Method for synthesizing acetonitrile through one-step ammoniating method with acetic acid

A technology of acetic acid and acetonitrile, which is applied in the purification/separation of carboxylic acid nitriles, organic chemistry, ammonia-carboxylic acid reaction preparation, etc. It can solve the problems of difficult quality assurance, long process flow, and shortage of acetonitrile, and achieve fewer types of impurities, The separation process is simple and the process is short

Active Publication Date: 2010-09-15
SHANDONG HEYI GAS CO LTD DONGYING CITY
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Problems solved by technology

[0003] At present, the industrial acetonitrile products are all produced by the acrylonitrile by-product method, the output is limited (about 2.5% of the acrylonitrile output), and the quality is difficult to guarantee
Such as Chinese patent, application number CN 03112026.1 disclosed "method for synthesizing high-purity acetonitrile by ammoxidation of acetic acid", has described a kind of method for synthesizing high-purity acetonitrile by ammoxidation of ethanol, is the method for synthesizing acrylonitrile with reference to propylene ammoxidation, with ethanol, liquid Ammonia and oxygen are used as raw materials, and fluidized bed catalytic reaction technology is adopted. The process consists of three parts: reaction process, recovery process and refining process. Due to the long process flow, large investmen

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The internal structure and parameters of the fixed bed reactor are as follows:

[0024] Above is the raw material distributor, the raw material distributor is multi-tube type, the distribution pipes are vertically downward, and the distribution pipes are arranged in a square or equilateral triangle. The number of distribution pipes per square meter of the reactor cross section is 20, and the aperture is 3.8mm;

[0025] (1) Reaction:

[0026] Acetic acid and liquid ammonia are respectively vaporized and preheated to 360°C, and sent from the multi-tubular raw material distributor on the upper part of the reactor to a fixed-bed reactor equipped with catalyst aluminum oxide for reaction to generate a mixed gas containing acetonitrile The reaction temperature is 380°C, the pressure at the top of the reactor is 0.005MPa gauge pressure, the linear velocity of the empty bed is 0.8m / s, the ratio of the amount of acetic acid feed to the reactor, that is, the reaction weight hourl...

Embodiment 2

[0041] In the reaction process, acetic acid and liquid ammonia are respectively vaporized and preheated to 380°C; ammoniation reaction is at 400°C; the pressure at the top of the reactor is 0.060Mpa gauge pressure; the linear velocity of the empty bed is 0.7m / s; the reaction weight hourly space velocity WWH0.2h -1 ;

[0042] In the refining process, the reflux ratio at the top of the deamination 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 flow to the side line withdrawal is 3.0;

[0043] All the other parts are identical with embodiment 1.

[0044] The result of embodiment 2:

[0045] Acetic acid conversion ≥ 99%, yield ≥ 90%

[0046] The relative content of acetonitrile in the product is ≥90%

[0047] Purity of refined acetonitrile ≥99.9%

[0048] Raw material consumption: acetic acid: 1.5 tons / ton, ammonia 0.5 tons / ton

[0049] The catalyst cost is about 200 yuan / ton.

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Abstract

The invention discloses a method for synthesizing acetonitrile through a one-step ammoniating method with acetic acid. The method comprises the following steps of: (1) reacting acetic acid with liquid ammonia in a fixed-bed reactor provided with a catalyst of aluminum oxide to generate a mixed gas containing the acetonitrile; and (2) continuously refining the gas mixture to obtain an acetonitrileproduct. By adopting the method, the acetonitrile product is relatively pure, the purity can reach more than 99.9%, the separation process is relatively simple, the process is short, the energy consumption in the production process is low, the energy consumption of a unit product is about 40% of the energy consumption with a by-product method, and the cost is lower. The separation process adopts a physical separation method, and avoids the problem of generating a great deal of wastewater and waste gas in the chemical process in the by-product method. Meanwhile, because the synthesis method isadopted, the limitation that the yield is restricted by the main product can be thoroughly avoided.

Description

technical field [0001] The invention relates to a method for synthesizing acetonitrile with acetic acid and ammonia as raw materials. Background technique [0002] Acetonitrile is an important fine chemical intermediate product and chemical solvent, and is an intermediate for the synthesis of medicines and spices, such as active medium solvents for the synthesis of vitamin B1, vitamin A, cortisone and amino acids, carbon amine drugs and other Intermediate solvent, which can replace chlorinated solvent; raw material for manufacturing triazine nitrogen fertilizer synergist; used as denaturant for acetic acid; used for preparing 2-picoline, triazine, ethylamine in organic synthesis , dipropionitrile, imidazole, propylene bisacetonitrile, etc. Acetonitrile can be used as an extractant for extracting butadiene and isoprene, a spinning flux for synthetic fibers and a solvent for special coatings such as vinyl coatings; it is used in the petroleum industry to remove tar, phenol an...

Claims

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Application Information

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IPC IPC(8): C07C255/03C07C253/22C07C253/34
Inventor 于景东张斌杜寿考郭天明
Owner SHANDONG HEYI GAS CO LTD DONGYING CITY
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