Synthesis method of zoalene

A synthesis method and technology of qiuli-ling are applied in the synthesis field of anti-coccidial medicine qiu-li-ling, which can solve the problems such as the accumulation of a large amount of sulfuric acid, a large amount of waste ammonia water, and the increase, so as to avoid product quality, improve utilization rate, and avoid waste. Effect

Active Publication Date: 2016-08-31
ZHEJIANG RONGYAO CHEM
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0006] In order to solve the technical problems of producing a large amount of waste acid liquid after the nitration reaction and the accumulation of sulfuric acid in the production process in the production process of the prior art, the present invention provides a A kind of synthetic method of coladrin that solves the problem of liquid and sulfuric acid accumulation
[0007] On the other hand, the present invention needs to solve the technical problem that a large amount of waste ammonia water is produced in the ammoniation process in the prior art in the production process of codiflualine, and provide a method for synthesizing cocifluazol that can recycle and reuse ammonia water

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Embodiment 1

[0031] Such as figure 1 , figure 2 A synthetic method of cocifluazol shown includes the following steps A, nitration process, step B, acyl chloride process, step C, ammonification process. In the nitration process of step A, put 300L of concentrated sulfuric acid into the enamel reaction kettle, turn on the agitator, then put in 75kg of o-toluic acid, stir until it is completely dissolved, then add 65L of nitric acid dropwise into the above system, and control the temperature of the system , continue to stir after dripping, cool, dilute feed liquid with distilled water, filter, the gained solid is through washing with water, dry to obtain nitration product 3,5-dinitro-o-toluic acid 117kg, yield is 93.9%.

[0032] In the step polymerization A, the recovery and reuse process of concentrated sulfuric acid is set, and the recovery and reuse process of the concentrated sulfuric acid is set to first recycle the waste acid 726L produced after nitration reaction dilution and washing...

Embodiment 2

[0035] Such as figure 1 , figure 2A synthetic method of cocifluazol shown includes the following steps A, nitration process, step B, acyl chloride process, step C, ammonification process. Step A is the same as in Example 1 during the nitration process. In step A, the recovery and reuse process of the concentrated sulfuric acid is set to first recycle the waste acid 750L produced after the nitration reaction dilution and washing, and then pass the waste acid to into the distillation pot for vacuum distillation, the temperature of the vacuum distillation is set to 150°C, the vacuum degree is set to 0.09MPa, the concentration of sulfuric acid is concentrated to 85%, and at the same time the residual nitric acid in the waste acid is evaporated, and the concentrated sulfuric acid is passed into Sulfur trioxide 95kg, stirred 1 hour, left standstill 4 hours again, can prevent like this from containing sulfur trioxide in sulfuric acid and take place sulfonation side reaction; Pass t...

Embodiment 3

[0038] Such as figure 1 , figure 2 The synthetic method of a kind of cudaloxine shown comprises the following steps A, nitration process, step B, acyl chloride process, step C, ammonification process, step A nitration process is the same as Example 1, and in step A, concentrated The process of sulfuric acid recovery and reuse is set as follows: first, 720L of waste acid produced after nitration reaction dilution and washing is recovered, and then the waste acid is passed into the distillation kettle for vacuum distillation. The temperature of vacuum distillation is set at 130°C, and the vacuum degree Set it to 0.08MPa to concentrate the sulfuric acid concentration to 80%, and at the same time distill off the residual nitric acid in the waste acid, pass 93kg of sulfur trioxide into the concentrated sulfuric acid, stir for 1.5 hours, and then let it stand for 6 hours, then pass in sulfur trioxide Finally, make the concentration of the prepared concentrated sulfuric acid reach ...

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Abstract

The invention discloses a synthesis method of zoalene, belonging to the technical field of pharmaceutical engineering. The method comprises the following steps: A. nitration process, B. acylating chlorination process, and C. ammonifying process, wherein in the step A, a process of recycling concentrated sulfuric acid is set, specifically, the collected waste acid is treated by reduced pressure distillation and is concentrated, sulfur trioxide is then added into the treated waste acid, and the newly prepared concentrated sulfuric acid is added into a reaction kettle again for carrying out a nitration reaction; in the step C, a process of recycling waste ammonia water is set. By recycling and reusing raw materials, the method does not cause accumulative increment of sulfuric acid and ammonia water, thus improving the utilization rate of the raw materials and lowering the production cost; furthermore, the method reduces the treatment cost of the waste acid and the waste ammonia water and greatly reduces the discharge amount of waste water, thus having an important significance for environmental protection.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical engineering, and relates to a green production process of coccidia, in particular to a method for synthesizing the anticoccidial coccidia. Background technique [0002] Zoalene, also known as Nitrolamide (DOT), chemical name is 3,5-dinitro-2-methylbenzamide, is a highly efficient, low toxicity, small drug resistance, no residue Nitramide is an anticoccidiostat, and it has the function of promoting the growth of poultry. This product is used in feed, and has good effects on various Eimeria coccidia in chickens and coccidia in turkeys. It is an excellent anticoccidiosis agents. [0003] The traditional production method of globulin is to synthesize o-toluic acid as the main starting material. The method is to firstly nitrate o-toluic acid to obtain 3,5 dinitro-o-toluene Formic acid is then chlorinated into acid chlorides, and finally ammonolysis is used to obtain cudalazine; but this method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/65
CPCC07C201/08C07C201/12C07C231/02C07C205/57C07C233/65
Inventor 陈仁尔陈建华张娜鲁泓波黄运奇
Owner ZHEJIANG RONGYAO CHEM
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