Synthesis process of 2-methyl-5-nitroimidazole

A nitroimidazole and synthesis process technology, applied in the chemical industry, can solve the problems of increasing production costs, increasing waste water volume and production costs, and inconvenient material management, so as to reduce the consumption of main materials, low comprehensive treatment costs, and facilitate recycling and sales Effect

Pending Publication Date: 2021-10-01
方耀
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  • Summary
  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

Due to the direct reaction with mixed acid, a large amount of nitrogen dioxide will emerge, and the product yield is low
The prior art is to add the mixture of sulfuric acid, urea and ammonium sulfate in the reaction system as the catalyst and stabilizer of the reaction, add the mixture of nitric acid, urea and ammonium sulfate in 2-methylimidazole, then increase the temperature and drop the concentrated sulfuric acid, after that Add a mixed acid composed of nitric acid and sulfuric acid, and finally adjust the pH with ammonia water to neutralize the nitration solution, and obtain 2-methyl-5-nitroimidazole after filtration, which can eliminate smoke and improve product yield. This method exists in the actual operation process. The disadvantages are as follows: 1) Neutralization with ammonia water, because of its moderate alkalinity, the neutralization end point is pH=4.0-5.0, requires the use of a

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0021] Example 1

[0022] (1) Synthesis reaction: 31% hydrochloric acid is 31% in the reaction kettle, stirred at 2-methylimidazole by 2-methylimidazole at a temperature of 70 ° C; 120 kg of sodium nitrate at 10 ° C; then control temperature 130 ° C The dropped mass fraction was 98% nitric acid 210L, the dropwise speed was 90 kg / h, the dropwise time was 35; the insulation reaction was maintained for 30 min; when the temperature was 10 ° C, when the temperature was 50 ° C, the medium and kettle was added to the drinking water 1300kg. , Cover the human hole cover, transfer the material in the reactor into the neutralization kettle;

[0023] (2) Medium sum, centrifugation: First check the carbonate hydroxine hydroxine hydroxine hydroxine hydroxine hydroxide by 150kg / h in a flow rate of 150 kg / h, and the control material is 100 ° C. When the temperature exceeds 100 ° C, it stops Liquid base, cooling with circulating water to less than 100 ° C, then continuously adding liquid

Example Embodiment

[0025] Example 2

[0026] (1) Synthesis reaction: 37% hydrochloric acid 27% in the reactor is 37%, stirred down; 2-methylimidazole 280 kg is put into 2-methylimidazole at a temperature of 68 ° C; control temperature 98 ° C 160kg; then control temperature 100 ° C The dropped mass fraction was 90% nitric acid 210L, and the dropped speed was 110 kg / h, and the dropwise time was 3 h; the insulation reaction was maintained at 100 ° C; when the temperature was 50 ° C, the medium and kettle was added to the drinking water 1450kg. , Cover the human hole cover, transfer the material in the reactor into the neutralization kettle;

[0027] (2) Medium and Centrifugation: First check the carnoid hydroxine hydroxine hydroxine hydroxine hydroxide by mass of 145 kg / h in a flow rate of 145kg / h, and the control material is added to 98 ° C. When the temperature exceeds 98 ° C, the addition is stopped The liquid base is cooled to 98 ° C or less, then continued to add liquid base to the neutra

Example Embodiment

[0029] Example 3

[0030] (1) Synthesis Reaction: Take a mass fraction of 35% hydrochloric acid in the reaction kettle, turn on stirring; 2-methylimidazole 250kg at a temperature of 70 ° C; control temperature 100 ° C is 0.0 kg of sodium nitrate; then control temperature 120 ° C The dropped mass fraction was 93% nitric acid 210L, the dropwise speed was 104.4 kg / h, and the dropwish is 3 h; the incubation reaction is 28 minutes, and it is maintained at 120 ° C; when the temperature is 50 ° C, when it is 50 ° C, add drinking water in the neutral and kettle. 1400kg, covering the human hole cover, transfer the liquid in the reaction kettle into the neutralization kettle;

[0031](2) Medium sum, centrifugation: First check the carbonate hydroxine hydroxine hydroxine hydroxine hydroxine hydroxide by 150kg / h in a flow rate of 150 kg / h, and the control material is 100 ° C. When the temperature exceeds 100 ° C, it stops The liquid base is cooled to 100 ° C below 100 ° C, then conti

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PUM

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Abstract

The invention discloses a synthesis process of 2-methyl-5-nitroimidazole. The synthesis process comprises the following steps: (1) performing synthesis reaction; (2) neutralizing and centrifuging; (3) drying and packaging; wherein the step (2) also comprises a sodium nitrite recovery process, namely adding the wastewater into a multi-effect evaporation crystallizer to concentrate mother liquor and crystallize sodium nitrate, separating sodium nitrate crystals through a horizontal spiral centrifuge, and drying through an airflow dryer to obtain a sodium nitrate finished product. The liquid caustic soda is used for neutralizing the reaction liquid, the neutralization index is easy to control, so that the process is more suitable for large-scale production, sodium nitrate and hydrochloric acid are used as catalysts for reaction, the consumption of main materials is greatly reduced, concentrated sulfuric acid is not added, and the production cost is lower. A sodium nitrate-hydrochloric acid mixed system is used, redundant nitric acid and hydrochloric acid in the reaction liquid can be removed more easily, the product yield reaches 97.0% or above, and the product content reaches 99.8% or above.

Description

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Claims

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Application Information

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Owner 方耀
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