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Method for producing nicotinic acid by using nicotinamide mother solution

A technology using nicotinamide mother and nicotinamide mother, which is applied in the direction of organic chemistry, can solve the problems of high impurity content of nicotinamide, poor quality of nicotinamide, quantity loss, etc., and achieve maximum benefit, simplified production process, energy consumption reduction effect

Inactive Publication Date: 2015-04-29
TIANJIN HANDEWEI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even if the mother liquor is recovered, the quality of the obtained nicotinamide is also very poor, and there will be a large amount of quantity loss in the recovery
In this process, the impurities in the mother liquor are also concentrated, and most of them are mixed in the recovered nicotinamide after centrifugation and filtration, and cannot be removed, so that the recovered nicotinamide contains high impurities and poor quality; Due to the high water solubility of nicotinamide, the discarded mother liquor after rejection filtration also contains a lot of nicotinamide, resulting in a certain amount of material loss

Method used

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  • Method for producing nicotinic acid by using nicotinamide mother solution
  • Method for producing nicotinic acid by using nicotinamide mother solution
  • Method for producing nicotinic acid by using nicotinamide mother solution

Examples

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Embodiment 1

[0032] A method for producing nicotinic acid using nicotinamide mother liquor, comprising the following preparation steps,

[0033] 1), hydrolysis reaction

[0034] Weigh 450g of nicotinamide mother liquor, wherein the mass concentration of nicotinamide in nicotinamide mother liquor is 28.0%, put nicotinamide mother liquor and caustic soda into a four-necked bottle, and then use a graduated cylinder to measure a certain amount of purified water into the four-necked bottle, The mass ratio of nicotinamide, sodium hydroxide and purified water in the four-necked bottle is 1:0.80:4; start stirring and start heating, when the temperature rises to 108°C, start timing, the temperature is controlled at 108-115°C, and the reaction time For 3 hours, during the hydrolysis reaction, add an appropriate amount of purified water to ensure that the volume of the liquid in the four-necked bottle does not change, and obtain 3-pyridine-sodium formate after the hydrolysis reaction;

[0035] 2), d...

Embodiment 2

[0045] A method for producing nicotinic acid using nicotinamide mother liquor, comprising the following preparation steps,

[0046] 1), hydrolysis reaction

[0047] Weigh 450g of nicotinamide mother liquor, wherein the mass concentration of nicotinamide in nicotinamide mother liquor is 28.0%, put nicotinamide mother liquor and caustic soda into a four-necked bottle, and then use a graduated cylinder to measure a certain amount of purified water and drag it into the four-necked bottle , the mass ratio of nicotinamide, sodium hydroxide and purified water in the four-necked bottle is 1:0.6:4; start stirring and start heating, when the temperature rises to 105°C, start timing, control the temperature at 105-112°C, and react The time is 2.5 to 3.5 hours. During the hydrolysis reaction, add an appropriate amount of purified water to ensure that the volume of the liquid in the four-necked bottle does not change. After the hydrolysis reaction, 3-pyridine-sodium formate is obtained;

...

Embodiment 3

[0059] A method for producing nicotinic acid using nicotinamide mother liquor, comprising the following preparation steps,

[0060] 1), hydrolysis reaction

[0061] Weigh 450g of nicotinamide mother liquor, wherein the mass concentration of nicotinamide in nicotinamide mother liquor is 28.0%, put nicotinamide mother liquor and caustic soda into a four-necked bottle, and then use a graduated cylinder to measure a certain amount of purified water and drag it into the four-necked bottle , the mass ratio of nicotinamide, sodium hydroxide and purified water in the four-necked bottle is 1:0.40:4; start stirring and start heating, when the temperature rises to 102°C, start timing, control the temperature at 102-108°C, and react The time is 3 hours. During the hydrolysis reaction, an appropriate amount of purified water is added to ensure that the volume of the liquid in the four-necked bottle does not change, and 3-pyridine-sodium formate is obtained after the hydrolysis reaction;

...

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Abstract

The invention provides a method for producing nicotinic acid by using a nicotinamide mother solution, which comprises the following steps: hydrolysis reaction: adding the nicotinamide mother solution and caustic soda flakes into a four-neck flask, measuring a certain amount of purified water by using a measuring cylinder, and adding into the four-neck flask, wherein the mass ratio of the nicotinamide, sodium hydroxide and purified water in the four-neck flask is 1:(0.39-0.80):(2-4); starting stirring and heating, starting timing when the temperature rises to 90-115 DEG C, and reacting for 2.5-3.5 hours while controlling the temperature at 90-115 DEG C, wherein a right amount of purified water is supplemented in the hydrolysis reaction process; after the hydrolysis reaction finishes, obtaining sodium 3-pyridyl-formate; and decolorizing, crystallizing, separating, drying and the like to obtain the nicotinic acid finished product. The method provides a powerful technical support for mother solution treatment in the nicotinamide technique, maximizes the benefits of the nicotinamide and nicotinic acid product, minimizes the discharge, and solves the problem of reuse of the nicotinamide mother solution, thereby enhancing the nicotinamide quality.

Description

technical field [0001] The invention relates to the technical field of production of nicotinic acid, in particular to a method for producing nicotinic acid by using nicotinamide mother liquor. Background technique [0002] Nicotinic acid is also called vitamin B3 or 3-pyridine-carboxylic acid, and niacinamide is also called 3-pyridine-carboxamide. Niacin and niacinamide are collectively called vitamin PP, which is one of the 13 essential vitamins for the human body. Niacin is converted to niacinamide in the body. Niacin and nicotinamide are used as feed additives for livestock and poultry after compounding with choline or choline chloride. Niacinamide and niacin are also widely used as food additives to enhance the nutritional value of foods. Pharmaceutical grades of niacin and niacinamide are also used in human vitamin tablets. [0003] No matter which process is used, the main raw material for the production of most nicotinamide and nicotinic acid is 3-cyanopyridine. T...

Claims

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Application Information

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IPC IPC(8): C07D213/80C07D213/803
CPCC07D213/803C07D213/80
Inventor 王立峰
Owner TIANJIN HANDEWEI PHARMA
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