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Method for preparing 2,5-furandicarboxylic acid by one-step cleaning

A furandicarboxylic acid, clean technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, organic chemistry, etc., can solve the problem of high price, high production cost of 2,5-furandialdehyde, HMF separation difficulties and other problems, to achieve the effect of easy transportation, reduce production costs and the difficulty of separation and purification, and improve catalytic efficiency

Active Publication Date: 2019-09-20
GUANGXI ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The production cost of 2,5-furandicarbaldehyde is very high based on the difficulty of separating the raw material HMF and the high price

Method used

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  • Method for preparing 2,5-furandicarboxylic acid by one-step cleaning
  • Method for preparing 2,5-furandicarboxylic acid by one-step cleaning
  • Method for preparing 2,5-furandicarboxylic acid by one-step cleaning

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] One-step cleaning method for preparing 2,5-furandicarboxylic acid, comprising the following steps:

[0048] Mix 8g of fructose, 0.5g of sodium carbonate-zinc glutarate with a mass ratio of 2:1, 0.45g of ruthenium lanthanum niobate catalyst, and 100g of hydrogen peroxide and 1,3-dimethyl- The mixed solvent composed of 2-imidazolinone solution and dimethyl carbonate is poured into the high-pressure reaction kettle, quickly sealed and stirred at a speed of 300r / min, and the volume ratio of 1:2.5 is introduced into the CO 2 / O 2 Mix the gas until the pressure in the autoclave is 8MPa, then heat it to 195°C, stop the reaction after 25 minutes of reaction, take 1mL of the reaction solution from the sampling tube and analyze the product by high performance liquid chromatography, and the following results are obtained: the fructose conversion rate is 98.78%, and the yield of 2,5-furandicarboxylic acid was 50.53%.

Embodiment 2

[0050] One-step cleaning method for preparing 2,5-furandicarboxylic acid, comprising the following steps:

[0051] Mix 15g of sucrose, 0.5g of sodium carbonate-zinc glutarate with a mass ratio of 4:1, 0.40g of ruthenium lanthanum niobate catalyst, and 100g of hydrogen peroxide and 1,3-dimethyl- The mixed solvent composed of 2-imidazolinone solution and dimethyl carbonate is poured into the high-pressure reaction kettle, and it is quickly sealed and stirred at a speed of 300r / min, and CO with a volume ratio of 1:3 is introduced. 2 / O 2 Mix the gas until the pressure in the autoclave is 6MPa, then heat it to 191°C, stop the reaction after 45 minutes of reaction, take 1mL of the reaction solution from the sampling tube and analyze the product with high performance liquid chromatography, and the following results are obtained: the conversion rate of sucrose is 94.38%, 2,5-furandicarboxylic acid yield was 20.21%.

Embodiment 3

[0053] One-step cleaning method for preparing 2,5-furandicarboxylic acid, comprising the following steps:

[0054] Mix 9g of glucose, 0.5g of sodium carbonate-zinc glutarate with a mass ratio of 1:1, 0.35g of ruthenium-based lanthanum niobate catalyst, and 100g of hydrogen peroxide and 1,3-dimethyl- The mixed solvent composed of 2-imidazolinone solution and dimethyl carbonate is poured into the high-pressure reaction kettle, and it is quickly sealed and stirred evenly at a speed of 300r / min, and CO with a volume ratio of 1:1 is introduced. 2 / O 2 Mix the gas until the pressure in the autoclave is 7.2 MPa, then heat it to 190°C, stop the reaction after 35 minutes of reaction, take 1mL of the reaction solution from the sampling tube and analyze the product by high performance liquid chromatography, and the following results are obtained: Glucose The conversion rate was 88.83%, and the yield of 2,5-furandicarboxylic acid was 30.24%.

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Abstract

The invention disclose a method for preparing 2,5-furandicarboxylic acid by one-step cleaning by using saccharide compounds as raw materials. The method concretely is to add the saccharide compounds, a catalyst and a reaction solvent into a high-pressure reaction vessel, stir the materials to form an uniform solution, and introduce CO2 / O2 mixed gas to the system until the pressure reaches 6-8 MPa for reaction at 185-195 DEG C for 10-45 min so as to efficiently catalyze the dehydration of the saccharide compounds to prepare the 2,5-furandicarboxylic acid. Meanwhile, a small amount of carbonate zinc-glutarate is added as a catalyst auxiliary agent so as to activate CO2 and increase the solubility of the CO2 in the high-temperature solvent, thereby improving the reaction efficiency. The method of the invention has the advantages of high selectivity, fast reaction speed, environmental protection and low cost, and can provide reliable technical support for the preparation of the 2,5-furandicarboxylic acid from the saccharide compounds.

Description

technical field [0001] The present invention relates to a one-step cleaning method for preparing 2,5-furandicarboxylic acid, specifically a method for preparing 2,5-furandicarboxylic acid by using carbohydrate compounds as raw materials through one-step catalytic conversion, which belongs to industrial catalysis and biomass field of basic chemicals. Background technique [0002] Coal, petroleum and other fossil resources are the cornerstone of the development of human society, providing reliable energy and material security for human beings. In recent years, with the rapid consumption of fossil energy and the accompanying environmental problems have become increasingly prominent, the development of new renewable clean energy has become increasingly urgent. Biomass is a sustainable resource with huge quantity, low price and biodegradable. Excavating renewable biomass resources to prepare new platform compounds is an important method to solve the current resource and energy ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/68B01J23/648
CPCC07D307/68B01J23/6484
Inventor 黎演明龙思宇唐培朵杜芳黎杜奇石
Owner GUANGXI ACAD OF SCI
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