Method for preparing menadione sodium bisulfite continuously in tubular type reactor

A technology of menadione sodium bisulfite and sodium pyrosulfite, which is applied in the field of continuous production of menadione sodium bisulfite using tubular reactors, and can solve the problems of long production auxiliary time, unstable product quality, and low production efficiency, etc. problems, to achieve the effect of large-scale production, easy automation control, and shortened production cycle

Active Publication Date: 2014-11-26
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above-mentioned production method has the following disadvantages: the reaction time is too long, causing a large part of the raw materials to be converted into tar without any use, thereb

Method used

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  • Method for preparing menadione sodium bisulfite continuously in tubular type reactor
  • Method for preparing menadione sodium bisulfite continuously in tubular type reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Make β-menadione and ethanol into β-menadione solution at 75°C, add it to storage tank 1, the mass fraction of β-menadione is 10%, add pre-prepared 75°C solution to storage tank 2 The mass fraction is 35% sodium metabisulfite aqueous solution, and the β-menadione solution and sodium metabisulfite solution preheated to 75°C are continuously pumped into the static mixer 5 at a volume flow ratio of 5.6:1. At this time, the β-menadione The molar ratio of quinone and sodium metabisulfite is 1:0.7, the mixed material enters the tubular reactor 6, the temperature of the reaction liquid is controlled at 75°C, and the reaction residence time is 5 minutes. The material at the outlet of the tubular reactor is cooled by the cooler 7 and put into the crystallization kettle 8, frozen to 0°C, heat-preserved and crystallized for 2 hours, centrifuged, washed with cold ethanol for crystallization, and dried to obtain menadione sodium bisulfite. The rate is 70%.

Embodiment 2

[0024] Make β-menadione and ethanol into β-menadione solution at 75°C, add it to storage tank 1, the mass fraction of β-menadione is 22%, add pre-prepared 75°C solution to storage tank 2 The mass fraction is 35% sodium metabisulfite aqueous solution, and the β-menadione solution and sodium metabisulfite solution preheated to 75°C are respectively continuously pumped into the static mixer 5 at a volume flow ratio of 2.5:1. At this time, the β-menadione The molar ratio of quinone and sodium metabisulfite is 1:0.7, the mixed material enters the tubular reactor 6, the temperature of the reaction liquid is controlled at 75°C, and the reaction residence time is 5 minutes. The material at the outlet of the reactor is cooled by the cooler 7 and put into the crystallization kettle 8, frozen to 0° C., heat-preserved and crystallized for 2 hours, centrifuged, washed with cold ethanol to crystallize, and dried to obtain menadione sodium bisulfite. The yield is 74%.

Embodiment 3

[0026] Mix β-menadione and ethanol into β-menaquinone solution at 75°C, add it to storage tank 1, the mass fraction of β-menadione is 18%, add pre-prepared 75°C solution to storage tank 2 The mass fraction is 25% sodium metabisulfite aqueous solution, and the β-menadione solution and sodium metabisulfite solution preheated to 75 ° C are continuously pumped into the static mixer 5 at a volume flow ratio of 2.2:1. At this time, the β-menadione The molar ratio of quinone and sodium metabisulfite is 1:0.7, the mixed material enters the tubular reactor 6, the temperature of the reaction liquid is controlled at 75°C, and the reaction residence time is 5 minutes. The material at the outlet of the reactor is cooled by the cooler 7 and put into the crystallization kettle 8, frozen to 0° C., heat-preserved and crystallized for 2 hours, centrifuged, washed with cold ethanol to crystallize, and dried to obtain menadione sodium bisulfite. The yield is 66%.

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Abstract

The invention discloses a method for preparing menadione sodium bisulfite continuously in a tubular type reactor. The method comprises the steps of passing a beta-menadione solution and a sodium metabisulfite solution which are preheated to a temperature of 50-80 DEG C through a metering pump respectively; mixing uniformly through a mixer; introducing the mixed materials into the tubular type reactor to carry out a reaction, controlling a temperature of a reaction solution at 50-80 DEG C and a reaction retention time in the tubular type reactor at 1-15 min; crystallizing the material obtained at a reactor outlet by cooling; separating a solid product by centrifugation; washing and drying to obtain menadione sodium bisulfite. The method takes use of the tubular type reactor to produce menadione sodium bisulfite, has a shortened production period, high product yield, stable quality, easily controllable reaction conditions and convenient and safe operations, can be controlled automatically easily, can realize continuous production, and can realize large-scale production only by a few investment in industry.

Description

(1) Technical field [0001] The present invention relates to a kind of vitamin K 3 A production method, especially a method for continuously producing menadione sodium bisulfite using a tubular reactor. (2) Background technology [0002] Sodium menadione sulfate (MSB) is the most commonly used vitamin K 3 , whose molecular formula is C 11 h 8 o 2 ·NaHSO 3 ·3H 2 O, the molecular weight is 330.29, its properties are white to light yellow crystalline powder, bitter taste, no odor or slight odor, easily soluble in water, hardly soluble in ethanol, almost insoluble in ether and benzene, stable at room temperature, easy to absorb Moisture, decomposes when exposed to light, and is irritating to the skin and respiratory tract. As a feed additive, this product is an indispensable nutrient for the growth and development of livestock and poultry. It can effectively prevent and treat hemorrhagic diseases of livestock and poultry, and enhance the ability to resist parasites and coc...

Claims

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Application Information

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IPC IPC(8): C07C309/44C07C303/32
Inventor 施湘君庄玉国陈仁尔
Owner ZHEJIANG UNIV OF TECH
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