Preparation method of nicotinic acid

A technology of nicotinic acid and sodium nicotinate, which is applied in the direction of organic chemistry, can solve the problems of high requirements and large corrosion, and achieve the effects of low cost, high conversion rate and convenient operation

Active Publication Date: 2014-05-07
浙江爱迪亚营养科技开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ammonia oxidation and nitric acid oxidation have high requirements on equipment, strong acid oxidants will cause great corrosion to equipment, and produce a large amount of industrial wastewater

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0019] The preparation method of niacin of the present invention comprises the following steps:

[0020] 1. Preparation of raw materials: Take 700-900 parts of 3-cyanopyridine and place in a container, then add 1600-1800 parts of deionized water and 3-cyanopyridine into the container and stir to form a solution;

[0021] 2. Heating the aqueous solution of 3-cyanopyridine to 90-95°C, adding 760-770 parts of 40% sodium hydroxide solution dropwise, and reacting in a container at a temperature of 90-95°C for 58-62 minutes, the 3- Hydrolysis of cyanopyridine generates sodium nicotinate solution; the reaction formula is: C 6 h 4 N 2 +NaOH+H 2 O→C 6 h 4 NO 2 Na+NH 3

[0022] 3. Add 10-12 parts of activated carbon for decolorization to the sodium nicotinate solution, and filter while it is hot, then add deionized water to the filtered filtrate until the concentration of the sodium nicotinate solution is diluted to 15%;

[0023] Four, the 15% sodium nicotinate solution flows t...

Embodiment 1

[0026] Dissolve 800g of 3-cyanopyridine in 1700g of deionized water, heat up to 90°C, add 768g of 40% sodium hydroxide solution dropwise, and the dropping temperature does not exceed 100°C. After adding the lye, continue the heat preservation reaction for 1h. Add 11g gac again in reactor, filter while hot. Add 6000 g of deionized water to the filtrate to adjust the sodium nicotinate solution to a content of 15%.

[0027] Pass the 15% sodium nicotinate solution through the resin layer at a flow rate of 300L / h. After all of it is passed through, use 1 times the resin volume of purified water to pass through the resin at a flow rate of 300L / h, and collect the filtered liquid as nicotinic acid ammonia solution. Niacin is obtained by evaporating the ion-exchanged nicotinic acid ammonium solution to dryness. The product is dried into 890g of white powder. Content: 99.28%. The melting point is 234.1-236°C. The residue on ignition was 0.08%. The molar yield was 94%.

Embodiment 2

[0029] The method is the same as in Example 1, and the resin is the resin used in Example 1. The final product is 898.8g, and the content is 99.45%. The melting point is 234.5-237.2°C. The residue on ignition is 0.05%. The molar yield was 95%.

[0030] Implementation example 3:

[0031] The method is the same as in Example 1, and the resin is the used regenerated resin in Example 1 and Example 2. The final product is 886.5 g, and the content is 99.3%. The melting point is 234.0-236.2°C. The residue on ignition was 0.07%. The molar yield was 93.9%. The method of resin regeneration is as follows: first soak with 4% hydrochloric acid for 4 hours (referring to the unit of hour, that is, English refers to hour, the same below), and then soak with 4% ammonia water for 4 hours to obtain the regenerated resin.

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Abstract

The invention relates to a preparation method of nicotinic acid, which comprises the following steps: placing 700-900 parts of 3-cyanopyridine in a container, adding 1600-1800 parts of de-ionized water into the 3-cyanopyridine in the container, and stirring to obtain a solution; dropwisely adding 760-770 parts of 40% sodium hydroxide solution at 90-95 DEG C, and reacting for 58-62 minutes to generate a sodium nicotinate solution; diluting the solution to 15%; passing the 15% sodium nicotinate solution through an ammonium cation exchange resin layer for ion exchange at a flow rate of 300 liters per hour, collecting to obtain an ammonium nicotinate solution; and evaporating the ammonium nicotinate solution to dryness so as to obtain nicotinic acid. In the invention, 3-cyanopyridine used as the raw material reacts with the sodium hydroxide solution used as hydrolytic agent at a temperature above 90 DEG C for 58-62 minutes to obtain sodium nicotinate. Thus, compared with the prior art, the invention overcomes the defects of high equipment requirements and large equipment corrosion of the original technology, and has the advantages of simpler process, more convenient operation, less waste, lower cost and higher conversion rate.

Description

technical field [0001] The invention relates to the technical field of chemical intermediate synthesis, in particular to a preparation method of nicotinic acid. Background technique [0002] Niacin also known as vitamin B 3 , or vitamin PP, molecular formula: C 6 h 5 NO 2 , heat resistance, can sublimate. Nicotinic acid is also known as nicotinic acid and anti-peaceae factor. In the human body also includes its derivative nicotinamide or nicotinamide. It is one of the 13 kinds of vitamins necessary for the human body. It is a water-soluble vitamin and belongs to the vitamin B group. Nicotinic acid is converted into nicotinamide in the human body. Niacinamide is a component of coenzyme I and coenzyme II, and participates in lipid metabolism in the body, the oxidation process of tissue respiration and the process of anaerobic decomposition of carbohydrates. The product and nicotinamide are collectively referred to as vitamin PP, which is used to resist pellagra, and can...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/80C07D213/803
Inventor 黄上马应国海陈启明
Owner 浙江爱迪亚营养科技开发有限公司
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