Preparation method of 5-hydroxymethyl furoic acid and 2,5-furandicarboxylic acid

A technology of hydroxymethylfuroic acid and furandicarboxylic acid, which is applied in chemical instruments and methods, molecular sieve catalysts, physical/chemical process catalysts, etc. Inactivation and other problems, to achieve the effect of high reaction efficiency and product selectivity, mild reaction conditions and stable performance

Active Publication Date: 2014-03-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method achieves a high yield, the carrier used does not have a strong stabilizing effect on gold nanoparticles, and catalytic inactivation occurs under the reaction conditions, which limits its large-scale preparation and application.

Method used

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  • Preparation method of 5-hydroxymethyl furoic acid and 2,5-furandicarboxylic acid
  • Preparation method of 5-hydroxymethyl furoic acid and 2,5-furandicarboxylic acid
  • Preparation method of 5-hydroxymethyl furoic acid and 2,5-furandicarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take 1.73 g HAuCl 4 Add the solution (1wt%) to 50 grams of deionized water, heat to 60°C, add 0.3 grams of HY and stir, add sodium citrate solution for reduction and stir for 2 hours, wash the catalyst to PH = 7, and bake it under a hydrogen atmosphere at 100°C After drying for 5 hours, the catalyst Au / HY was finally obtained.

[0034] Take 0.317 g of HMF, 2.8 g of KOH (20%) and 3 ml of water into the reactor. The reaction vessel is a high-pressure reactor with 10 ml of polytetrafluoroethylene lining inside. Take 0.30 g of Au / HY (Au2wt%) as Catalyst, after temperature program is raised to 60 ℃, be filled with 0.3MPa oxygen, react for 6 hours, constantly supplement oxygen in the reaction process, guarantee that reaction is carried out under constant temperature and pressure. After the reaction product was centrifuged, the supernatant was removed and analyzed by HPLC. After testing, the conversion rate of the raw material HMF was 100%, and the FDA yield was 98%. The rea...

Embodiment 2

[0036] Take 1.73 g HAuCl 4 Add the solution (1wt%) to 50 grams of deionized water, heat to 60°C, add 0.3 grams of HX and stir, add sodium borohydride solution for reduction and stir for 2 hours, wash the catalyst to PH=7, and bake in a hydrogen atmosphere at 100°C After drying for 5 hours, the catalyst Au / HX was finally obtained.

[0037] Take 0.317 g of HMF, 2 g of NaOH (20%) and 3 ml of water into the reactor. The reaction vessel is a high-pressure reactor with 10 ml of Teflon lining inside. Catalyst, after temperature program is raised to 60 ℃, be filled with 0.3MPa oxygen, react for 6 hours, constantly supplement oxygen in the reaction process, guarantee that reaction is carried out under constant temperature and pressure. After the reaction product was centrifuged, the supernatant was removed and analyzed by HPLC. After testing, the conversion rate of raw material HMF was 100%, and the yield of HMFA was 90%. The reaction results are shown in Table 1.

Embodiment 3

[0039] Dissolve 1 g of NaY in 50 g of deionized water, heat up to 60°C, add 0.1 g of NH 4 CL was mixed and stirred for 2 hours, washed and centrifuged until the solution pH=7, and dried at 200°C for 4 hours to obtain the exchanged H x Na 1-x Y. Take 1.73 g HAuCl 4 The solution (1wt%) was added to 50 g of deionized water, heated to 60°C, and 0.3 g of H x Na 1-x Stir with Y, add sodium citrate solution to reduce and stir for 2 hours, wash the catalyst to PH=7, and dry it for 5 hours under a hydrogen atmosphere at 100 ° C to finally obtain the catalyst Au / H x Na 1-x Y.

[0040] Take 0.317g of HMF, 2g of NaOH (20%), and 3ml of water into the reactor. x Na 1-x Y (Au2wt%) is the catalyst. After the temperature is programmed to 60°C, 0.3MPa oxygen is charged, and the reaction is carried out for 6 hours. During the reaction, oxygen is continuously replenished to ensure that the reaction is carried out at constant temperature and pressure. After the reaction product was centri...

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Abstract

The invention discloses a preparation method of 5-hydroxymethyl furoic acid and 2,5-furandicarboxylic acid by selective oxidation of 5-hydroxymethylfurfural. The method comprises the following steps: taking a precious metal loaded acidic carrier as the catalyst, under mild conditions (temperature is in a range of 25 to 100 DEG C, and the oxygen pressure is in a range of 0.1 to 3.0 MPa), and modulating the temperature, pressure and reaction time so as to rapidly and high-efficiently oxidize 5-hydroxymethylfurfural to generate 5-hydroxymethyl furoic acid or 2,5-furandicarboxylic acid. The conversion rate of 5-hydroxymethylfurfural can reach 100%, the selectivity of 5-hydroxymethyl furoic acid reaches 98%, and the selectivity of 2,5-furandicarboxylic acid reaches 99%. The method has the advantages of high efficiency and environment-friendliness, and the products have a big application value and a wide application prospect.

Description

technical field [0001] The invention relates to the field of chemistry and chemical engineering, in particular to a method for preparing 5-hydroxymethylfuroic acid and 2,5-furandicarboxylic acid by catalytic oxidation of 5-hydroxymethylfurfural and an application thereof. Background technique [0002] So far, chemical platform compounds are mainly obtained from petroleum resources, and with the massive consumption of non-renewable resources such as petroleum, the price of crude oil continues to rise, and the cost of the chemical industry using petroleum as raw material will continue to increase, which has brought great pressure to the chemical industry. heavy burden. With the popularization of the concept of sustainable development, biomass, as a sustainable resource with low price, abundant reserves and continuous regeneration, has attracted more and more attention from scientists. Therefore, discovering renewable biological resources to prepare platform compounds is an im...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/68B01J29/12
CPCB01J29/123B01J29/126B01J2229/186C07D307/68
Inventor 徐杰蔡嘉莹马红黄义争宋奇苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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