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Method for preparing 2, 5-dimethyloltetrahydrofuran through hydrogenation of 5-hydroxymethylfurfural

A 5-HMF, hydrogen technology, applied in chemical instruments and methods, catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of complex reaction process, increased cost, etc., and achieve simple operation. , The effect of low equipment requirements and high product selectivity

Pending Publication Date: 2021-12-10
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using a two-step method to prepare BHMTH not only complicates the reaction process, but also increases the cost

Method used

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  • Method for preparing 2, 5-dimethyloltetrahydrofuran through hydrogenation of 5-hydroxymethylfurfural
  • Method for preparing 2, 5-dimethyloltetrahydrofuran through hydrogenation of 5-hydroxymethylfurfural
  • Method for preparing 2, 5-dimethyloltetrahydrofuran through hydrogenation of 5-hydroxymethylfurfural

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Catalyst preparation: weigh 0.003mol of Ni(NO 3 ) 2 ·6H 2 O and 0.009mol of Co(NO 3 ) 2 ·6H 2 O in 150ml deionized water, then add 1g of CeO 2 to obtain precursors. Then weigh 3g Na 2 CO 3 and 1g NaOH in 10ml deionized water. Add dropwise to the precursor mixture and keep stirring. Stir until pH = 10, continue to age for 10h. The aged mixture was washed to neutral with deionized water. After that, it was dried in an oven at 100°C for 12 hours. Then calcined at 500°C for 4h, and reduced in hydrogen atmosphere before use, the bimetallic catalyst can be obtained.

[0016] Preparation of BHMTHF: Weigh 0.2g 5-HMF, 10mL water and 0.06g catalyst (Ni x -Co y / CeO 2 , where x=1, y=3, CeO 2 as a carrier) and put it into a 40mL reactor. Replace the air in the kettle with nitrogen for three to four times, then fill it with hydrogen until the initial pressure is 3MPa, turn on the stirring device at about 400r / min, heat to 110°C and react for 4h, then cool down, the ...

Embodiment 2

[0018] The preparation method of catalyst is the same as embodiment 1, but wherein CeO 2 Replaced by gas phase SiO 2 , and the reacted catalyst is recovered by a magnet for repeated cycle experiments.

[0019] The preparation method of BHMTHF was carried out with reference to the method in Example 1. Product adopts high performance liquid chromatography (HPLC, Thermo Scientific) to carry out qualitative and quantitative analysis, the liquid phase chromatogram under this condition is as follows image 3 shown. The peak at 22-24min represents BHMTHF. As a result, the conversion rate of 5-HMF was 100%, and the yield rate of BHMTHF was 82.9%.

Embodiment 3-5

[0021] Prepare by the method for embodiment 2 and obtain corresponding bimetallic metal catalyst, wherein the Co / Ni atomic ratio in embodiment 3 is 1 / 1 (promptly take the Ni (NO of 0.003mol) 3 ) 2 ·6H 2 O and 0.003mol of Co(NO 3 ) 2 ·6H 2 O); Co / Ni atomic ratio in embodiment 4 is 2 / 1 (promptly taking the Ni (NO of 0.003mol 3 ) 2 ·6H 2 O and 0.006mol of Co(NO 3 ) 2 ·6H 2 O); the Co / Ni atomic ratio in embodiment 5 is 4 / 1 (the Ni of 0.003mol (NO 3 ) 2 ·6H 2 O and 0.012mol of Co(NO 3 ) 2 ·6H 2 O).

[0022] The catalyst prepared above was tested according to the method of Example 2, and the conversion rate and selectivity of the product obtained by the reaction were measured, which are listed in Table 1.

[0023] Table 1 Preparation of different types of catalysts and their effects on the conversion and selectivity of 5-HMF aqueous phase hydrogenation to BHMTHF

[0024]

[0025] Comprehensive embodiment 1 to 5 know, carrier gas phase SiO 2 Compared with CeO 2 ...

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Abstract

The invention discloses a method for preparing 2, 5-dihydroxymethyl tetrahydrofuran (BHMTHF) through catalytic hydrogenation of 5-hydroxymethylfurfural (5-HMF) and application of the 2, 5-dihydroxymethyl tetrahydrofuran (BHMTHF). According to the invention, by using a supported catalyst, a first active component and a second component of the supported catalyst are respectively from corresponding non-noble metal salt solutions and are selected from Ni(NO3)2.6H2O and Co(NO3)2.6H2O; typical acidic oxide gas phase SiO2 is used as a carrier, the loading capacity of the two active components is (4 / 1)-(1 / 1), and the bimetallic catalyst is prepared by adopting a coprecipitation method; and the catalyst is simple and convenient in preparation method, low in price and cyclical, the catalytic reaction system is green, the reaction substrate is renewable, the reaction condition is mild, the input cost is low, and the catalyst has a wide industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of a non-noble bimetallic supported catalyst and a method for preparing 2,5-dimethyloltetrahydrofuran by hydrogenating 5-hydroxymethylfurfural. Background technique [0002] At present, 5-hydroxymethylfurfural (5-HMF) has attracted extensive attention as an important multifunctional platform compound. Usually it is obtained by the dehydration of carbohydrates derived from biomass under the action of acid catalysis. 5-HMF can be converted into high value-added chemical 2,5-dimethyloltetrahydrofuran (BHMTHF) after complete hydrogenation. BHMTH can be used as a green solvent with degradable, low toxicity and high stability. In addition, it can also be used as a substrate for further hydrogenation into high value-added linear polyols. For example, 1,5 pentanediol and 1,6 hexanediol etc. (Keiichi Tomishige, ACS Catal. 2014, 4, 2718-2726). Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/12B01J23/75B01J37/18
CPCC07D307/12B01J23/75B01J37/18
Inventor 林鹿田野曾宪海陈炳霖李闯李铮唐兴杨述良孙勇
Owner XIAMEN UNIV
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