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Method for preparing 2, 5-dimethylfuran by catalyzing 2, 5-furandimethanol

A technology for furandimethanol and dimethylfuran, which is applied in the field of preparing 2,5-dimethylfuran, can solve the problems of hydrogen limitation, reduced safety factor, inconvenience and the like, achieves improvement of selectivity and yield, avoids high temperature and high pressure Condition, effects on storage and transport

Pending Publication Date: 2022-07-01
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the higher reaction temperature and pressure not only reduces the safety factor of the reaction and increases the production cost, but also leads to the transitional hydrogenation of HMF to produce more by-products, such as 2,5-dimethyltetrahydrofuran (DMTHF) , levulinic acid (LA), 2,5-dimethyloltetrahydrofuran (DHMTHF)
Furthermore, the non-renewable nature and its flammable and explosive properties limit the use of hydrogen in hydrodeoxygenation applications
The raw material HMF is easily deliquified in the air, which also brings great inconvenience to production and transportation.

Method used

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  • Method for preparing 2, 5-dimethylfuran by catalyzing 2, 5-furandimethanol
  • Method for preparing 2, 5-dimethylfuran by catalyzing 2, 5-furandimethanol
  • Method for preparing 2, 5-dimethylfuran by catalyzing 2, 5-furandimethanol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] (1) Add 0.5g XC-72, 45mL deionized water, 5mL ethanol to the beaker, add 0.235mmol Na after sonicating for 40min 2 PdCl 4 , and stirred at room temperature for 6h. Then, 5 mL of freshly prepared 0.2 mol / L sodium borohydride solution was added for reduction for 2 h, and the Pd / XC-72 catalyst was obtained by washing.

[0066] (2) Take 0.26g of 2,5-furandimethanol and add it to 15mL of dioxane to prepare a reaction substrate solution. Combine the reaction substrate solution, 0.76mL of anhydrous formic acid and 0.2g of the prepared solution in (1). The Pd / XC-72 catalyst was mixed and placed in the reaction kettle, the gas in the kettle was replaced with nitrogen five times, the air was exhausted, and the reaction was heated to 120 °C at a stirring rate of 400 r / min for 15 h to obtain the product 2,5-dimethylfuran.

[0067] like figure 1 Shown is the XRD pattern of the prepared Pd / XC-72 catalyst, which has an obvious diffraction peak at the 2-theta angle of 25.0 (002), wh...

Embodiment 2

[0077] (1) Add 0.5g CNT, 45mL deionized water, 5mL ethanol to the beaker, add 0.235mmolNa after sonicating for 40min 2 PdCl 4 , and stirred at room temperature for 6h. Then, 5 mL of freshly prepared 0.2 mol / L sodium borohydride solution was added for reduction for 2 h, and the Pd / CNT catalyst was obtained by washing.

[0078] (2) Take 0.26g of 2,5-furandimethanol and add it to 15mL of dioxane to prepare a reaction substrate solution. Combine the reaction substrate solution, 0.76mL of anhydrous formic acid and 0.2g of the prepared solution in (1). The Pd / CNT catalyst was mixed and placed in the reaction kettle, the gas in the kettle was replaced with nitrogen five times, the air was exhausted, and the reaction was heated to 120 °C at a stirring rate of 400 r / min for 15 h to obtain the product 2,5-dimethylfuran.

[0079] The reaction results are shown in Table 2. After the reaction for 15 hours, the conversion rate of BHMF reached more than 99%, and the yield of DMF was 73%, w...

Embodiment 3

[0081] (1) Add 0.5g activated carbon, 45mL deionized water, 5mL ethanol to the beaker, add 0.235mmol Na after sonicating for 40min 2 PdCl 4 , and stirred at room temperature for 6h. Then, 5 mL of freshly prepared 0.2 mol / L sodium borohydride solution was added for reduction for 2 h, and the Pd / AC catalyst was obtained by washing.

[0082] (2) Take 0.26g of 2,5-furandimethanol and add it to 15mL of dioxane to prepare a reaction substrate solution. Combine the reaction substrate solution, 0.76mL of anhydrous formic acid and 0.2g of the prepared solution in (1). The Pd / AC catalyst was mixed and placed in the reaction kettle, the gas in the kettle was replaced with nitrogen five times, the air was exhausted, and the reaction was heated to 120 °C at a stirring rate of 400 r / min for 15 h to obtain the product 2,5-dimethylfuran.

[0083] The reaction results are shown in Table 2. After the reaction for 15h, the conversion rate of BHMF reached more than 99%, and the yield of DMF was...

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Abstract

The invention discloses a method for preparing 2, 5-dimethylfuran by catalyzing 2, 5-furandimethanol. The method comprises the following steps: putting a mixture containing a reaction substrate solution, formic acid and a catalyst into a closed container, and reacting to obtain the 2, 5-dimethylfuran, the reaction substrate solution comprises 2, 5-furandimethanol and an organic solvent. According to the method, 2, 5-furandimethanol which is more stable at normal temperature is used for replacing 5-hydroxymethylfurfural as a raw material, so that storage and transportation are facilitated. Formic acid is used for replacing hydrogen, so that reaction conditions are milder, high-temperature and high-pressure conditions and generation of furan ring transition hydrogenation products are avoided, and the selectivity and yield of the products are improved. The method has important theoretical and practical significance for development of clean energy and high-value utilization of biological resources.

Description

technical field [0001] The application relates to a method for catalyzing 2,5-furandimethanol to prepare 2,5-dimethylfuran under mild conditions, belonging to the field of chemical industry. Background technique [0002] With the rapid development of the global economy, traditional energy is rapidly consumed, and the development of renewable new energy fuels to replace fossil fuels has become a current research focus. Biomass, as a wide-ranging, low-cost sustainable resource, can be regenerated by the sun's photosynthesis, and has broad application prospects. Among them, the biomass-derived chemical 2,5-dimethylfuran (DMF) has many excellent properties similar to gasoline, such as high energy density (30MJ / L) and high octane number (119), with a boiling point of 92~ At 94°C, the solubility in water is only 0.26wt%, and it can be miscible with gasoline or used alone. Compared with biofuel ethanol, which is easily soluble in water, difficult to preserve and has low combustio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/36B01J23/42B01J23/52B01J23/46
CPCC07D307/36B01J23/42B01J23/52B01J23/462
Inventor 张建赵玺吕明鑫杨勇郝盼盼
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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