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Method for preparing furfuryl alcohol by utilizing hydrogen transfer reaction to catalyze furfural

A hydrogen transfer and furfural technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve problems such as hexavalent chromium environmental pollution, high energy consumption, and increased equipment investment costs, achieving low cost, Low energy consumption and the effect of reducing production costs

Inactive Publication Date: 2017-03-29
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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AI Technical Summary

Problems solved by technology

[0005] (1) The gas-phase hydrogenation of furfural into furfuryl alcohol is mainly based on copper-based catalysts and requires high temperature And high pressure (30bar) operation (J.Mol.Catal.A,2007,265,90-97.), so the energy consumption is higher;
[0006] (2) Furfural is converted into furfuryl alcohol by liquid-phase hydrogenation. Copper chromium oxide catalysts are widely used in industry, but the toxicity of hexavalent chromium can cause serious environmental pollution;
[0007] (3) Some chromium-free catalyst systems such as noble metal catalysts (platinum, ruthenium, iridium), alloyed bimetallic catalysts containing promoters such as (Co-Mo-B, Ni-Ce-B, Ni-Fe-B), and Bimetallic catalysts without additives (Ni-Cu, Pt-Sn / Si0 2 , Ni-Sn / Ti0 2 , Cu-Fe oxides) have realized the selective hydrogenation of furfural into furfuryl alcohol, but liquid phase hydrogenation usually requires the use of high-pressure hydrogen, which increases the cost of equipment investment

Method used

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  • Method for preparing furfuryl alcohol by utilizing hydrogen transfer reaction to catalyze furfural
  • Method for preparing furfuryl alcohol by utilizing hydrogen transfer reaction to catalyze furfural
  • Method for preparing furfuryl alcohol by utilizing hydrogen transfer reaction to catalyze furfural

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preparation example Construction

[0026] The preparation method of the heterogeneous magnetic hydroxyapatite catalyst used in the present invention, the steps are:

[0027] ① Weigh 2.64g (NH4) 2 HPO 4 , add 90mL distilled water to dissolve, then add concentrated ammonia (25-28wt.%) to adjust the pH to 11; ②Weigh 7.95g Ca(NO 3 ) 2 4H 2 O, add 90mL distilled water to dissolve, then add concentrated ammonia water (25-28wt.%) to adjust the pH to 11; ③at room temperature, put a suitable stirring bar into a 500mL two-necked flask, add 0.514g FeSO 4 ·7H 2 O and 1gFeCl 3 ·6H 2 O, pass nitrogen to exhaust the air in the flask, continue to pass nitrogen, add 30mL of distilled water at the same time, add 10mL of 26.5wt.% ammonia water, after stirring for 15 minutes, drop the two solutions obtained in steps ① and ② at the same time, and heat up to 90 ° C. After stirring for 2 hours, stop stirring and let stand overnight; ④ filter, wash 4 times with water, dry at 80°C, and calcined at 300°C for 3 hours to obtain a r...

Embodiment 1

[0031] A kind of method utilizing hydrogen transfer reaction catalysis furfural to prepare furfuryl alcohol, comprises the following steps:

[0032] 120mg catalyst γ-Fe 2 o 3 Add @HAP to the lining of a clean autoclave, then add 1mmol furfural and 15mL methanol (both as a hydrogen donor and as a reaction solvent), seal the stainless steel autoclave, and use N 2 Change air three times, then fill with 10barN at room temperature 2 , react at 190°C for 10h, and detect the composition of the product by liquid chromatography after the reaction (such as figure 1 ), conversion rate 100%, productive rate 30.8%, selectivity 30.8%.

Embodiment 2-7

[0034] This embodiment provides the experiment of reducing furfural to furfuryl alcohol under different hydrogen donors;

[0035] A kind of method utilizing hydrogen transfer reaction catalysis furfural to prepare furfuryl alcohol, comprises the following steps:

[0036] 40mg catalyst γ-Fe 2 o 3 Add @HAP to the lining of a clean autoclave, add 1mmol furfural and 15mL of different alcohol compounds (both as a hydrogen donor and as a reaction solvent), seal the stainless steel autoclave and use N 2 Change air three times, then fill with 10barN at room temperature 2 , reacted at 180°C for 3h; using different alcohol compounds, the specific experimental results are shown in Table 1:

[0037] Table 1 Catalytic effects when using different hydrogen donors

[0038] Example Hydrogen Donor and Solvent Conversion rates(%) Yield(%) selectivity (%) 2 ethanol 64.0 45.4 70.9 3 n-propanol 65.7 53.6 81.5 4 Isopropanol 64.9 59.5 91.8 5 But...

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Abstract

The invention provides a method for preparing furfuryl alcohol by utilizing a hydrogen transfer reaction to catalyze furfural. The method comprises the following steps that under the catalysis of a heterogeneous catalyst, namely magnetic hydroxyapatite, the furfural and alcoholic compounds with hydrogen donors are subjected to the hydrogen transfer reaction, wherein the ratio of the magnetic hydroxyapatite to the alcoholic compounds to the furfural is 20-120 g to 8-20 L to 1 mol. A reaction container is filled with nitrogen (N2) of which pressure is 1-20 bar at room temperature, the reaction temperature is 100 DEG C-200 DEG C, and a reduced product, namely the furfuryl alcohol, is obtained after 1-12 h. The method for preparing the furfuryl alcohol by utilizing the hydrogen transfer reaction to catalyze the furfural is simple in process, convenient to operate and safe and environmentally friendly. The catalyst is a non-precious metal catalyst and cheap and easy to obtain, has magnetism and is easy to separate, and can be reused repeatedly. The activity does not decrease. The industrial cost of preparing the furfuryl alcohol can be lowered to a large extent, ethyl levulinate can be catalyzed to react and gamma-valerolactone is generated, and other compounds containing C=O bonds can be also reduced.

Description

technical field [0001] The invention belongs to the field of furfuryl alcohol preparation and production, and in particular relates to a method for preparing furfuryl alcohol by catalyzing furfural through a hydrogen transfer reaction. Background technique [0002] With rapid economic development and increasing demand for energy, as well as dwindling fossil resources, one challenge for researchers is to find a sustainable pathway to utilize renewable biomass or biomass-derived chemicals. [0003] As a biomass derivative, furfural can be produced by hydrolysis of agricultural waste such as corncobs and bagasse, and is an important chemical platform substance. Selective reduction of furfural is an important way to prepare other valuable chemicals, and the reduction of carbon-oxygen double bonds in furfural to furfuryl alcohol is one of the most important reactions. Furfuryl alcohol is an important chemical raw material and an important intermediate for synthetic resins, dyes,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/44B01J27/185
CPCB01J27/1853C07D307/44
Inventor 张泽会汪帆姜亮
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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