Method for recovering nylon 66 material by means of alcoholysis
A recovery method, nylon technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of amino compounds, etc., to achieve high purity, simple operation, easy control, and low cost
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Embodiment 1
[0022] In a high-pressure reaction kettle with a thermometer, add 1 mol of nylon 66 particles, 2 mol of sulfuric acid, and 20 mol of methanol in sequence, and stir the reaction at 160°C at a speed of 300r / min for 4 hours. Ethyl is extracted 5 times from the alcoholysis reaction mixture with ethyl ester at a volume ratio of 5:1, and the combined extracts are evaporated under reduced pressure to remove ethyl acetate, then distilled under reduced pressure by an oil pump, and collected at 109~110°C under a pressure of 12~14mmHg. Fraction dimethyl adipate, the yield is 86.85%; add 2mol calcium hydroxide to the raffinate phase hexamethylenediamine sulfate aqueous solution at room temperature, stir, react for a period of time and then heat to 50°C to make the reaction complete . Oil pump decompression distillation, under the pressure of 4-6mmHg, the fraction hexamethylenediamine at 90-110°C is collected, and the yield is 87.82%; the alcoholysis rate of nylon 66 is 100%.
[0023] Dep...
Embodiment 2
[0030]In a high-pressure reaction kettle with a thermometer, add 1 mol of nylon 66 particles, 3 mol of formic acid, and 25 mol of methanol in sequence, stir and react at 120°C at a speed of 400r / min for 6h, cool to room temperature naturally, open the kettle, and use the organic solvent tetrachloride Carbon dioxide extracts the mixed liquid after alcoholysis reaction for 4 times according to the volume ratio of 6:1, and the combined extraction phases are decompressed and rotary evaporated to remove carbon tetrachloride, and then the oil pump is distilled under reduced pressure. The fraction of dimethyl adipate has a yield of 80.85%; add 4.5 mol of sodium bicarbonate to the raffinate aqueous solution of hexamethylenediamine formate at room temperature, stir, and heat to 40°C after a period of reaction. to complete the reaction. Oil pump vacuum distillation, under the pressure of 4 ~ 6mmHg to collect the fraction of hexamethylenediamine at 90 ~ 110 ° C, the yield is 80.16%; the ...
Embodiment 3
[0032] In a high-pressure reaction kettle with a thermometer, add 1 mol of nylon 66 particles, 3.5 mol of phosphoric acid, and 15 mol of ethanol in sequence, and stir at 140°C for 8 hours at a speed of 350 r / min. The mixed solution of hexane and chloroform is extracted 7 times from the mixed solution after the alcoholysis reaction according to the volume ratio of 4:1, and the combined extraction phase is decompressed and rotary evaporated to remove the organic solvent, and the oil pump is distilled under reduced pressure. Collect diethyl adipate diethyl adipate at 110-120°C, and the yield is 82.85%; add 3 mol of sodium hydroxide to the raffinate phase hexamethylenediamine phosphate aqueous solution at room temperature, stir, react for a period of time and then heat to 55°C to complete the reaction. Oil pump decompression distillation, under the pressure of 4 ~ 6mmHg to collect the fraction of hexamethylenediamine at 90 ~ 110 ℃, the yield is 81.64%; the alcoholysis rate of nylo...
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