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Method for producing vitamin K3

A production method and vitamin technology, applied in the preparation of sulfonic acid, organic chemistry and other directions, can solve the problems of product purity only reaching 94%, difficult to recycle, waste of resources, etc., to achieve product yield and quality improvement, product yield Improve and avoid waste

Inactive Publication Date: 2008-08-20
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] 2) The product purity can only reach 94%
[0014] 3) The consumption of ethanol to MSB is as high as 1.5:1
[0015] 4) A large amount of distilled ethanol causes high energy consumption in production, and nearly 8 tons of coal are consumed per ton of MSB
[0016] 5) Nearly 50% of 2-methyl-1,4-naphthoquinone is converted into tar without any use, thus causing environmental pollution
[0017] 6) The residual part of MSB in the reaction mother liquor and the refined mother liquor is difficult to recycle, resulting in a waste of resources

Method used

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  • Method for producing vitamin K3
  • Method for producing vitamin K3

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Experimental program
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Embodiment 1

[0038] Add 500L of solvent water, 250kg of pure 2-methyl-1,4-naphthoquinone, and 225kg of sodium bisulfite into a 1000L reactor, start stirring, raise the temperature to 40-50°C, react for 120 minutes, and feed into the addition crystallization kettle , frozen to below 10°C, incubated for 120 minutes to crystallize, and centrifuged to obtain 390kg of MSB crude wet product. Throw the wet MSB crude product into a 2000L reactor, add 1200L of ethanol, 12kg of activated carbon, and 12kg of sodium bisulfite, heat to 70°C, keep stirring for 30 minutes, filter while it is hot, wash the filter with hot ethanol, and discharge the filtrate and lotion to Refining the crystallization kettle, freezing to below 10°C, insulated for crystallization for 60 minutes, centrifugal separation, washing the crystallization with cold ethanol, centrifugal separation, and drying the crystallization at 50°C to obtain 296kg of MSB product, the yield was 61.7%, and the product purity was greater than or equa...

Embodiment 2

[0040] Put 550L of addition reaction mother liquor, 220kg of 2-methyl-1,4-naphthoquinone, and 195kg of sodium bisulfite into the 1000L reactor, start stirring, raise the temperature to 45°C, react for 120 minutes, and feed until addition The crystallization kettle was frozen to below 10°C, incubated for 120 minutes for crystallization, and centrifuged to obtain 390kg of wet MSB crude product. Throw the wet MSB crude product into a 2000L reactor, add 1200L batch of refined mother liquor, 12kg of activated carbon, and 12kg of sodium bisulfite, heat to 70°C, keep stirring for 30 minutes, filter while it is hot, wash the filter with hot ethanol, discharge the filtrate and Put the washing liquid into a refined crystallization kettle, freeze to below 10°C, insulate and crystallize for 60 minutes, centrifuge, wash the crystals with cold ethanol, centrifuge, and dry the crystals at 50°C to obtain 274kg of MSB product with a yield of 65.0% and a product purity of ≥50% ( Calculated as 2...

Embodiment 3

[0042] Put 255kg of nicotinamide and 215kg of 35% hydrochloric acid into the 2000L reactor, turn on the machine and stir, keep the reaction at 25°C for 30 minutes, put in 700L of MSB addition reaction mother liquor (equivalent to MSB550g), and keep it at 25°C for 120 minutes. Add the material to the crystallization kettle, freeze to below ℃, insulate and crystallize for 120 minutes, centrifuge, wash and crystallize three times, and dry at 50°C to obtain 570kg of MNB with a yield of 91.0% and a product purity of ≥50% (based on 2-methyl-1,4 - Naphthoquinone meter).

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Abstract

The invention relates to a method of synthesizing fiber K3 (menadione sodium bisulfite) in a new solvent system, which comprises the following steps: (1) adding 2-methyl-1, 4-naphthoquinone and sodium bisulfite into the solvent and heating and stirring the solution and carrying out addition reaction; (2) cooling the reactants which goes through the addition reaction to less than 10 DEG C and carrying out centrifugal separation to get an MSB crude product; (3) adding ethanol, activated carbon and the sodium bisulfite into the MSB crude product, heating and dissolving the mixture, carrying out immediate filtration when the mixture is still hot, cooling the filtrate to less than 10 DEG C, and carrying out centrifugal separation, crystallization and drying to obtain an MSB purified product. The method of synthesizing fiber K3 has the advantages of fast reaction, high product yield and good quality; the method avoids the consumption of the ethanol, improves product yield, reduces side products, avoids the waste of resource and improves the purity of the product.

Description

technical field [0001] The present invention relates to a kind of vitamin K 3 method of production, in particular to a method for synthesizing vitamin K in a new solvent system 3 (sodium bisulfite menadione) method. Background technique [0002] 1. Vitamin K 3 Chemical name is sodium menadione sulfate (sodium menadione sulfate, MSB), stable vitamin K 3 It is menadione nicotinamide bisulfite (MNB), which belongs to vitamin drugs and is a biologically active substance. It is mainly used in the field of feed additives, and is also widely used in medicine, cosmetics, health products and industry. MSB is synthesized by addition reaction of 2-methyl-1,4-naphthoquinone with sodium bisulfite. [0003] For a long time, vitamin K 3 In the field of production and scientific research, researchers focus on how to synthesize the intermediate 2-methyl-1,4-naphthoquinone, which is difficult to process, but there are relatively few studies on the above reaction and its matching refining...

Claims

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Application Information

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IPC IPC(8): C07C309/44C07C303/20
Inventor 刘玉王友德
Owner QILU UNIV OF TECH
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