Vitamin K3 synthesis method and device

A synthesis method and vitamin technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of sulfonates, etc., can solve the problems of low product recovery rate, poor MNB stability, prolonged reaction time, etc.

Pending Publication Date: 2021-05-11
BROTHER ENTERPRISES HLDG CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The synthesis of MSB needs to be completed in a certain water phase system, but due to the considerable solubility of MSB in water, the recovery rate of MSB products is low, and the amount of ethanol in the synthesis system is not enough to completely dissolve β-menaquinone, and partial synthesis The reaction is a solid-liquid reaction, so that the reaction time is prolonged, the by-products increase, and the MSB conversion rate decreases
However, the solubility of MNB in ​​water is low, and there is ethanol in the reaction system, which will cause the precipitation of inorga...

Method used

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  • Vitamin K3 synthesis method and device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A kind of synthetic method of vitamin K3, the concrete steps of this method are:

[0043] Preparation of S1, intermediate β-menadione

[0044] 1. β-methylnaphthalene, sulfuric acid, sodium dichromate, and water continuously enter the jet flow continuous oxidation reactor, the flow rate of β-methylnaphthalene is 30kg / h, the flow rate of sulfuric acid is 240kg / h, and the feeding amount of sodium dichromate is 300kg / h, the batching water flow rate is 200kg / h, the temperature of the reaction solution is controlled at 50±1°C, and the residence time is 10h to obtain the oxidation reaction solution of β-menadione.

[0045] In the initial reaction system, the concentration of each substance is: β-methylnaphthalene 68.6g / L, sulfuric acid 549g / L, sodium dichromate 686.3g / L.

[0046] 2. The oxidation reaction solution obtained in the previous step is continuously filtered into the filter and washed with water, and the washing water volume is 400kg / h;

[0047] 3. ...

Embodiment 2

[0059] A method for synthesizing vitamin K3 is based on Example 1, reducing the residence time of the oxidation reaction and reducing the reaction temperature; after the MSB reaction solution is used to prepare MSB, co-production is still used to prepare MNB.

[0060] Preparation of S1, intermediate β-menadione

[0061] 1. β-methylnaphthalene, sulfuric acid, sodium dichromate, and water continuously enter the jet flow continuous oxidation reactor, the flow rate of β-methylnaphthalene is 150kg / h, the flow rate of sulfuric acid is 1200kg / h, and the feeding amount of sodium dichromate is 1400kg / h, the batching water flow rate is 700kg / h, the temperature of the reaction solution is controlled at 35±1°C, and the residence time is 2h.

[0062] In the initial reaction system, the concentration of each substance is: β-methylnaphthalene 71.7g / L, sulfuric acid 573.9g / L, sodium dichromate 669.6g / L.

[0063] 2. The oxidation reaction solution obtained in the previous step i...

Embodiment 3

[0076] A method for synthesizing vitamin K3 is based on Example 1, reducing the residence time of the oxidation reaction and increasing the reaction temperature; the MSB reaction solution is divided by 50% to prepare MSB and then co-produced to prepare MNB.

[0077] Preparation of S1, intermediate β-menadione

[0078] 1. β-methylnaphthalene, sulfuric acid, sodium dichromate, and water continuously enter the jet flow continuous oxidation reactor, the flow rate of β-methylnaphthalene is 100kg / h, the flow rate of sulfuric acid is 800kg / h, and the feeding amount of sodium dichromate is 900kg / h, the batching water flow rate is 3000kg / h, the temperature of the reaction solution is controlled at 65±1°C, and the residence time is 1.5h.

[0079] In the initial reaction system, the concentration of each substance is: β-methylnaphthalene 34.4g / L, sulfuric acid 275g / L, sodium dichromate 309.4g / L.

[0080] 2. The oxidation reaction solution obtained in the previous step is c...

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Abstract

The invention relates to a vitamin synthesis method, in particular to a vitamin K3 synthesis method and device, and belongs to the technical field of chemical synthesis. The vitamin K3 synthesis method mainly comprises the following two steps: S1, preparing an intermediate beta-menadione; and S2, adopting co-production to synthesize menadione sodium bisulfite (MSB) and menadione nicotinamide bisulfite (MNB), namely, based on the different water solubility of MSB and MNB, firstly performing sulfonation reaction synthesis and crystallization on the intermediate beta-menadione to obtain MSB, and then performing condensation synthesis on MSB mother liquor to obtain MNB. The method comprises preparation of a key intermediate beta-menadione and synthesis of MSB (menadione sodium bisulfite) and MNB (menadione nicotinamide bisulfite), a co-production process is adopted, namely, based on the different water solubility of MSB and MNB, synthesizing and crystallizing are carried out to obtain MSB, and then MNB is synthesized by utilizing mother liquor.

Description

technical field [0001] The invention relates to a vitamin synthesis method, in particular to a vitamin K3 synthesis method and device, and belongs to the technical field of chemical synthesis. Background technique [0002] Vitamin K3, Chinese name: menadione, menadione sodium bisulfite (MSB) and nicotinamide menadione bisulfite (MNB). Vitamin K3 is a vitamin nutritional supplement, which belongs to procoagulant drugs, and can be used to treat hemorrhagic diseases caused by vitamin K deficiency, such as neonatal hemorrhage, vitamin K deficiency and hypoprothrombinemia caused by intestinal malabsorption Wait. [0003] The domestic production of menadione sodium bisulfite (MSB) and menadione nicotinamide hydrogen sulfite (MNB) generally adopts an independent production system, that is, the production of MSB products is based on the batch reaction of β-methylnaphthalene as raw material to prepare β- Menadione, and then use β-menaquinone to prepare MSB reaction solution in sodi...

Claims

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Application Information

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IPC IPC(8): C07C46/04C07C46/10C07C50/12C07C303/32C07C303/44C07C309/44C07C303/26C07C309/74C07D213/82B01J19/26
CPCC07C46/04C07C46/10C07C303/32C07C303/44C07C303/26C07D213/82B01J19/26C07C2602/10C07C50/12C07C309/44C07C309/74
Inventor 潘炎烽钱卫新顾益平胡泽清周中平
Owner BROTHER ENTERPRISES HLDG CO LTD
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