A kind of method that takes meta-position oil as raw material to prepare m-phenylenediamine
A technology for m-phenylenediamine, nitrochlorobenzene meta-position oil, which is applied in the preparation of amino compounds, chemical instruments and methods, preparation of nitro compounds, etc., can solve the waste of resources, insufficient m-nitrochlorobenzene, and influence on Problems such as the yield of nitrochlorobenzene, to achieve the effect of green environmental protection cost, simple process and easy operation
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Embodiment 1
[0029] A method for preparing m-phenylenediamine from nitrochlorobenzene meta-oil as a raw material comprises two steps: nitrochlorobenzene meta-oil nitration and catalyst hydrogenation.
[0030] Nitrification of nitrochlorobenzene meta-oil: add nitrochlorobenzene meta-oil to the reaction kettle, add concentrated sulfuric acid, raise the temperature to 60-80°C, add fuming nitric acid dropwise, and carry out nitration reaction. After the addition of nitric acid is completed, continue the reaction After standing for 2 hours, the waste acid was separated, and the material was washed twice with water to obtain a mixture of 2,4-nitrochlorobenzene and 3,5-dinitrochlorobenzene.
[0031] Catalytic hydrogenation reaction: use the mixture of 2,4-dinitrochlorobenzene and 3,5-dinitrochlorobenzene as raw material, methanol as solvent, sodium hydroxide, sodium acetate, sodium carbonate, sodium bicarbonate, Alkaline substances such as triethylamine are used as acid-binding agents, and the pr...
Embodiment 2
[0043] Nitration of nitrochlorobenzene meta-oil:
[0044] (1) Add 2000kg of meta oil and 1310kg of concentrated sulfuric acid with a mass fraction of 98% to a 5000L reactor, start stirring and raise the temperature to 75°C.
[0045] (2) Add 833 kg of fuming nitric acid (mass fraction 98%) dropwise at 75°C, the reaction is exothermic, feed circulating water to keep the temperature of the kettle at 75°C, and control it not to exceed 80°C, after the dropwise addition, keep stirring at 75°C 2 hours.
[0046] (3) Stand still to remove the waste acid, transfer the material to a washing kettle for washing, add alkali to adjust the pH value to 9-10 under the first washing and stirring, and let stand to separate the upper washing water, and wash the pH value of the washing material for the second time To neutrality, let stand to separate the upper layer of water, the lower layer of material is the intermediate 2,4-dinitrochlorobenzene and 3,5-dinitrochlorobenzene mixture. Note that the...
Embodiment 3
[0053] Nitration of nitrochlorobenzene meta-oil:
[0054] (1) Add 2000kg of meta oil and 1310kg of concentrated sulfuric acid with a mass fraction of 98% to a 5000L reactor, start stirring and raise the temperature to 75°C.
[0055] (2) Add 833 kg of fuming nitric acid (mass fraction 98%) dropwise at 75°C, the reaction is exothermic, feed circulating water to keep the temperature of the kettle at 75°C, and control it not to exceed 80°C, after the dropwise addition, keep stirring at 75°C 2 hours.
[0056] (3) Stand still to remove the waste acid, transfer the material to a washing kettle for washing, add alkali to adjust the pH value to 9-10 under the first washing and stirring, and let stand to separate the upper washing water, and wash the pH value of the washing material for the second time To neutrality, let stand to separate the upper layer of water, the lower layer of material is the intermediate 2,4-dinitrochlorobenzene and 3,5-dinitrochlorobenzene mixture. Note that t...
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