Method for preparing high-purity acetonitrile from acetic acid and ammonia by two steps
A high-purity, two-step technology, applied in the preparation of ammonia-carboxylic acid reaction, purification/separation of carboxylic acid nitrile, organic chemistry, etc., can solve the contradiction between supply and demand of by-product acetonitrile intensified by market demand, no industrial reports, and difficult quality Guarantee and other issues, to achieve the effect of low cost, less variety, and short process
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Embodiment 1
[0027] The internal structure and parameters of the fixed bed reactor are as follows:
[0028] The single reactor tube has a diameter of 45mm, an inner diameter of 40mm, and a length of 1500mm. It contains 700ml of catalyst;
[0029] (1) Response:
[0030] First, acetic acid and ammonia are neutralized to produce ammonium acetate.
[0031] The molar ratio of ammonium acetate to ammonia is: ammonium acetate: ammonia = 1.0: 1.5;
[0032] Liquid hourly space velocity of ammonium acetate 0.3h -1
[0033] The water content in the feed ammonium acetate is about 25%.
[0034] The aqueous solution of ammonium acetate is fed by a pump, and the ammonia is fed in a gaseous state. After the two are mixed and preheated to 320°C, they enter the fixed bed reactor containing the catalyst aluminum oxide from the upper part of the reactor to react; The temperature is 350°C, and the gauge pressure at the top of the reactor is 0.03 MPa.
[0035] (2) Refining:
[0036] a) The resulting product is sent to the a...
Embodiment 2
[0048] In the reaction process, the mixed raw materials are preheated to 340°C; the ammoniating reaction is 360°C; the pressure at the top of the reactor is 0.060Mpa gauge; the molar ratio of ammonium acetate to ammonia is: ammonium acetate: ammonia = 1.0: 1.6; ammonium acetate liquid space-time Speed 0.9h -1
[0049] In the refining process, the reflux ratio at the top of the ammonia removal tower is 5.0, and the operating pressure is 0.10Mpa; the top of the finished product tower adopts internal reflux, and the ratio of the reflux to the sideline withdrawal is 3.0;
[0050] The rest is the same as in Example 1.
[0051] Results of Example 2:
[0052] Acetic acid conversion rate=99%, yield=94%
[0053] Relative content of acetonitrile in the product=92%
[0054] Purity of acetonitrile after purification = 99.9%
[0055] Raw material consumption: acetic acid: 1.5 tons / ton, ammonia 0.6 tons / ton
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