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Preparation method of menadione nicotinamide bisulfite

A technology of menaquinone hydrogen sulfite nicotinamide and naphthoquinone is applied in the field of preparation of menaquinone hydrogen sulfite nicotinamide, and can solve the problems of low recovery rate of tetravalent cerium salt, high electrical energy consumption, expensive electrolysis equipment and the like , to achieve the effect of low cost, easy operation and simple process

Active Publication Date: 2011-01-26
北京颖泰嘉和分析技术有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above method requires expensive electrolysis equipment, high power consumption, and the recovery rate of tetravalent cerium salt prepared from trivalent cerium salt is not high

Method used

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  • Preparation method of menadione nicotinamide bisulfite
  • Preparation method of menadione nicotinamide bisulfite
  • Preparation method of menadione nicotinamide bisulfite

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preparation example Construction

[0015] According to the present invention, in the preparation method of the menadione bisulfite nicotinamide, the trivalent cerium salt contained in the aqueous solution is oxidized, and the method for preparing the tetravalent cerium compound comprises:

[0016] (1) contacting and reacting an aqueous solution containing a trivalent cerium salt with a precipitating agent, and performing solid-liquid separation to obtain a double salt precipitation product of trivalent cerium;

[0017] (2) Precipitate the double salt precipitation product obtained in step (1) and the hydroxide of alkali metal in water, and carry out solid-liquid separation to obtain Ce(OH) 3 ;

[0018] (3) Ce(OH) obtained in step (2) 3 Oxidation to give Ce(OH) 4 .

[0019] The inventors of the present invention have found that in the method of oxidizing the trivalent cerium salt contained in the aqueous solution to prepare the tetravalent cerium compound, since the aqueous solution containing the trivalent c...

Embodiment 1

[0054] This example is used to illustrate the preparation of menadione nicotinamide bisulfite.

[0055] Step (1): the preparation of 2-menaphthoquinone

[0056]Add 730g of cerium sulfate and 3650ml of distilled water to a 5000ml four-necked bottle successively, slowly add 540g of concentrated sulfuric acid (98% by mass) under stirring, then raise the temperature to 60°C, keep the temperature at 60±5°C and dropwise add 32g of 2 - 190g of cyclohexane solution of methylnaphthalene, added in about 10 minutes, after 50 minutes of heat preservation, liquid separation was carried out, and the separated aqueous phase containing trivalent cerium salt (about 3000mL containing 0.2mol / L trivalent cerium ion ) to recover tetravalent cerium salt. Cool the separated oil phase to 5±2°C and keep it warm for 3 hours. After the solids are fully separated, filter, wash the filter cake twice with 50ml×2 cold cyclohexane, filter, and dry at 45°C for 2 hours. 21.6 g of solids were obtained. Accord...

Embodiment 2

[0070] This example is used to illustrate the preparation of menadione nicotinamide hydrogen sulfite.

[0071] Prepare menadione nicotinamide bisulfite according to the method in Example 1, except that in step 4, add 3000 mL of an aqueous solution containing 0.2 mol / L trivalent cerium ions into a 5000 mL flask, start stirring, and heat to 80 °C , slowly add 0.45 moles of ammonium nitrate to the above solution, and keep warm at 95°C for 3.5 hours; filter while hot, and wash the filter cake twice with hot water until the pH value of the washing water is 7-8.

[0072] Transfer the filter cake into a 2000mL flask, add 1000mL of water, stir to adjust the slurry, add 170g of sodium hydroxide while stirring, and heat up to 80°C for 5 hours. The above mixture was filtered, and the filter cake was washed with water at 80°C until the pH of the washing water was 7-8.

[0073] Put the filter cake in a hot air drying oven, dry it at 100°C, take it out and grind it, pass hot air at 120°C f...

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Abstract

The invention discloses a preparation method of menadione nicotinamide bisulfate, comprising the steps of: reacting2-methylnaphthalene with an aqueous solution of an oxidant quadrivalent cerium salt and carrying out oil-water separation on the obtained reaction product to obtain an oil phase including 2-methyl-1,4-naphthoquinone and 6-methyl-1,4-naphthoquinone as well as an aqueous solution including cerous salt; preparing the menadione nicotinamide bisulfate from the 2-methyl-1,4-naphthoquinone in the oil phase and oxidizing the cerous salt included in the aqueous solution to obtain a quadrivalent cerium compound, wherein the method for oxidizing the cerous salt included in the aqueous solution to obtain the quadrivalent cerium compound comprises the steps of: (1) carrying out contact reaction on the aqueous solution including the cerous salt and a precipitant, and carrying solid-liquid separation to obtain a composite salt precipitate; (2) carrying out precipitation reaction on the obtained composite salt precipitate and the hydroxide of alkali metal in the water, and carrying solid-liquid separation to obtain Ce(OH)3; and (3) oxidizing the Ce(OH)3 obtained in the step (2) to obtain Ce(OH)4. The yield of the quadrivalent cerium compound obtained via the method provided by the invention is higher.

Description

technical field [0001] The invention relates to a preparation method of menadione bisulfite nicotinamide. Background technique [0002] Menadione nicotinamide bisulfite (MNB) is a vitamin K 3 (Stabilized salt of menadione sodium bisulfite (MSB)), its structural formula is as follows: [0003] [0004] By reacting 2-methyl-1,4-naphthoquinone with sodium bisulfite to generate sodium bisulfite menadione (MSB), and form a stable salt (MNB) with nicotinamide, its water solubility can be improved, Moreover, it is stable against light, heat, moisture, etc., and is not easy to decompose. [0005] Menadione nicotinamide bisulfite (MNB) is widely used as a feed additive because of its hemostatic, growth-promoting, and antispasmodic effects. In addition, EP 1479295 reported that MNB can kill microscopic organisms or inhibit their growth, and can be used in ships' ballast water to kill infected aquatic organisms or inhibit their growth. MNB can also be used to control phytoplankt...

Claims

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Application Information

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IPC IPC(8): C01F17/00C07D213/82
Inventor 刘世禄母灿先王文军张永忠李俊卿张政谭徐林魏泱黄希
Owner 北京颖泰嘉和分析技术有限公司
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