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Method for preparing furoic acid by oxidizing furfural on micro-channel reactor

A micro-channel reactor, furfural technology, applied in chemical instruments and methods, chemical/physical/physical chemical reactors, organic chemistry, etc., can solve the problems of low mixing efficiency of materials, difficult control of thermal energy, side reactions, etc. Yield, reduced by-products, reduced side-reaction effects

Active Publication Date: 2020-02-28
浙江清和新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method still has the problems of low material mixing efficiency, difficult control of heat energy in the exothermic reaction, easy side reactions, and low yield.

Method used

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  • Method for preparing furoic acid by oxidizing furfural on micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The specific preparation process of the capillary in the microchannel reactor is as follows:

[0025] (1) Al 2 o 3 Heat the superfine powder at 300°C for 2 hours, add 1,3-propanediol to make a suspension, ultrasonicate the suspension for 1 hour to make the dispersion uniform, and remove the dissolved air, and inject the suspension into the quartz capillary;

[0026] (2) Turn on nitrogen, flow through the whole capillary with low-speed nitrogen, pass the liquid plug formed by the suspension in the capillary through the whole capillary, and then pass low-speed nitrogen for 4 hours to remove the suspension, and then heat to 200°C to remove the solvent;

[0027] (3) Repeat the above steps 3 times;

[0028] (4) Dissolve 5.0 g of copper nitrate in 8-10 mL of distilled water, stir to dissolve, and immerse the capillary loaded with alumina particles in the copper nitrate solution for 10 h;

[0029] (5) Take out the capillary, dry it in an oven at 110 °C for 10 h, and finally...

Embodiment 2

[0031] (1) 48.3 g furfural and an equimolar amount of NaOH solution, the concentration of NaOH solution is 1.0 mol / L, are transported into the microchannel reactor by a plunger pump, and the air is fed at a space velocity of 1000 h -1 Pass into the microchannel reactor, control the reaction temperature to 40°C, and the reaction residence time to 10min, and obtain the reaction liquid from the outlet of the reactor.

[0032] The above-mentioned microchannel reactor is composed of 30 capillary tubes with an inner diameter of 0.32 mm and a length of 10 cm obtained in Example 1, which are divided into an inlet section and an outlet section, and are fixed by connecting screws. The two ends of the capillary are respectively packaged in the inlet section and the outlet section by the packaging board, and the two packaging boards are respectively provided with at least one heating hole and a measurement and control thermocouple socket.

[0033] (2) Control the temperature of the reacti...

Embodiment 3

[0036] (1) 38.3 g furfural and an equimolar amount of NaOH solution, the concentration of NaOH solution is 1.0 mol / L, are transported into the microchannel reactor by a plunger pump, and the air is fed at a space velocity of 3000 h -1 Pass it into a microchannel reactor, control the reaction temperature at 45°C, and the reaction residence time for 5 min, and obtain the reaction liquid from the outlet of the reactor.

[0037] The above-mentioned microchannel reactor is composed of 30 capillary tubes with an inner diameter of 0.32 mm and a length of 10 cm obtained in Example 1, which are divided into an inlet section and an outlet section, and are fixed by connecting screws. The two ends of the capillary are respectively packaged in the inlet section and the outlet section by the packaging board, and the two packaging boards are respectively provided with at least one heating hole and a measurement and control thermocouple socket.

[0038] (2) Control the temperature of the reac...

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Abstract

The invention relates to a method for preparing furoic acid by oxidizing furfural on a micro-channel reactor. The method comprises the following steps: (1) conveying furfural and a NaOH solution intoa micro-channel reactor by a plunger pump, introducing air into the micro-channel reactor, and obtaining a reaction solution from the outlet of the reactor; (2) performing acidification, crystal growing, filtering and ice water leaching to obtain a furoic acid wet product; and (3) performing vacuum drying to obtain solid furoic acid. According to the invention, by utilizing the micro-channel reactor, the reaction heat can be well controlled, the continuous production of furoic acid is realized, the reaction speed is high, the residence time is short, the purity of the prepared furoic acid is more than 99.5%, and the yield is more than 97.6%.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a method for preparing furoic acid by oxidizing furfural in a microchannel reactor. Background technique [0002] Furoic acid, also known as 2-furoic acid or 2-furancarboxylic acid, is a white monoclinic long fusiform crystal, which can be used as an important industrial raw material for synthetic resins, drugs, and insecticides. Furoic acid is usually prepared by oxidation of furfural, and the main methods include Cannizzaro method, chemical oxidation method and catalytic oxidation method. [0003] Under the action of a strong base, the Cannizzaro method undergoes an intermolecular oxidation-reduction reaction, the yield of which is no more than 50%, and generates a large amount of by-product furfuryl alcohol, which is difficult to separate and industrialize; It is reduced during the process and cannot be regenerated, and if the oxidant is not quenched after the reaction, there is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/68B01J19/00
CPCB01J19/0093C07D307/68
Inventor 林桂海徐铁勇符建琼王建王杰
Owner 浙江清和新材料科技有限公司
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