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Method for synthesizing ethylene glycol from noble metal load nanometer titanium dioxide through photocatalysis

A nano-titanium dioxide, precious metal technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of poor product selectivity, low conversion rate, loss of activity, etc. To achieve the effect of environmental friendliness, low price and good selectivity

Active Publication Date: 2011-05-25
SYNFUELS CHINA INNER MONGOLIA CO LTD
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  • Abstract
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AI Technical Summary

Problems solved by technology

Although the synthesis technology of ethylene glycol has been greatly developed and improved, it is still within the scope of traditional organic synthesis and has not fundamentally met the requirements of energy saving and environmental friendliness.
[0004] The photocatalytic synthesis of ethylene glycol from methanol has been reported on nano-ZnS catalysts. For details, see the reference: Photocatalytic oxidation of ethanol on the surface of nano- and micro-semiconductor particles, Bernd R. Müller, Journal of Photochemistry and Photobiology A : Chemistry 151 (2002) 253-265), but conversion rate is low, product selectivity is poor
In addition, due to the photocorrosion phenomenon of ZnS nanoparticles, the stability of ZnS nanocatalysts is poor, it is easy to lose activity, and cannot continue to react.

Method used

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  • Method for synthesizing ethylene glycol from noble metal load nanometer titanium dioxide through photocatalysis
  • Method for synthesizing ethylene glycol from noble metal load nanometer titanium dioxide through photocatalysis
  • Method for synthesizing ethylene glycol from noble metal load nanometer titanium dioxide through photocatalysis

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 125ml of isopropanol and 12.5ml of isopropyl titanate were mixed evenly, and under the condition of magnetic stirring and reflux, they were added dropwise in a 500ml round-bottomed flask equipped with water and isopropanol within 30min (the amount of water and isopropanol The ratio is 50:1), after the hydrolysis is complete, continue to stir and reflux for 2h. The reaction solution was transferred into a 50ml polytetrafluoroethylene-lined hydrothermal kettle, reacted at 80°C for 1 day, centrifuged and precipitated, and washed with distilled water to obtain pure anatase nanospheres. Move to a muffle furnace and bake at 1000°C for 10 hours to obtain pure rutile nanospheres. Take 1g of pure rutile TiO 2 The nanospheres were dispersed into 200ml of methanol-water reaction solution with a methanol volume fraction of 30%, and 0.3ml of chloroplatinic acid (1g / 10ml) was added according to the loading capacity of 3%, magnetically stirred and nitrogen gas was introduced. After ...

Embodiment 2

[0023] 125ml of isopropanol and 12.5ml of isopropyl titanate were mixed evenly, and under the condition of magnetic stirring and reflux, they were added dropwise in a 500ml round-bottomed flask equipped with water and isopropanol within 30min (the amount of water and isopropanol The ratio is 50:1), after the hydrolysis is complete, continue to stir and reflux for 2h. The reaction solution was transferred to a 50ml polytetrafluoroethylene-lined hydrothermal kettle, reacted at 80°C for 1 day, centrifuged and precipitated, and washed with distilled water to obtain pure anatase nanorods. Moved to the muffle furnace, roasted at 550°C for 5 hours to obtain TiO with anatase and rutile ratio of 30:70 2 Nano stave. Take 1g of TiO with a ratio of anatase and rutile of 30:70 2 The nanorods were dispersed into 400ml of methanol-water reaction liquid with a methanol volume fraction of 50%, and 0.2ml of palladium chloride (1g / 10ml) was added according to the loading capacity of 2%, and ni...

Embodiment 3

[0025]125ml of isopropanol and 12.5ml of isopropyl titanate were mixed evenly, and under the condition of magnetic stirring and reflux, they were added dropwise in a 500ml round-bottomed flask equipped with water and isopropanol within 30min (the amount of water and isopropanol The ratio is 50:1), after the hydrolysis is complete, continue to stir and reflux for 2h. The reaction solution was transferred to a 50ml polytetrafluoroethylene-lined hydrothermal kettle, reacted at 80°C for 1 day, centrifuged and precipitated, and washed with distilled water to obtain pure anatase nanorods. Move to a muffle furnace and bake at 600° C. for 8 hours to obtain nanorods with a ratio of anatase and rutile of 20:80. Get 1g anatase and rutile ratio and be that 20:80 nanorod is dispersed in the methanol-water reaction solution of 300mL methanol volume fraction 30%, add 0.4ml chloroauric acid (1g / 10ml) by loading capacity 4%, magnetically stir and Vacuum. After removing the oxygen in the syst...

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Abstract

The invention relates to a method for synthesizing ethylene glycol from noble metal load nanometer titanium dioxide through photocatalysis, which comprises the following steps: preparing P25TiO2 nanometer particles into nanometer balls or nanometer bars by a sol-gel method; preparing nanometer tubes or nanometer bars by a hydro-thermal method for carrying out roasting treatment to obtain pure anatase and pure rutile or TiO2 in a mixed crystal type nanometer structure formed by the anatase and the rutile in different proportions; and adding the prepared TiO2 into methanol-water reaction solution, adding noble metal source solution at the same time, pumping the vacuum or introducing the nitrogen gas under the effect of magnetic force or mechanical stirring, and turning on an ultraviolet lamp with the power between 10W and 2000W or a visible light source for reaction for 10 to 240h after the oxygen gas in the system is removed. The method provided by the invention has the advantages of stable property, high conversion rate, good selectivity, low price and environment protection.

Description

technical field [0001] The invention belongs to a method for synthesizing ethylene glycol, in particular to a method for photocatalytically synthesizing ethylene glycol supported by noble metal nano-titanium dioxide. Background technique [0002] Semiconductor photocatalysis is usually used to degrade organic and inorganic pollutants in gas and liquid phases, and its advantages are mild reaction conditions, non-toxic, and non-polluting. A large number of scientific studies have reported the application of semiconductor photocatalytic reaction in organic synthesis, but the reaction selectivity is low, and the photocatalytic reaction selectivity is further reduced in aqueous solution system, so photocatalysis has not been widely used in photocatalytic organic synthesis. C-C coupling is the core of organic synthesis. Applying semiconductor photocatalysis to C-C coupling to prepare high-value compounds is a promising organic synthesis route in the 21st century. [0003] Ethylen...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/34B01J23/42B01J23/44B01J23/52B01J23/50
CPCY02P20/52
Inventor 朱珍平张健赵江红卢海强李莉郑剑锋
Owner SYNFUELS CHINA INNER MONGOLIA CO LTD
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