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A kind of method for tubular continuous preparation of β-menadione

A menadione, tubular technology, applied in the field of continuous production of β-menaquinone by using tubular reactors, can solve the problems of unstable quality between batches, large amount of one-time input material, difficult temperature control, etc. Achieve the effects of easy control, high production continuity and simple operation

Active Publication Date: 2018-03-20
SICHUAN YINHE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Menaquinone synthesis technology currently adopts the production process of kettle-type intermittent oxidation of methylnaphthalene. Due to the large amount of one-time input material, the violent oxidation reaction and the release of a large amount of heat during the intermittent feeding process, it is difficult to control the temperature during the reaction process, resulting in The product yield is low, the quality between batches is unstable, and there is a serious waste of oxidation solution

Method used

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  • A kind of method for tubular continuous preparation of β-menadione

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Experimental program
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Effect test

Embodiment 1

[0034] At a temperature of 35°C, add β-methylnaphthalene, an emulsifier and water into the β-methylnaphthalene emulsion storage tank 1 to prepare a β-methylnaphthalene emulsion, wherein the obtained β-methylnaphthalene emulsion contains β - the massfraction of methylnaphthalene is 16%, adds oxidation solution in the storage tank of oxidation solution, 300g / L of red alum sodium concentration in the oxidation solution, acid value is that the concentration of acid is 500g / L with sulfuric acid, and β-methylnaphthalene The emulsion and the oxidation liquid pass through the first metering pump 3 and the second metering pump 4 respectively and are measured according to the volume ratio of β-methylnaphthalene emulsion: oxidation liquid at a ratio of 1:2.3, and then enter the tubular reactor 7 with an ultrasonic device To carry out the reaction, the reaction temperature is controlled at 45-55°C by a constant temperature water bath device, and the residence time in the tubular reactor is...

Embodiment 2

[0036] At a temperature of 35°C, add β-methylnaphthalene, an emulsifier and water into the β-methylnaphthalene emulsion storage tank 1 to prepare a β-methylnaphthalene emulsion, wherein the obtained β-methylnaphthalene emulsion contains β - the massfraction of methylnaphthalene is 18%, adds oxidation solution in the storage tank of oxidation solution, 300g / L of red alum sodium concentration in the oxidation solution, acid value is that the concentration of acid is 500g / L with sulfuric acid, and β-methylnaphthalene The emulsion and the oxidizing liquid pass through the first metering pump 3 and the second metering pump 4 respectively and are measured according to the volume ratio of β-methylnaphthalene emulsion: oxidizing liquid at a ratio of 1:2.0, and then enter the tubular reactor 7 with an ultrasonic device To carry out the reaction, the reaction temperature is controlled at 40-60°C by a constant temperature water bath device, and the residence time in the tubular reactor is...

Embodiment 3

[0038]At a temperature of 35°C, add β-methylnaphthalene, an emulsifier and water into the β-methylnaphthalene emulsion storage tank 1 to prepare a β-methylnaphthalene emulsion, wherein the obtained β-methylnaphthalene emulsion contains β - the massfraction of methylnaphthalene is 16%, adds oxidation solution in the storage tank of oxidation solution, 350g / L of red alum sodium concentration in the oxidation solution, acid value is that the concentration of acid is 550g / L with sulfuric acid, and β-methylnaphthalene The emulsion and the oxidizing liquid pass through the first metering pump 3 and the second metering pump 4 respectively and are measured according to the volume ratio of β-methylnaphthalene emulsion: oxidizing liquid at a ratio of 1:2.5, and then enter the tubular reactor 7 with an ultrasonic device To carry out the reaction, the reaction temperature is controlled at 48-52°C by a constant temperature water bath device, and the residence time in the tubular reactor is ...

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Abstract

The invention discloses a tubular continuous method for preparing beta-menadione, which comprises the following steps: preparing a beta-methylnaphthalene emulsion, heating the beta-methylnaphthalene emulsion, metering the beta-methylnaphthalene emulsion and an oxidation solution respectively by a measuring pump, adding into a tubular reactor provided with an ultrasonic generator, and carrying out ultrasonic reaction, wherein the retention time of the reactants in the tubular reactor is 1-300 minutes; supplementing dilute sulfuric acid to the outlet of the tubular reactor, adding into a curing tank, and curing for 1-10 hours while keeping the temperature; after finishing curing, filtering, washing, carrying out centrifugal dehydration and drying to obtain the beta-menadione finished product. By using the tubular reactor to produce the beta-menadione, the method has the advantages of high production continuity and short period; and the product has the advantages of high yield, low impurity content and stable quality. The reaction process is easy to control, simple to operate and high in automatic control degree; the material performs forced flow in the tubular reactor to substitute mechanical stirring, thereby implementing industrialized continuous production; and thus, the method has the characteristics of low input cost and short reconstruction period, and can perform large-scale industrial production.

Description

technical field [0001] The invention relates to a production method of β-menadione, in particular to a method for continuously producing β-menaquinone by using a tubular reactor. Background technique [0002] Menaquinone synthesis technology currently adopts the production process of kettle-type intermittent oxidation of methylnaphthalene. Due to the large amount of one-time input material, the violent oxidation reaction and the release of a large amount of heat during the intermittent feeding process, it is difficult to control the temperature during the reaction process, resulting in The product yield is low, the quality between batches is unstable, and there is a serious waste of oxidation solution. [0003] Continuously add the methylnaphthalene emulsion and the oxidized liquid flow into the water bath to keep the temperature at a certain ratio, and improve the quality and yield of naphthoquinone by controlling the temperature of the water bath, the pre-reaction time of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C50/10C07C46/04
CPCC07C46/04C07C50/10
Inventor 李先荣陈宁董明甫王方兵谢友才向林
Owner SICHUAN YINHE CHEM
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