SU63224A1 - The method of producing nitroanilines - Google Patents

Description

The production of nitro-ankpins from the corresponding nitrochlorobenzenes by aminating with a conventional method, i.e. 23-2b-percent aqueous solutions of ammonia at 170-185 °, leads to the formation of several by-products along with the main product and significant gum formation. As a result, a relatively small yield of nitroanilines is obtained by this method. The resulting product nulls with a cleaning waste, which further reduces the yield of the final product.

According to the invention, it is proposed to produce an aminirovanne nitrochloride "ashes" at 140 ° using 50-80% ammonia solution. In this case, amination occurs with: at a sufficient rate even at a pressure of 40-55 atm.

The proposed method of aminers. And nitrochlorobesiol gives a product of high purity with quantitative yield.

Example 1. Obtaining | e n-n and tr o aiH Il IN1 a. In a steel autoclave with a capacity of 2 liters. with root

200 g of p-nitrochlorobenzene are poured in with a mixer; poured 800-830 cm of 25% ammonium water. Then the autoclave is sealed and when cooled, ammonia gas is introduced into it from a cylinder with liquid ammonia. The depth of ammonia water saturation in the autoclave is controlled by temperature and pressure. When the saturation of ammonia water is complete, close the valve and begin heating to a temperature of 140 °, at which they give a shutter speed for 12-18 hours (in: depending on the depth of saturation of ammonia water).

At the end of the ammonia lysis, the ammonia pressure is lowered through a reflux condenser (to condense steam water) into another such autoclave, the BI which is loaded with p-nitrochlorobenzene and 20-25% ammonia water. Thus, there is no need to use liquid ammonia each time for fortified ammonia water. It is also possible to lower the pressure of ammonia at the end of ammonolysis B to any autoclave, calculated for a low pressure, in which the primary is loaded with weak

amdtachny paicTBOp. The strong ammonia solution obtained in this autoclave (50-80 per cent, # 1) can be extruded under its own long-term closure in the autoclae® for ammonolysis, after a pre-load of i-nitrochlorobenzene. At the end of the ammonolysis, the p-nitroaikline is filtered and washed with water. The output is almost quantitative (99% of theoretical). The product under analysis is almost 100 percent (over 99.5%).

Example 2. P: 0i l u c e n t e n i ntroanilnna from o- “and t roxl o rb e 3 o l a.

The process is carried out exactly the same as when p-nitrolniline is obtained, but the "exposure time of 140 ° in this case is only 7-10 hours". The yield is 99% of the theoretical. The quality of the product is very high (over 99.5%).

Example 3. Getting pn l about rn and t r about a n and l and from a p d and X l about r and t r o b e N 3 o l a.

The process is carried out in the same way as in examples 1 and 2. Exposure at a temperature of 140 ° lasts 8-12 hours. (depending on the depth of ammonia water). The output is quantitative. The resulting product is highly pure.

Ammonolysis is also carried out at a temperature of 145-150 ° C, and the duration of ammoniation is shortened accordingly;

The subject matter of the method of producing nitroanilines by treating nitrochlorobenzol® with one ammonia at elevated temperatures and temperatures, characterized in that the reaction is carried out at a temperature of 140-150 ° using 50-80 percent aqueous solution. ammonia solution.