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A method for continuously preparing 2,5-furandicarboxylic acid using a microchannel reaction device

A technology of channel reaction device and microchannel reaction, which is applied in the direction of organic chemistry, can solve the problems of poor selectivity, high requirements for reactor design, high energy consumption, etc., and achieve high yield of reactants and good selectivity of target products , the effect of low reaction temperature

Active Publication Date: 2020-08-07
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The technical problem to be solved in the present invention is to provide a method for continuously preparing 2,5-furandicarboxylic acid using a microchannel reaction device to solve the existing problems in the prior art, such as high requirements for reactor design, poor selectivity, and energy consumption. major issues

Method used

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  • A method for continuously preparing 2,5-furandicarboxylic acid using a microchannel reaction device
  • A method for continuously preparing 2,5-furandicarboxylic acid using a microchannel reaction device
  • A method for continuously preparing 2,5-furandicarboxylic acid using a microchannel reaction device

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Experimental program
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Embodiment 1

[0039]Weigh 0.504g of 5-hydroxymethylfurfural and 0.06g of 2,2,6,6-tetramethylpiperidine-N-oxide and dissolve them in 30mL of water, then add 4 drops of acetic acid dropwise within 1 minute, Stir at room temperature to mix evenly to make homogeneous solvent A and load it in a syringe. Weigh 0.08g of sodium bromide and 2.712g of sodium chlorite and dissolve them in 30mL of water, stir at room temperature to mix evenly to make a homogeneous solution B and load it into a syringe. Weigh 0.021g of sodium hydroxide and dissolve it in 10mL of water, stir at room temperature to make it evenly mixed to make a homogeneous solution C and load it into a syringe. The homogeneous solution A and the homogeneous solution B are pumped into the Y-type mixer at a flow rate of 0.875mL / min respectively, and after mixing, they are passed into the first microreactor with a coil inner diameter of 1mm. The volume of the reactor is 5mL. The temperature is controlled at 30°C, and the reaction residence...

Embodiment 2

[0041] Weigh 0.504g of 5-hydroxymethylfurfural and 0.06g of 2,2,6,6-tetramethylpiperidine-N-oxide and dissolve them in 30mL of water, then add 4 drops of acetic acid dropwise within 1 minute, Stir at room temperature to mix evenly to make a homogeneous solution A and load it in a syringe. Weigh 0.08g of sodium bromide and 2.712g of sodium chlorite and dissolve them in 30mL of water, stir at room temperature to mix evenly to make a homogeneous solution B and load it into a syringe. Weigh 0.021g of sodium hydroxide and dissolve it in 10mL of water, stir at room temperature to make it evenly mixed to make a homogeneous solution C and load it into a syringe. The homogeneous solution A and the homogeneous solution B are pumped into the Y-shaped mixer at a flow rate of 0.438mL / min respectively, and after mixing, they are passed into the first microreactor with a coil inner diameter of 1mm. The volume of the reactor is 10mL. The temperature is controlled at 40°C, and the reaction re...

Embodiment 3

[0043] Weigh 0.504g of 5-hydroxymethylfurfural and 0.06g of 2,2,6,6-tetramethylpiperidine-N-oxide and dissolve them in 30mL of water, then add 4 drops of acetic acid dropwise within 1 minute, Stir at room temperature to mix evenly to make a homogeneous solution A and load it in a syringe. Weigh 0.08g of sodium bromide and 2.712g of sodium chlorite and dissolve them in 30mL of water, stir at room temperature to mix evenly to make a homogeneous solution B and load it into a syringe. Weigh 0.021g of sodium hydroxide and dissolve it in 10mL of water, stir at room temperature to make it evenly mixed to make a homogeneous solution C and load it into a syringe. The homogeneous solution A and the homogeneous solution B are pumped into the Y-shaped mixer at a flow rate of 0.438mL / min respectively, and after mixing, they are passed into the first microreactor with a coil inner diameter of 1mm. The volume of the reactor is 15mL. The temperature is controlled at 50°C, and the reaction re...

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Abstract

The invention discloses a method for continuously preparing 2,5-furandiformic acid by using a microchannel reaction device. The method comprises the following steps that 5-hydroxymethylfurfural and 2,2,6,6-tetramethylpiperidine-N-oxide are dissolved in water, and acetic acid is added dropwise to prepare a homogeneous solution A; sodium bromide and sodium chlorite are dissolved in water to preparea homogeneous solution B; sodium hydroxide is dissolved in water to prepare a homogeneous solution C; the homogeneous solution A and the homogeneous solution B are simultaneously pumped into a first micro-mixer and introduced into a first micro-reactor respectively; the homogeneous solution C and an effluent of the first micro-reactor are simultaneously pumped into a second micro-mixer and introduced into a second micro-reactor respectively, and an effluent is collected to obtain a product. The method for continuously preparing the 2,5-furandiformic acid by using the microchannel reaction device has the advantages that the sodium chlorite is taken as an oxidant, so that the low oxidant price, moderate reaction temperature, higher yield, better target product selectivity and other advantages are provided; the method is simple in operation and low in cost, continuous and uninterrupted production can be achieved, and the industrial application prospect is good.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for continuously preparing 2,5-furandicarboxylic acid by using a microchannel reaction device. Background technique [0002] With the increasing environmental pollution and the decline of fossil fuel reserves, the search for green renewable resources to replace fossil resources has become the focus of human attention. Biomass is a renewable energy source with a wide range of sources and low pollution. The preparation of new platform compounds from biomass to replace fossil resource products has attracted more and more attention. 5-Hydroxymethylfurfural (5-HMF) is a widely used platform compound prepared from biomass conversion. Catalytic oxidation of 5-HMF can produce 2,5-furandicarboxylic acid (FDCA) with high added value compound of. In this way, there is no need to obtain raw materials from petroleum, making full use of abundant biomass resources and r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/68
CPCC07D307/68
Inventor 郭凯蔡谨琳方正张经明张锴欧阳平凯
Owner NANJING TECH UNIV