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Technique for synthesizing niacinamide and co-producing niacin by hydrolyzing 3-cyanopyridine

A cyanopyridine and nicotinamide technology, applied in organic chemistry and other directions, can solve the problems of easy spoilage, unsafe, affect reaction and product quality, etc., and achieve the effect of simple operation process and small equipment investment.

Active Publication Date: 2009-12-09
NANTONG ACETIC ACID CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0022] The biochemical method is easy to deteriorate due to the bacteria, which will affect the reaction and product quality. The ammonia water method needs to use high-pressure equipment for production and is unsafe.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A process for synthesizing nicotinamide by hydrolysis of 3-cyanopyridine and co-producing nicotinic acid, comprising the following steps:

[0045] (1) Production of nicotinamide:

[0046] In a stirring 500ml three-neck flask, add 80g of 3-cyanopyridine and 160g of deionized water, heat up to 40°C, add 30g of 48% sodium hydroxide at one time, stir, heat up to 50°C, and keep warm 30 minutes, then heat up to 80°C, heat preservation reaction for 6h, end the reaction, cool down, add seed crystals when the temperature drops to 60°C, keep stirring at this temperature for 2 hours, then cool down to 5°C, then filter, and drain the filter cake, Wash with 30g of water, drain, centrifuge the filter cake, and dry to obtain nicotinamide;

[0047] Mother liquor and washing liquid were distilled under negative pressure until the mass concentration of nicotinamide was 20-50%, then cooled, solids were precipitated, and filtered to obtain 77.9 g of nicotinamide, and the total yield of ni...

Embodiment 2

[0051] (1) Production of nicotinamide:

[0052] On the basis of Example 1, the amount of deionized water was reduced to 80g, and the heat preservation reaction temperature was increased to 90°C. Others were the same as in Example 1, and 80.3g of nicotinamide was obtained, and the total yield of nicotinamide was 85.6% (molar yield)

[0053] (2) Production of niacin:

[0054] On the basis of Example 1, add 30% sodium hydroxide, the adjusted pH value is raised to 11, other conditions are the same as Example 1, obtain niacin finished product 12.4g, the yield of niacin is 13.1% (molar yield ).

Embodiment 3

[0056] (1) Production of nicotinamide:

[0057] On the basis of Example 2, the amount of 30% sodium hydroxide used for the reaction is reduced to 15g, the heat preservation reaction temperature is increased to 95°C, the temperature when adding the seed crystal is reduced to 50°C, and the crystal growth time is extended to 4 hours , the amount of water for washing was reduced to 15g, and others were the same as in Example 2 to obtain 84.5g of nicotinamide, and the total yield of nicotinamide was 90.0% (molar yield)

[0058] (2) Production of niacin:

[0059] On the basis of Example 2, the time of the heat preservation reaction was extended to 10 hours, and 30% hydrochloric acid was added to increase the pH value adjusted to 5.0, and the amount of washing water was reduced to 20g. Other conditions were the same as in Example 2, and niacin finished product 8.5 g, the yield of niacin is 9.0% (molar yield).

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PUM

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Abstract

The invention discloses a technique for synthesizing niacinamide and co-producing niacin by hydrolyzing 3-cyanopyridine, comprising the steps of producing niacinamide, producing niacin and the like. The invention has simple technological operation process and little equipment investment and is a niacin and niacinamide co-producing technique, the conversion ratio of 3-cyanopyridine is 100%, the recovery of niacinamide is 90%, and the total recovery of niacin is 99.8%.

Description

Technical field: [0001] The invention relates to a production process of nicotinamide and nicotinic acid. Background technique: [0002] Niacinamide, also known as nicotinamide, nicotinamide, 3-pyridine carboxamide, nicotine amine, vitamin PP [0003] Molecular formula and molecular weight: C6H6N2O=122.13 [0004] Physical and chemical properties: [0005] This product is white crystalline powder, odorless or almost odorless, bitter in taste, soluble in water or ethanol, soluble in glycerin. [0006] Function and use: [0007] Vitamin medicine, which participates in the metabolic process in the body, and is used to prevent and treat niacin deficiency such as pellagra. It is soluble in water and can be synthesized by tryptophan in the human body. It is an indispensable substance for the synthesis of sex hormones. It is effective for seborrheic dermatitis and eczema, has the effect of whitening and activating skin cells, and is widely used in food industry, feed industry,...

Claims

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Application Information

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IPC IPC(8): C07D213/82C07D213/80C07D213/803
Inventor 丁彩峰朱小刚刘芳周新建薛建锋
Owner NANTONG ACETIC ACID CHEM
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