Preparation method for m-xylylenediamine
A technology for m-xylylenediamine and isophthalonitrile, which is applied in the field of preparation of high-purity m-xylylenediamine, can solve the problems of large loss of m-xylylenediamine, complicated operation, many steps, etc., and saves energy. consumption, good yield, and the effect of reducing impurities
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Embodiment 1
[0058] 1) Ammoxidation reaction:
[0059] Ammoxidation uses catalysts with alumina as a carrier, the carrier content accounts for 55% of the catalyst weight, and other components are composed of V, Cr, Mo and P in a ratio of 1:1:0.1:0.1. Fill 5kg of this catalyst in the fluidized bed reactor, the reaction raw material is preheated to 400 DEG C before entering the reactor, the reaction hot spot temperature is 450 DEG C, the source of oxygen is air, m-xylene: ammonia: the mol ratio of air is 3: 20:77. The reaction pressure is 0.02-0.05MPa. The gas residence time is controlled at 0.5s. The gas containing isophthalonitrile was obtained. Based on the m-xylene added to the reaction system, the molar yield of IPN was 85.1%, and the yield of methylbenzonitrile was 2.5%.
[0060] 2) Solvent extraction:
[0061] The gas containing isophthalonitrile is added to the extraction tower from the bottom of the extraction tower. The inner diameter of the extraction tower is 100mm, the heig...
Embodiment 2
[0069] 1) Ammoxidation reaction:
[0070] Ammoxidation uses catalysts with alumina as the carrier, the carrier content accounts for 55% of the catalyst weight, and other components are composed of V, Cr, Mo and Fe in a ratio of 1:1:0.1:0.1. Load 5kg of the catalyst into the fluidized bed reactor. The reaction raw material is preheated to a reaction hot spot temperature of 480°C before entering the reactor. The oxygen source is air, and the volume ratio of m-xylene:ammonia:air is 1:6:28. The reaction pressure is 0.02-0.05MPa. The gas residence time is controlled at 1s. The gas containing isophthalonitrile was obtained. Based on the m-xylene added to the reaction system, the molar yield of IPN was 85.3%, and the yield of methylbenzonitrile was 2.5%.
[0071] 2) Solvent extraction:
[0072] The gas containing isophthalonitrile is added to the extraction tower from the bottom of the extraction tower. The inner diameter of the extraction tower is 100mm, the height is 850mm, and...
Embodiment 3
[0080] 1) Ammoxidation reaction:
[0081] Ammoxidation adopts catalyst with alumina as the carrier, the carrier content accounts for 55% of the catalyst weight, and other components are composed of V, Cr, Fe and P in the ratio of 1:1:0.1:0.1. Load 5kg of the catalyst into the fluidized bed reactor. The reaction raw material is preheated to a reaction hot spot temperature of 350°C before entering the reactor. The source of oxygen is air. The molar ratio of m-xylene:ammonia:air is 1:4:20. The reaction pressure is 0.02-0.05MPa. The gas residence time is controlled at 1s. The gas containing isophthalonitrile was obtained. Based on the m-xylene added to the reaction system, the molar yield of IPN was 84.9%, and the yield of methylbenzonitrile was 2.5%.
[0082] 2) Solvent extraction:
[0083]The gas containing isophthalonitrile is added to the extraction tower from the bottom of the extraction tower. The inner diameter of the extraction tower is 100mm, the height is 850mm, and ...
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