Method for preparing organic diamine from amino nitrile organic matter
A technology of organic diamine and aminonitrile, which is applied in the preparation of amino compounds, the preparation of organic compounds, the purification/separation of amino compounds, etc. It can solve the problems of low product purity and easy deactivation of catalysts, and achieve high purity and high reaction Selectivity and conversion rate, energy saving effect
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[0199] Catalyst A is a carbon-based cobalt catalyst co-doped with nitrogen and phosphorus, and its preparation method comprises the steps:
[0200] (I) Mix 100.84g activated carbon (carbon content 84.5%, pore volume 9.6cm 3 / g, the specific surface area is 273m 2 / g), 30.72g cobalt nitrate hexahydrate, 51.03g urea, 9.79g triphenylphosphine and solvent (100.66g water and 101.29g ethanol), the time of stirring and mixing is 12h, obtains the mixed material;
[0201] (II) The mixed material is slowly evaporated to dryness at 55° C. for 24 hours to remove the solvent to obtain the precipitated material;
[0202] (Ⅲ) The desolvated material is placed in a tube furnace after being uniformly ground, and pyrolyzed in an argon atmosphere, and the mass space velocity of the argon is 1h -1 , the temperature was raised to 600°C at 5°C / min, and the pyrolysis time was 2h to obtain a nitrogen-phosphorus co-doped carbon-based cobalt catalyst.
[0203] The nitrogen adsorption and desorption ...
Embodiment 1
[0241] This embodiment provides a method for preparing hexamethylenediamine from 6-aminocapronitrile, the magnetically stable reaction device used in the method is as Figure 4 As shown, specifically, the magnetically stable reaction device includes a first heating device 1 and a second tubular reactor 2 connected in sequence; the second tubular reactor 2 is provided with 4 Hex The Helmholtz coils 9; the Helmholtz coils 9 are independently connected to the transformer.
[0242] Each of the Helmholtz coils 9 has 500 turns.
[0243] A heating component 3 is arranged outside the first heating device 1 . Quartz filler is arranged in the first heating device 1 . The first heating device 1 is a tubular reactor with a length of 500 mm, an inner diameter of 5 mm, and a stainless steel tube. The bottom and / or lower side of the first heating device 1 is provided with a first inlet 4 , and the top is provided with a first outlet 5 .
[0244] The length of the second tubular reactor 2...
Embodiment 2
[0250] This embodiment provides a method for preparing hexamethylenediamine from 6-aminocapronitrile, the magnetically stabilized bed reaction device used in the method includes a first heating device and a second tubular reactor connected in sequence; the second tube There are six Helmholtz coils arranged axially outside the reactor; each of the Helmholtz coils is independently connected to the transformer.
[0251] Each of the Helmholtz coils has 200 turns.
[0252] A heating component is arranged outside the first heating device. A glass filler is arranged in the first heating device. The first heating device is a tubular reactor with a length of 800 mm, an inner diameter of 10 mm, and a stainless steel tube. The bottom and / or lower side of the first heating device is provided with a first inlet, and the top is provided with a first outlet.
[0253]The length of the second tubular reactor is 800 mm, the inner diameter is 10 mm, and the material is stainless steel tube. ...
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