is 260°C, and the pressure is 10.0MPa, Esterification time was 2 hours. After the reaction was finished, samples were taken and analyzed, and the calculated residue TA conversion rate was 83.8%, and the complete methyl esterification rate was 75.5%. The results are listed in Table 3 for comparison.
Embodiment 3
[0060] The methyl esterification reaction of the residue was carried out similarly to Example 2, the feed to the reactor was also 250.0 g residue and 500.0 g anhydrous methanol, and the esterification temperature was also 260° C. The difference is that after esterification at 260°C for 2 hours, the shut-off valve is slowly opened, and the back pressure valve is adjusted to reduce the pressure to 2.5MPa. The plug pump continuously feeds methanol at 2ml / min into the autoclave, and maintains the reaction temperature at 260°C by electric heating. The water and methanol vapor continuously evaporated in the autoclave are recovered to the solvent tank through the condenser. After methanol was continuously fed for about 1 hour (250.0 g of methanol was continuously fed), the outlet valve was closed, and the temperature was lowered to terminate the reaction. Sampling and analysis showed that the conversion rate of residue TA was 98.8%, and the complete methyl esterification rate was 93....
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