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Method for preparing tetrahydrofurfuryl alcohol, and supported nickel catalyst

A technology of tetrahydrofurfuryl alcohol and nickel catalyst, which is applied in the direction of catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, etc., which can solve the problem that the catalyst cannot be directly recycled and the production process is dangerous high energy consumption of the reaction process, etc., to achieve the effect of mild reaction conditions, high yield and high catalytic activity

Inactive Publication Date: 2019-09-17
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the existing technical routes mentioned above, it is necessary to realize the furfural hydrogenation process under the conditions of high temperature or high pressure or the use of relatively expensive solvents or noble metal catalysts, and there are disadvantages such as high energy consumption of the reaction process, difficult operation, and high risk of the production process.
And all the above-mentioned technical routes are completed in the reactor, the catalyst cannot be directly recycled, and it is not easy to realize industrial production and application

Method used

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  • Method for preparing tetrahydrofurfuryl alcohol, and supported nickel catalyst
  • Method for preparing tetrahydrofurfuryl alcohol, and supported nickel catalyst
  • Method for preparing tetrahydrofurfuryl alcohol, and supported nickel catalyst

Examples

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Effect test

Embodiment 1

[0042] The preparation of embodiment 1 supported nickel catalyst

[0043] The silica carrier was uniformly dispersed in isopropanol solution, and tetrabutyl titanate (TiO 2 : SiO 2 =0.1, mass ratio), stirred overnight, suction filtered, oven-dried at 80°C for 12h, taken out and placed in a tube furnace for 2h at 500°C, with a heating rate of 3°C / min, to obtain 10TiO 2 / SiO 2 . Then use the excess impregnation method to load nickel, and disperse nickel nitrate hexahydrate in an appropriate amount of water (Ni: 10TiO 2 / SiO 2 =0.2, mass ratio), add ethylene glycol to control the particle size (ethylene glycol: metal nickel=5, molar ratio), stir evenly, add the obtained carrier 10TiO 2 / SiO 2 , stirred at 60°C until the solution was evaporated to dryness, dried in an oven at 80°C for 12 hours, took it out and put it in a tube furnace for 2 hours at 500°C, with a heating rate of 3°C / min, and then reduced it in hydrogen at 650°C for 2 hours, at a heating rate of 5°C / min, to o...

Embodiment 2

[0046] Use the catalyst prepared in Example 1 to prepare tetrahydrofurfuryl alcohol by furfural hydrogenation, and load catalyst 20Ni-5TiO in fixed bed 2 / SiO 2 , add raw material furfural, solvent ethanol, solvent dilution ratio is about 99:1 (water: furfural, volume ratio), reaction temperature is 90 ℃, hydrogen pressure 1MPa, hydrogen flow rate is 60ml / min, raw material flow rate is 0.05ml / min, The flow rate ratio of the supported nickel catalyst to the raw material is W / F=20g*min / mL, the catalytic activity remains stable within eight hours, the conversion rate of furfural remains 100%, and the selectivity of the target product remains 100%. Embodiment 3 furfural hydrogenation reaction

Embodiment 3

[0047] Use the catalyst prepared in Example 1 to prepare tetrahydrofurfuryl alcohol by furfural hydrogenation, and load catalyst 20Ni-5TiO in fixed bed 2 / SiO 2 , add raw material furfural, solvent ethanol, solvent dilution ratio is about 99:1 (water: furfural, volume ratio), reaction temperature is 90 ℃, hydrogen pressure 1MPa, hydrogen flow rate is 60ml / min, raw material flow rate is 0.1ml / min, The flow rate ratio of the supported nickel catalyst to the raw material W / F=10g*min / mL, the catalytic activity remained stable within eight hours, the conversion rate of furfural remained at 99%, and the selectivity of the target product remained at 96%.

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Abstract

The invention discloses a method for preparing tetrahydrofurfuryl alcohol. According to the method, a supported nickel catalyst is adopted to perform hydrogenation on furfural, so that the tetrahydrofurfuryl alcohol can be obtained; the raw material conversion rate is greater than 99%, and the product selectivity is greater than 99%. The invention also discloses a preparation method of the supported nickel catalyst, and application of the supported nickel catalyst in a hydrogenation reaction of the furfural. The technical route provided by the invention has the beneficial characteristics of being simple and convenient to operate, mild in reaction conditions, high in target product yield and low in energy consumption.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and relates to a method for preparing tetrahydrofurfuryl alcohol by hydrogenation, in particular to a method for directly hydrogenating furfural as a raw material to produce high-purity tetrahydrofurfuryl alcohol, and a supported nickel catalyst required in the process . Background technique [0002] Tetrahydrofurfuryl alcohol, also known as tetrahydrofuran methanol, can be used as a solvent for fats, waxes, paints, dyes, synthetic rubber and resins because of its low toxicity and environmental friendliness. It is also an important organic intermediate, which can be used in the synthesis of succinic acid, glutaric acid, tetrahydrofuran, long-acting vitamins, furan and pyridine. It is also widely used in production and life. It is used as a lubricant and dispersant in the printing and dyeing industry; it is used as a decolorizing and deodorizing agent in pharmaceuticals; it is also used as a raw...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/12B01J23/755B01J37/08B01J37/18
CPCC07D307/12B01J23/755B01J37/08B01J37/18
Inventor 关业军崔倩倩吴鹏
Owner EAST CHINA NORMAL UNIV
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