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Method of producing nicotinic acid from niacinamide as raw material

A technology of nicotinamide and nicotinic acid, which is applied in the direction of organic chemistry, can solve the problems of excessive NOx, inorganic waste, high production cost, and large energy consumption, and achieve the effects of protecting the environment, saving raw materials, and reducing emissions

Inactive Publication Date: 2019-01-18
ANHUI RUIBANG BIOLOGICAL SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition to the need to add a large amount of additives during the reaction process, the liquid-phase oxidation method also produces more by-products such as NOx and inorganic waste, and consumes a lot of energy during purification, and the production cost is high in large-scale production. Liquid and waste gas all have serious pollution to the environment; for this reason, the present invention proposes a kind of method that is raw material production nicotinic acid with nicotinic acid amine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A method for producing nicotinic acid using nicotinamide as a raw material, the method mainly comprising the following steps:

[0019] (1) Put the nicotinic acid amine solution with a mass concentration of 42% into the stirring container and stir evenly, then evenly add the hydrochloric acid solution with a molar concentration of 0.05mol / L into the nicotinic acid amine solution for acidification, the acidification process is at 500r / min Stir and heat up at a constant speed, evenly heat up to 60°C, detect the pH of the reaction solution and adjust it to 4.5 by continuing to drop hydrochloric acid solution, stop stirring after the reaction solution turns white, and keep warm for 30 minutes;

[0020] (2) Cultivate the above reaction solution at room temperature for 21 hours, then pass through the filter cake and filtrate that have been vacuum filtered and washed, dry and pulverize the filter cake in an oven at 75°C to obtain niacin.

[0021] Wherein, hydrochloric acid solu...

Embodiment 2

[0023] A method for producing nicotinic acid using nicotinamide as a raw material, the method mainly comprising the following steps:

[0024] (1) Put the nicotinic acid amine solution with a mass concentration of 43% into the stirring container and stir evenly, then evenly add the hydrochloric acid solution with a molar concentration of 0.06mol / L into the nicotinic acid amine solution for acidification, the acidification process is at 400r / min Stir and heat up at a constant speed, uniformly heat up to 50°C, detect the pH of the reaction solution and adjust it to 6 by adding hydrochloric acid solution dropwise, stop stirring after the reaction solution turns white, and keep warm for 40 minutes;

[0025] (2) Cultivate the above reaction solution at room temperature for 20 hours, then pass through the filter cake and filtrate that have been vacuum filtered and washed, dry and pulverize the filter cake in an oven at 70°C to obtain niacin.

[0026] Wherein, hydrochloric acid soluti...

Embodiment 3

[0028] A method for producing nicotinic acid using nicotinamide as a raw material, the method mainly comprising the following steps:

[0029] (1) Put the nicotinic acid amine solution with a mass concentration of 44% into the stirring container and stir evenly, then evenly add the hydrochloric acid solution with a molar concentration of 0.03mol / L into the nicotinic acid amine solution for acidification, the acidification process is at 600r / min Stir and heat up at a constant speed, evenly heat up to 65°C, detect the pH of the reaction solution and adjust it to 3.5 by continuing to drop hydrochloric acid solution, stop stirring after the reaction solution turns white, and keep warm for 30 minutes;

[0030] (2) Cultivate the above reaction solution at room temperature for 22 hours, then vacuum filter and wash the filter cake and filtrate, dry and pulverize the filter cake in an oven at 80°C to obtain nicotinic acid.

[0031] Wherein, hydrochloric acid solution is added dropwise t...

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PUM

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Abstract

The invention discloses a method of producing nicotinic acid from niacinamide as a raw material. The method primarily comprises the following steps: inputting a niacinamide solution in a stirring container to be stirred uniformly; then, adding a hydrochloric acid solution uniformly into the niacinamide solution to be acidified; in the acidifying process, stirring and heating the solution at a rotating speed of 400-600 r / min; uniformly heating the solution to 50-60 DEG C; detecting the pH of a reaction solution and continuously dropwise adding the hydrochloric acid solution to adjust the pH to3.5-6; stopping stirring till the reaction solution is white and keeping the temperature for 30-40 minutes; and growing grains of the reaction solution at constant temperature for 20-22 hours, carrying out vacuum filtration to obtain a washed filter cake and a filtrate, and drying and crushing the filter cake in an oven at 70-80 DEG C to obtain nicotinic acid. The method not only saves the reaction raw materials, but also shortens the path and time of producing the nicotinic acid, lowers the production cost and improves the production efficiency; the prepared nicotinic acid has the advantagesof being fine in grain, high in purity and good in crystal form; meanwhile, waste liquor is recycled again, so that the discharge of the waste liquor is reduced, the environment is protected, and theutilization ratio of the raw material is improved.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for producing nicotinic acid by using nicotinamide as a raw material. Background technique [0002] Niacin, also known as pyridine-3-carboxylic acid, is an important water-soluble B vitamin, also known as vitamin B3 or vitamin PP. As an important intermediate, niacin is widely used in the field of medicine, such as the production of inositol niacinate, nicosyl, niacinamide and isoniazid. In addition, nicotinic acid is also widely used in food and feed additives, dye industry, daily chemicals and other fields. The synthesis of nicotinic acid has been widely concerned by the chemical industry. In the current industrial production, nicotinic acid is mainly prepared by oxidation of 3-picoline, and the main methods are divided into liquid phase oxidation method and gas phase oxidation method. In addition to the need to add a large amount of additives during the r...

Claims

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Application Information

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IPC IPC(8): C07D213/80C07D213/803
CPCC07D213/80C07D213/803
Inventor 朱文洁史玉龙王辉沈东升王本超
Owner ANHUI RUIBANG BIOLOGICAL SCI & TECH CO LTD
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