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Method for preparing dihydroxymethyl tetrahydrofuran

A technology of dimethyloltetrahydrofuran and hydroxymethylfurfural, which is applied in the field of preparation of dimethyloltetrahydrofuran, can solve the problems of high reaction conditions (reaction temperature or reaction pressure, etc.), and achieve high yield and mild reaction conditions

Inactive Publication Date: 2015-04-08
林康艺
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, in the prior art, selective hydrogenation from 5-hydroxymethylfurfural to dimethyloltetrahydrofuran requires higher reaction conditions (reaction temperature or reaction pressure)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of metal-loaded carbon nitride materials:

[0024] Disperse 500 mg of carbon nitride into 10 ml of distilled water, add an aqueous solution containing 70 mg of potassium chloropalladate, stir at 80 °C for 1 h, then slowly add sodium borohydride solution (NaBH 4 / Pd molar ratio is 5:1), stirred at room temperature for 4 h, filtered, washed with distilled water, and dried in vacuum at 80 °C to obtain a carbon nitride material loaded with 5% palladium (5% Pd / C 3 N 4 ).

[0025] Catalytic preparation of dimethyloltetrahydrofuran from 5-hydroxymethylfurfural (HMF):

[0026] Accurately weigh 200 mg of 5-hydroxymethylfurfural and 100 mg of catalyst into the lining of the autoclave, and add 3 ml of water. After sealing the stainless steel autoclave, it was ventilated with hydrogen for 3 times, and then flushed with 1 MPa hydrogen at room temperature. Preheat the oil bath to the required temperature, put it into the autoclave, react at 60°C for 4h, stop the rea...

Embodiment 2~11

[0029] The difference from Example 1 is that the reaction temperature, hydrogen pressure, metal load, the mass ratio (X) of metal-loaded carbon nitride material to 5-hydroxymethylfurfural and different metals, the results are shown in the table 1.

[0030] Table 1

[0031] Example catalyst Reaction temperature / ℃ Hydrogen pressure / MPa Metal load / % X Yield / % 2 Pd / C 3 N 4 80 1 5 0.5 95 3 Pd / C 3 N 4 40 1 5 0.5 80 4 Pd / C 3 N 4 60 0.5 5 0.5 86 5 Pd / C 3 N 4 60 2 5 0.5 94 6 Pd / C 3 N 4 60 1 1 0.5 90 7 Pd / C 3 N 4 60 1 3 0.5 92 8 Pd / C 3 N 4 60 1 5 0.2 89 9 Pd / C 3 N 4 60 1 5 0.8 95 10 Ru / C 3 N 4 60 1 5 0.5 86 11 Pt / C 3 N 4 60 1 5 0.5 74

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PUM

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Abstract

The invention discloses a method for preparing dihydroxymethyl tetrahydrofuran, which comprises the following steps: arranging 5-hydroxymethylfurfural and a metal loaded carbon nitride material in a reactor, adding distilled water, introducing hydrogen gas, and reacting at 40-80 DEG C for 1-6 hours to obtain the dihydroxymethyl tetrahydrofuran, wherein the metal is a ruthenium / palladium / platinum loaded carbon nitride material; the loaded amount of the metal is 1-10%; the pressure of the hydrogen gas is 0.5-2 MPa; and the mass ratio of the metal loaded carbon nitride material to the 5-hydroxymethylfurfural is (0.2-0.8):1. The method is mild in reaction conditions and has high dihydroxymethyl tetrahydrofuran yield.

Description

technical field [0001] The invention relates to a method for preparing dimethylol tetrahydrofuran. Background technique [0002] Hydrogenation reaction is one of the important reactions for converting biomass raw materials to produce fuels and fine chemicals. 5-Hydroxymethylfurfural from biomass raw materials is an excellent platform compound that can be used to prepare other important fine chemicals through hydrogenation reactions. 5-Hydroxymethylfurfural can be selectively hydrogenated to dimethyloltetrahydrofuran, among which DHMTHF is a valuable chemical, which can be used as a solvent, monomer and as a precursor for the production of other high value-added chemicals, is A platform chemical that can be used in the production of polymers and specialty fine chemicals. [0003] However, in the prior art, the selective hydrogenation from 5-hydroxymethylfurfural to dimethyloltetrahydrofuran requires relatively high reaction conditions (reaction temperature or reaction press...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/12B01J27/24
CPCC07D307/12B01J27/24
Inventor 林康艺
Owner 林康艺
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