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Preparation method for 2,5-dimethylfuran

A technology of dimethylfuran and tetrahydrofuran, applied in chemical instruments and methods, organic chemistry, physical/chemical process catalysts, etc., can solve the problems of low selectivity and low activity of non-noble metal catalysts, and achieve high catalytic activity and low Response costs and requirements for equipment, the effect of short time

Inactive Publication Date: 2018-11-23
枣庄九星生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although non-noble metal catalysts such as copper and nickel have been reported, there are still many problems to be solved, such as the low selectivity of 2,5-dimethylfuran and the low activity of non-noble metal catalysts.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] This example provides a method for preparing 2,5-dimethylfuran from 5-hydroxymethylfurfural catalyzed by a supported metal catalyst, which includes the following steps:

[0029] S1, adding 0.5 mmol of 5-hydroxymethylfurfural to 20 mL of tetrahydrofuran to prepare a 5-hydroxymethylfurfural solution;

[0030] S2, the above-mentioned 5-hydroxymethylfurfural solution and 0.1g of loaded metal catalyst are mixed and placed in a closed autoclave, and the 2 or H 2 / Ar mixed gas to replace the air 3-4 times, and then filled with H 2 or H 2 / Ar, heated to 200-350°C under high pressure of 0.8-2MPa and stirred for hydrodeoxygenation reaction for 12h, the gas flow rate was 20-100ml / min, and detected by gas chromatography and gas chromatography-mass spectrometry to obtain The conversion rate of methylfurfural was 73.0%, and the yield of product 2,5-dimethylfuran was 32.5%;

[0031] Wherein the above-mentioned supported metal catalyst, the catalyst includes component A and compone...

Embodiment 2

[0045] The difference between this embodiment and Example 1 is that the amount of Ni(NO3)2·6H2O is 3.8g, that is, in the step of loading transition metals, it is specifically:

[0046] Take 3.8g Ni(NO3)2·6H2O and add it to 8.0g N,N-dimethylformamide, stir and dissolve at room temperature, then add 5g of the above-mentioned aluminum-containing precursor, stir at room temperature for 1h, let it stand for 12h, then raise the temperature to 120°C Volatilize for 24 hours to completely volatilize ethanol, roast in the air at 600°C for 3 hours, and after natural cooling, pass in hydrogen and reduce at 550°C to obtain a Ni / Al2O3 catalyst.

[0047] This example also provides a method for preparing 2,5-dimethylfuran from 5-hydroxymethylfurfural catalyzed by the above-mentioned supported metal catalyst, the steps of which are similar to Example 1.

Embodiment 3

[0049] Ni(NO3)2.6H2O in embodiment 1 is changed into MgO, Al(NO3)3 is changed into Mg(NO3)2, the mixed solution of Ni(NO3)2, Mg(NO3)2 and Al(NO3)3 It is formulated according to the mass ratio of Ni, MgO and Al2O3 being 1:1:8, and the other implementation process is similar to that of Example 1, and a 10% Ni / MgO catalyst can be prepared.

[0050] This example also provides a method for preparing 2,5-dimethylfuran from 5-hydroxymethylfurfural catalyzed by the above-mentioned supported metal catalyst, the steps of which are similar to Example 1 of Example S.

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Abstract

The invention discloses a preparation method for 2,5-dimethylfuran. The preparation method comprises the following steps: adding 0.5 mmol of 5-hydroxymethylfurfural to 20 mL of tetrahydrofuran to prepare 5-hydroxymethylfurfural solution; mixing the 5-hydroxymethylfurfural solution and 0.1 g of a load-type metal catalyst and placing in a closed high-pressure reaction kettle, replacing air for 3-4 times by using H2 or a mixed gas of H2 / Ar, re-charging the H2 or H2 / Ar, heating to 200-350 DEG C in a high pressure of 0.8-2 MPa, stirring and performing a hydrodeoxygenation reaction for 12 h, whereina gas flow rate is 20-100 ml / min, and detecting by using a gas chromatography and gas chromatography-mass spectrometer. The preparation method has the beneficial effect that a non-noble metal catalyst is developed, the 2,5-dimethylfuran is efficiently and continuously prepared in a moderate reaction condition, and selectivity of the 5-hydroxymethylfurfural is greater than 95%.

Description

technical field [0001] The invention relates to the technical field of organic matter preparation, in particular to a method for preparing 2,5-dimethylfuran. Background technique [0002] With the continuous reduction of fossil resources such as petroleum, the continuous increase of greenhouse gas emissions, and the increasingly serious environmental pollution, the use of renewable new energy to replace traditional fossil energy has become an important research direction at present, and biomass energy is the only one containing Renewable energy sources of organic carbon are considered to be the most ideal substitutes for fossil energy sources. 5-Hydroxymethylfurfural, which can be prepared by acidic hydrolysis of cellulose, has been considered as one of the most important platform chemicals in biomass conversion processes. 2,5-Dimethylfuran is the most attractive of 5-hydroxymethylfurfural derivatives, which has excellent properties similar to gasoline, high energy density ...

Claims

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Application Information

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IPC IPC(8): C07D307/36B01J23/755B01J35/02
CPCC07D307/36B01J23/755B01J23/78B01J35/50
Inventor 孙彦
Owner 枣庄九星生物科技有限公司
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