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Method for coupling hydrogenation reaction with hydrogen-producing reaction by means of photocatalysis

A technology of hydrogenation reaction and photocatalysis, which is applied in the direction of chemical instruments and methods, organic chemical methods, and the preparation of organic compounds. It can solve the problems of harsh reaction conditions and high equipment requirements, and achieve high product selectivity and yield. The effect of less emission and simple process

Active Publication Date: 2008-11-05
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, we found that the entire reaction process still needs to be carried out at a temperature of 393K-513K and a pressure of 0.6MPa-5.0MPa, and Raney-Ni or noble metal doped catalysts must participate in the reaction. The reaction conditions are relatively harsh and the equipment requirements are high.

Method used

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  • Method for coupling hydrogenation reaction with hydrogen-producing reaction by means of photocatalysis

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Experimental program
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Effect test

Embodiment 1

[0022] Weigh 0.06g p-nitrophenol and 0.3gTiO 2 Powder (P25 type, commercial catalyst, containing about 80% anatase type and 20% rutile type, average particle diameter 30nm), it is put into 500ml quartz glass reactor, add 250ml concentration and be 10% methanol solution, put into With a magnetic stirring bar, start the magnetic stirrer, and pass through nitrogen to exhaust oxygen for 30 minutes. Turn on a light source with a dominant wavelength of 365nm, irradiate for 1 hour, and terminate the reaction, filter to remove the photocatalyst, and perform product analysis on the obtained filtrate by high-pressure liquid chromatography (HPLC) to obtain p-aminophenol with a yield of 98%.

Embodiment 2

[0024] Get 0.25mmol p-nitrobenzene and 0.5mmol Hombikat UV100 commercial photocatalyst, put it into 500ml quartz glass reactor, add 250ml concentration and be 15% biomass ethanol solution, put into magnetic stirrer, start magnetic stirrer, Nitrogen exhaust oxygen 30min. Turn on a light source with a dominant wavelength of 254nm, irradiate for 10 hours, and terminate the reaction. Filter and remove the photocatalyst. The resulting filtrate is analyzed by high-pressure liquid chromatography (HPLC) to obtain p-aminobenzene with a yield of 96%.

Embodiment 3

[0026] Take 1.25mmol acetophenone and 3.75mmol Pt-TiO 2 (the loading capacity of platinum is 1%), put it into 500ml quartz glass reactor, add 250ml concentration and be 10% glucose solution, put into magnetic stirrer, start magnetic stirrer, logical nitrogen exhausts oxygen 30min. Turn on the light source with a dominant wavelength of 800nm, irradiate for 0.45h and finish the reaction, filter to remove the photocatalyst, and analyze the obtained filtrate by high pressure liquid chromatography (HPLC) to obtain α-phenylethanol with a yield of 95%.

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Abstract

The invention discloses a method for coupling hydrogen-producing reaction with hydrogenation reaction by utilizing photocatalysis, which includes: adding a hydrogenation precursor, a photocatalyst and a hydrogen source precursor into a reactor; reacting for 0.1 to 10h under the irradiation of a light source with the wavelength being 180nm to 800nm after being fully mixed; filtering and removing the photocatalyst to obtain a reducing product; wherein, the quality concentration of the water liquor of the hydrogen source precursor is 1 to 50 percent; the method can generate reaction under the thermal condition caused by constant temperature and uviol lamp, thus having the advantages of low cost, needing no expensive hydrogen storage and transmission devices, being safe to be operated, simple technique as well as higher reducing conversion rate and yield coefficient; besides, the utilized electron transferring efficiency ratio is higher than the electron transferring efficiency utilized by producing hydrogen under the same conditions by two orders of magnitude.

Description

technical field [0001] The invention belongs to the field of synthesis methods of organic compounds, and particularly proposes a method for coupling hydrogen production reaction and hydrogenation reaction by using photocatalysis technology. Background technique [0002] The existing organic hydrogenation reaction process in the chemical industry usually hydrogenates the reactants under the conditions of high temperature and high pressure, external hydrogen supply and the presence of metal catalysts, which consumes a lot of energy and also brings serious environmental pollution, which is not conducive to national energy conservation and emission reduction achievement of goals [1，2] . Professor Li Xiaonian from Zhejiang University of Technology proposed a new reaction system for liquid-phase catalytic hydrogenation, which couples the two reactions of aqueous phase reforming hydrogen production and liquid-phase catalytic hydrogenation. Eliminates the need for special hydrogen...

Claims

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Application Information

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IPC IPC(8): C07B31/00C07C209/32C07C29/136
Inventor 陆小华柏扬杨祝红李东李伟朱银华冯新
Owner NANJING UNIV OF TECH