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Method for producing vitamin K3

A production method and vitamin technology, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of product purity only reaching 94%, difficult to recycle, environmental pollution, etc., to achieve product yield and quality improvement, product yield The effect of improving and shortening the reaction time

Inactive Publication Date: 2010-07-28
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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
  • Method for producing vitamin K3

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Put 500L of solvent water, 250kg of 2-methyl-1,4-naphthoquinone, 225kg of sodium bisulfite into the 1000L reactor, start stirring, heat up to 40~50℃, react for 120 minutes, add to the addition crystallization kettle , Freeze to below 10℃, keep for 120 minutes to crystallize, and centrifuge to obtain 390kg of crude MSB wet product. Put the crude MSB wet product into a 2000L reactor, add 1200L ethanol, 12kg activated carbon, 12kg sodium bisulfite, heat to 70°C, keep stirring for 30 minutes, filter while hot, wash the filter with hot ethanol, discharge the filtrate and washing liquid to Refining the crystallization kettle, freezing to below 10°C, keeping the temperature for crystallization for 60 minutes, centrifuging, washing the crystals with cold ethanol, centrifuging, and drying the crystals at 50°C to obtain 296kg MSB product, with a yield of 61.7%, and product purity ≥50% (with 2- Methyl-1,4-naphthoquinone).

Embodiment 2

[0040] Put 550L of addition reaction mother liquor in the 1000L reactor, 220kg of 2-methyl-1,4-naphthoquinone, 195kg of sodium bisulfite, start stirring, heat up to 45℃, react for 120 minutes, and add to the addition The crystallization kettle was frozen to below 10°C, kept for 120 minutes for crystallization, and centrifuged to obtain 390 kg of crude MSB wet product. Put the crude MSB wet product into a 2000L reactor, add 1200L of batch refined mother liquor, 12kg of activated carbon, 12kg of sodium bisulfite, heat to 70℃, keep warm and stir for 30 minutes, filter while hot, wash the filter with hot ethanol, and drain the filtrate and Wash the lotion to the refined crystallization kettle, freeze to below 10°C, keep for 60 minutes to crystallize, 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 product purity ≥50% ( Based on 2-methyl-1,4-naphthoquinone).

Embodiment 3

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

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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 vitamin K 3 Production method, especially involving the synthesis of vitamin K in a new solvent system 3 (Menadione sodium bisulfite) method. Background technique [0002] 1. Vitamin K 3 The chemical name is sodium menadione sulfate (MSB), stable vitamin K 3 It is menadione nicotinamide bisulfite (MNB), a vitamin drug, and a biologically active substance. It is mainly used in the field of feed additives, and has a wide range of applications in medicine, cosmetics, health products and industry. MSB is synthesized using 2-methyl-1,4-naphthoquinone as a raw material and an addition reaction with sodium bisulfite. [0003] For a long time, in vitamin K 3 In the field of production and scientific research, researchers are concerned about how to synthesize the difficult intermediate 2-methyl-1,4-naphthoquinone, but there are relatively few studies on the above-mentioned reaction and the matching purification process. So far, the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/44C07C303/20
Inventor 刘玉王友德
Owner QILU UNIV OF TECH