Method for eliminating oxalic acid in dimethyl ester through esterification reaction and obtaining polyester-grade ethylene glycol
A technology of esterification reaction and medium oxalic acid, which is applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylate, etc., can solve the problem of decreased thermal stability of polyester products, difficulty in hydrogenation, inability to ensure desorption In addition to other issues
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Embodiment 1
[0040] according to figure 1 In the process flow shown, a fixed-bed reactor is used, and the raw material dimethyl oxalate (containing a certain amount of oxalic acid) is mixed with methanol 20 times its mass into the reactor, and the mass space velocity of the mixed raw material is 5.0h -1 , the esterification temperature is 68°C, and the pressure is 0.1MPa. After 4 hours of reaction, samples were taken for chromatographic analysis and calculation. The influence of different catalysts on the conversion rate of raw materials is shown in Table 1.
[0041] .
[0042] Reaction conditions: pressure: 0.1 MPa, methanol multiple: 20, catalyst: 100 g, reaction temperature 68°C, reaction time 4h.
[0043] It can be seen from Table 1 that different catalysts have a great influence on the catalyst activity, when 11%Fe 2 o 3 -2%La 2 o 3 - When 3%CaO / 3A is used as the catalyst, the catalytic effect is the best, and the conversion rate of oxalic acid can reach 98.9%.
Embodiment 2
[0045] according to figure 1 The process flow shown, using a fixed bed reactor, the catalyst is 11% Fe 2 o 3 -2%La 2 o 3 - 3%CaO / 3A, the raw material dimethyl oxalate (containing a certain amount of oxalic acid) is mixed with 10-40 times the mass of methanol into the reactor, and the mass space velocity of the mixed raw material is 5.0h -1 , the esterification temperature is 68°C, and the pressure is 0.1MPa. After 4 hours of reaction, samples were taken for chromatographic analysis and calculation. The influence of different mass multiples of methanol on the conversion rate of raw materials is shown in Table 2.
[0046] .
[0047] Reaction conditions: pressure: 0.1 MPa, catalyst: 100 g, reaction temperature 68°C, reaction time 4 h.
[0048] It can be seen from Table 2 that with the increase of methanol multiple, the conversion rate of oxalic acid gradually increases. When the methanol multiple is more than 20 times, the catalytic effect is the best, and the conversion ...
Embodiment 3
[0050] according to figure 1 The process flow shown, using a fixed bed reactor, the catalyst is 11% Fe 2 o 3 -2%La 2 o 3 - 3%CaO / 3A, the raw material dimethyl oxalate (containing a certain amount of oxalic acid) is mixed with ethanol 20 times its mass into the reactor, and the mass space velocity of the mixed raw material is 5.0h -1 , pressure 0.1MPa. After 4 hours of reaction, samples were taken for chromatographic analysis and calculation. The effects of different temperatures on the conversion of raw materials are shown in Table 3.
[0051] .
[0052] Reaction conditions: pressure: 0.1 MPa, catalyst: 100 g, space velocity: 5h -1 , reaction time 4 h.
[0053] It can be seen from Table 3 that as the reaction temperature increases, the conversion of oxalic acid first increases and then decreases. When the temperature is 100 °C, the conversion rate of oxalic acid can reach 98.6%.
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