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Production method and production system of p-nitrobenzamide

A technology of nitrobenzamide and nitrobenzoyl chloride is applied in the field of production methods and production systems of p-nitrobenzamide, and can solve the problems of waste of resources, difficulty in wastewater treatment, high ammonia nitrogen content in wastewater, and high cost, and achieves the Achieve cleaner production, reduce ammonia nitrogen content, and reduce the amount of production

Pending Publication Date: 2022-04-05
宁夏彩妍科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Based on this, the present invention provides a kind of production method of p-nitrobenzamide, to solve existing in the prior art when using p-nitrobenzoyl chloride as raw material to produce p-nitrobenzamide, the ammonia nitrogen content of waste water is high, causes Resource waste and waste water treatment are difficult and costly technical problems

Method used

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  • Production method and production system of p-nitrobenzamide
  • Production method and production system of p-nitrobenzamide
  • Production method and production system of p-nitrobenzamide

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0063] Configuration mass concentration is 10% ammonia solution, get 95g of this ammonia solution, add in the four-necked flask, be warmed up to 75 ℃, in the four-necked flask, drip the p-nitrobenzoyl chloride of melting, reduce to the pH value of reaction solution to below 10. In the four-necked flask, dropwise add 10% NaOH solution simultaneously, adjust the pH value of reaction solution respectively to be 8~9,9~10,10~11,11~12, drop 92.8g ( 0.5mol) of molten p-nitrobenzoyl chloride. The temperature of the reaction solution was raised to 85° C. and kept for 1 h. Cool down to room temperature, filter the feed liquid to obtain a mixture of solid p-nitrobenzamide and p-nitrobenzoyl chloride, the liquid is NaCl solution, and test the content of solid p-nitrobenzamide and p-nitrobenzoyl chloride , to test the ammonia nitrogen content of the NaCl solution, and the test results are shown in Table 1.

[0064] Table 1 Experimental Example 1 Test Results

[0065]

experiment example 2

[0067] Configure ammonia water mixed solution A. In ammonia water mixed solution A, the mass concentration of ammonia water is 10%, and the mass concentration of NaCl is 10%. Molten p-nitrobenzoyl chloride was added dropwise until the pH value of the reaction solution was lowered to below 10. In the four-necked flask, dropwise add 10% NaOH solution simultaneously, adjust the pH value of reaction solution respectively to be 8~9,9~10,10~11,11~12, drop 92.8g ( 0.5mol) of molten p-nitrobenzoyl chloride. The temperature of the reaction solution was raised to 85°C and kept for 2h. Cool down to room temperature, filter the feed liquid to obtain a mixture of solid p-nitrobenzamide and p-nitrobenzoyl chloride, the liquid is NaCl solution, and test the content of solid p-nitrobenzamide and p-nitrobenzoyl chloride , to test the ammonia nitrogen content of the NaCl solution, and the test results are shown in Table 2.

[0068] Table 2 Experimental Example 2 Test Results

[0069]

experiment example 3

[0071] Using the waste water generated in Experimental Example 2, a mixed solution of ammonia and water was prepared. In the mixed solution of ammonia and water, the mass concentration of ammonia was 10%. Take 95g of the aqueous ammonia solution, put it into a four-necked flask, raise the temperature to 80°C, and drop molten p-nitrobenzoyl chloride into the four-necked flask until the pH value of the reaction solution drops below 10. In the four-necked flask, dropwise add 10% NaOH solution simultaneously, adjust the pH value of reaction solution respectively to be 8~9,9~10,10~11,11~12, drop 92.8g ( 0.5mol) of molten p-nitrobenzoyl chloride. The temperature of the reaction solution was raised to 85°C and kept for 2h. Cool down to room temperature, filter the feed liquid to obtain a mixture of solid p-nitrobenzamide and p-nitrobenzoyl chloride, the liquid is NaCl solution, and test the content of solid p-nitrobenzamide and p-nitrobenzoyl chloride , to test the ammonia nitrogen...

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Abstract

The invention provides a production method and a production system of p-nitrobenzamide, and belongs to the technical field of fine chemical engineering. The method comprises the following steps: firstly, dropwise adding molten p-nitrobenzoyl chloride into an ammonia water mixed solution A at the temperature of 75-80 DEG C, enabling all p-nitrobenzoyl chloride to be subjected to ammonolysis to form p-nitrobenzamide, and meanwhile, absorbing part of ammonia water to form NH4Cl; when the pH value of the reaction solution is reduced to be below 10, the ammonia water is used up, at the moment, strong alkali is dropwise added into the reaction solution, the strong alkali reacts with NH4Cl in the reaction solution, free ammonia is released, the strong alkali continues to react with p-nitrobenzoyl chloride, p-nitrobenzamide is generated, and therefore the content of ammonia nitrogen in the generated wastewater is greatly reduced. Meanwhile, the generated wastewater is recycled and used for preparing the ammonia water mixed solution A, so that the wastewater generation amount is greatly reduced, effective recycling of resources is realized, and clean production is realized.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, in particular to a production method and production system of p-nitrobenzamide. Background technique [0002] P-aminobenzamide (also known as red base DB-70) is an important fine chemical intermediate, which is widely used in the dye industry. An important process route for the industrial synthesis of p-aminobenzamide is: using p-nitrobenzoic acid as a raw material, undergoing acid chloride reaction, condensation reaction, and reduction reaction in turn to make p-aminobenzamide. The reaction process is as follows: [0003] [0004] In the prior art, for example, the Chinese invention patent with the patent number 201410380825.0 discloses a method for preparing p-aminobenzamide, wherein, in the process of preparing p-nitrobenzamide from p-nitrobenzoyl chloride, in the reaction vessel Add ammonia water with a concentration of 10wt% to 30wt%, start stirring, and add p-nitrobenzoyl chlorid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/65B01J19/00
Inventor 申井会吴建良
Owner 宁夏彩妍科技有限公司
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