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Method for preparing tetrahydrofurfuryl alcohol from furfural by aqueous phase hydrogenation

A technology for the preparation of tetrahydrofurfuryl alcohol and hydrogen, which is applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, organic chemistry, etc., and can solve problems such as unstable nickel framework, increased risk, and increased cost , to avoid separation and purification, reduce intermediate steps, and reduce production costs

Inactive Publication Date: 2015-06-03
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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AI Technical Summary

Problems solved by technology

Cai Tianxi et al. used a heteropolyacid-modified framework nickel catalyst to prepare THF from furfural at 2.0 MPa and 80 °C. The conversion rate of furfural and the selectivity of THF reached 98.1% and 98.5%, respectively (Applied Catalysis A: General1998,171:117-122). Keiichi Tomishige etc. used Ni-Pd / SiO 2 As a catalyst, hydrogenation of furfural under relatively mild conditions (40°C, 8MPaH2), the selectivity of tetrahydrofurfuryl alcohol reached 96% (Catalysis Communications2010, 12:154156). Although the preparation of tetrahydrofurfuryl alcohol from furfural has a good effect , but most of them use unstable nickel catalysts, which increases the danger in the production process; some even use noble metal catalysts, which increases the cost

Method used

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  • Method for preparing tetrahydrofurfuryl alcohol from furfural by aqueous phase hydrogenation
  • Method for preparing tetrahydrofurfuryl alcohol from furfural by aqueous phase hydrogenation

Examples

Experimental program
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Embodiment 1

[0018] Catalyst preparation: weigh 4.95g Ni(NO 3 ) 2 ·6H 2 O and add 2.70g of water and stir to dissolve. Add 10g of activated alumina, stir well to form a paste, let stand for 15h, dry at 120°C, then bake at 550°C for 4h, activate at 500°C in a hydrogen atmosphere for 4h before use. figure 1 .

[0019] The catalytic reaction was carried out in a 50ml stainless steel reactor. Add 0.1g of catalyst, 1.5g of furfural, and 8.5g of water into a stainless steel autoclave with a polytetrafluoroethylene lining, and then use Na 2 CO 3 Adjust the pH to 8-9. After closing the reactor, replace the gas in the reactor with hydrogen four times, control the temperature to rise to 140°C with a temperature controller, fill in hydrogen to 4MPa, and start stirring. Keep the pressure constant during the reaction process. After the hydrogenation reaction is completed, after cooling and releasing the pressure, the samples are analyzed by gas chromatography. figure 2 . The reaction time and...

Embodiment 2

[0021] In the nickel nitrate solution in embodiment 1, add 0.50g Co(NO 3 ) 2 ·6H 2 O, other are all with embodiment 1. The results are shown in Table 1.

Embodiment 3

[0023] Change the cobalt nitrate in embodiment 2 into 2.10g Cu(NO 3 ) 2 ·3H 2 O other are all with embodiment 2. The results are shown in Table 1.

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Abstract

The invention discloses a method for preparing tetrahydrofurfuryl alcohol from furfural by aqueous phase hydrogenation. According to the method, furfural is directly converted into tetrahydrofurfuryl alcohol by using water as a solvent in a 0.5-10MPa hydrogen atmosphere at 80-180 DEG C in the presence of a nickel-based catalyst and an alkali additive, wherein the yield of the tetrahydrofurfuryl alcohol can reach 94%.

Description

technical field [0001] The invention relates to a method for preparing tetrahydrofurfuryl alcohol, in particular to a new system for directly preparing tetrahydrofurfuryl alcohol by using furfural as a raw material through aqueous phase hydrogenation. Background technique [0002] Tetrahydrofurfuryl alcohol (also known as tetrahydrofuran methanol), is an excellent solvent and an important organic chemical raw material, such as a solvent for coatings, resins and oils; it can also be used as a raw material for the preparation of pyridine, tetrahydrofuran, lysine, etc. ; Can also be used to prepare plasticizers, insecticides, antifreeze, herbicides, etc. [0003] At present, tetrahydrofurfuryl alcohol is mainly produced industrially through a two-step method. Furfural is first selectively hydrogenated to obtain furfuryl alcohol, and then tetrahydrofurfuryl alcohol is prepared by further selective hydrogenation of furfuryl alcohol. The catalyst used in the hydrogenation of furf...

Claims

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Application Information

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IPC IPC(8): C07D307/12B01J23/755B01J23/83B01J23/80B01J23/889
Inventor 徐杰杨艳良杜中田路芳高进马红苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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