Method for preparing tetrahydrofurfuryl alcohol by liquid phase hydrogenation and catalyst used by method

A technology of tetrahydrofurfuryl alcohol and liquid phase hydrogenation, which is applied in the field of liquid phase hydrogenation, can solve the problems of high production cost and high energy consumption, and achieve the effects of high selectivity, low energy consumption and mild reaction conditions

Inactive Publication Date: 2015-05-13
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Among the methods proposed in the above-mentioned prior art, the catalytic reaction process for producing tetrahydrofurfuryl alcohol with furfuryl alcohol as the starting material needs to be carried out under high temperature and high pressure conditions, which consumes a lot of energy.
Moreover, the high ratio of hydrogen to oil in the existing method means that the reaction requires a large amount of hydrogen to participate in the reaction, making the production cost higher

Method used

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  • Method for preparing tetrahydrofurfuryl alcohol by liquid phase hydrogenation and catalyst used by method
  • Method for preparing tetrahydrofurfuryl alcohol by liquid phase hydrogenation and catalyst used by method

Examples

Experimental program
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Embodiment 1

[0031] The preparation of embodiment 1 catalyst:

[0032] TiO 2 Add the powder into 5-15M NaOH concentrated solution, react at 100-150°C for 2-3 days, then cool to room temperature, filter and wash with water, then dry to obtain titanium nanotube material, its XRD pattern is as follows figure 1 shown. From figure 2 The SEM image shown in (a) shows that the titanium nanotube material prepared by the present invention is very uniform and has good nanotube morphology.

[0033] Take appropriate amount of PdCl 2 Add the solution into the aqueous solution of titanium oxide nanotubes, stir evenly and adjust the pH to pd 2+ After the precipitation is complete, sodium borohydride is added for reduction and then filtered and dried to prepare a supported palladium catalyst with a specific surface area of ​​95-120m 2 / g, from figure 2 The TEM image shown in (b) shows that palladium metal nanoparticles are evenly distributed on the carrier, the size of which is in the range of 2-10...

Embodiment 2

[0037] Use the catalyst prepared in Example 1 to carry out the preparation of tetrahydrofurfuryl alcohol by furfuryl alcohol liquid-phase hydrogenation. In the round bottom flask, the catalyst is loaded, and the consumption is about 5% (accounting for furfuryl alcohol mass percent), and the solvent (ethanol) dilution ratio is about 20: 1 (ethanol: furfuryl alcohol, volume ratio), reaction temperature is 25 ℃, under the condition of hydrogen balloon (0.1MPa) reaction 1 hour, conversion rate of furfuryl alcohol is 98%, tetrahydrofurfuryl alcohol selectivity is 98%.

Embodiment 3

[0039]Use the catalyzer prepared in embodiment 1 to prepare tetrahydrofurfuryl alcohol by furfuryl alcohol liquid-phase hydrogenation, under the conditions of the reaction device and reaction temperature and pressure with embodiment 2, catalyst consumption is about 5% (accounting for furfuryl alcohol mass percent), solvent (Isopropanol) dilution ratio is about 20: 1 (isopropanol: furfuryl alcohol, volume ratio), reaction 1 hour, furfuryl alcohol conversion rate 70%, tetrahydrofurfuryl alcohol selectivity 99%.

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Abstract

The invention discloses a method for preparing tetrahydrofurfuryl alcohol by liquid phase hydrogenation. According to the method disclosed by the invention, the tetrahydrofurfuryl alcohol is prepared through the following steps: applying a loaded palladium catalyst for performing high-selective hydrogenation on furfuryl alcohol under the conditions of a low temperature and low pressure, and performing a reaction. The carrier of the loaded palladium catalyst is a titania material, and palladium nanometer metal ions are loaded on the carrier. The invention further discloses a preparation method of the loaded palladium catalyst. The method disclosed by the invention has the characteristics of mild reaction condition, high catalytic activity, high selectivity of the tetrahydrofurfuryl alcohol and the like.

Description

technical field [0001] The invention relates to a liquid-phase hydrogenation method for directly producing high-purity tetrahydrofurfuryl alcohol from furfuryl alcohol, and a supported palladium catalyst used in the process. Background technique [0002] Tetrahydrofurfuryl alcohol, also known as tetrahydrofuran methanol, is a green solvent and an important organic intermediate, which is widely used in agriculture and industry. It can be used to make dihydrofuran, tetrahydrofuran, lysine and long-acting vitamin B1; it can be used to produce amide plastics, antifreeze, herbicides and insecticides; it can be used as a lubricating oil dispersant and medicine in printing and dyeing Decolorizing and deodorizing agent. [0003] In industry, tetrahydrofurfuryl alcohol is generally synthesized by continuous two-step catalytic hydrogenation of furfural. The basic process is that furfural is first hydrogenated on a copper chromium catalyst to generate furfuryl alcohol, and furfuryl al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/12B01J23/44
CPCB01J23/44C07D307/12
Inventor 关业军袁庆庆
Owner EAST CHINA NORMAL UNIV
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