Method for removing formic acid online in the process of trioxymethylene synthesis
A paraformaldehyde synthesis process technology, applied in fractionation, organic chemistry, etc., can solve problems that affect the normal progress of paraformaldehyde synthesis reactions, affect the quality of paraformaldehyde products, increase equipment and processing costs, and achieve low operating costs , Reduce energy consumption, low cost of raw materials
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Embodiment 1
[0029] In a 500mL reactor, add 200g of 58.7wt% formaldehyde solution and 8.1g of acidic ionic liquid catalyst. Control the temperature of the oil bath to 125°C, and the temperature in the reactor to 100°C. The mixture gas of formaldehyde, product paraformaldehyde and by-product formic acid in the reaction kettle will continue to fractionate and return to the reaction kettle after passing through the formic acid removal device to complete the reactive distillation process.
[0030] The formic acid removal device is a 500mL three-necked bottle placed in an oil bath at 105°C, and the bottle contains 5wt% CaCO 3 Suspension, the internal temperature of the solution is 90°C.
[0031] After the reaction is stable, adjust the reflux ratio R=2, and at the same time, add 58.7wt% formaldehyde solution at the flow acceleration rate of 50ml / h. The paraformaldehyde product was extracted at a rate of 50ml / h.
[0032] According to gas chromatography analysis, the extracted product componen...
Embodiment 2
[0034] Add 2wt% MgCO to the formic acid removal unit 3 Suspension, all the other reaction conditions are with embodiment 1. According to gas chromatography analysis, the extracted product components are formaldehyde 18.94wt%, paraformaldehyde 18.48wt%, methanol 1.92wt%, formic acid 127.56ppm, and the remaining components are water.
Embodiment 3
[0036] Add 0.6wt% BaCO to the formic acid removal unit 3 Suspension, all the other reaction conditions are with embodiment 1. According to gas chromatography analysis, the extracted product components are 21.92wt% formaldehyde, 22.04wt% paraformaldehyde, 2.63wt% methanol, 194.68ppm formic acid, and the remaining components are water.
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