Method for synthesizing low-impurity content glyoxal through gas phase oxidation

A gas-phase oxidation and glyoxal technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of carbon-based compounds, etc., can solve problems such as unsatisfactory selectivity, and achieve the effect of accelerating nucleation speed.

Active Publication Date: 2014-05-07
FUDAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent ZL200710038313 uses electroless plating to load copper on the surface of crystalline silver. Compared with the above catalysts, electroless plating of copper-loaded crystalline silver shows a very high conversion rate of ethylene glycol and yield of glyoxal, and its stability is also significantly better than the above patents. reported catalysts, but the content of formaldehyde and glycolaldehyde, which have an important impact on product quality, is still relatively high
ZL200710038313 discloses electroless copper-plated crystalline silver, the crystalline silver surface is very small, copper is deposited on the smooth crystalline silver surface, covering part of the active surface of silver, resulting in selectivity is still not ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] First, the electrolytic silver catalyst is pretreated, 5 grams of electrolytic silver catalyst is put into a stainless steel reactor with a diameter of 14mm, the distilled water is pumped into the gasifier with a metering pump to vaporize, mixed with the preheated air, and then passed through After heating, enter the reaction section to pretreat the electrolytic silver, and the liquid hourly space velocity of distilled water is 20hr -1 , the air flow rate is 0.035M 3 / h, the pretreatment temperature is 600°C, stop the steam after 8 hours of treatment time, and cool and dry under the air flow.

[0026]Dissolve copper nitrate and silver nitrate in distilled water to prepare a solution containing 0.05mol / L copper nitrate and 0.45mol / L silver nitrate, then slowly add ammonia water while stirring, first form copper hydroxide and silver hydroxide precipitation, add A blue mixed solution of copper ammonium complex and silver ammonium complex is formed after excessive ammonia ...

Embodiment 2

[0029] Adopt the method similar to example 1 to carry out pretreatment to electrolytic silver, the liquid hourly space velocity of distilled water is 10hr -1 , the air flow rate is 0.020M 3 / h, the pretreatment temperature is 300°C, stop the steam after 36 hours of treatment time, and cool and dry under the air flow.

[0030] Dissolve copper nitrate and silver nitrate in distilled water to prepare a solution containing 0.45 mol / L copper nitrate and 0.05 mol / L silver nitrate, then slowly add ammonia water while stirring, first form copper hydroxide and silver hydroxide precipitation, add A blue mixed solution of copper ammonium complex and silver ammonium complex is formed after excessive ammonia water, and the molar ratio of excess ammonia to ammonium complex ions is 1. Add reducing agent tartrate in another distilled aqueous solution, its molar ratio to ammonium complex ion is 2, adjust alkalinity with NaOH, make NaOH concentration be 0.4mol / L. After the above two solutions...

Embodiment 3

[0033] Adopt the method similar to example 1 to carry out pretreatment to electrolytic silver, the liquid hourly space velocity of distilled water is 50hr -1 , the air flow rate is 0.055M 3 / h, the pretreatment temperature is 500°C, stop the steam after 12 hours of treatment time, and cool and dry under the air flow.

[0034] Dissolve copper nitrate and silver nitrate in distilled water to prepare a solution containing 0.1mol / L copper nitrate and 0.1mol / L silver nitrate, then slowly add ammonia water while stirring to form copper hydroxide and silver hydroxide precipitation first, add A blue mixed solution of copper ammonium complex and silver ammonium complex is formed after excessive ammonia water, and the molar ratio of excess ammonia to ammonium complex ions is 10. Add reducing agent glucose to the above solution, the molar ratio of glucose to ammonia complex ion is 9, and mix well to obtain the electroless plating solution. Put the pretreated crystalline silver into the...

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Abstract

The invention belongs to the technical fields of chemistry and chemical engineering and in particular relates to a method for synthesizing low-impurity content glyoxal through gas phase catalytic oxidation. The method comprises the following steps: taking crystallized silver prepared by an electrolytic process as a carrier; performing high-temperature treatment, performing metal deposition, drying and roasting to obtain crystallized silver containing copper-silver alloy particles; taking the crystallized silver loaded with the copper-silver alloy particles as a catalyst, carrying out an oxidizing reaction among ethylene glycol, oxygen, water and inert gases to generate glyoxal in the presence of a catalyst. The 40 percent of glyoxal aqueous liquid in which the formaldehyde content is less than 500ppm and the glycolaldehyde content is less than 0.5 percent is directly obtained by performing air oxidation on ethylene glycol. The catalyst is easily regenerated and can be regenerated with a similar electrolytic silver method, and the prepared glyoxal is high in product quality.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and specifically relates to a method for synthesizing glyoxal with low impurity content by gas-phase catalytic oxidation of ethylene glycol. The method uses crystalline silver of silver-loaded copper alloy particles as a catalyst. Background technique [0002] The production of glyoxal by reacting ethylene glycol with air on a silver or copper catalyst is the main route for the production of glyoxal. The research on ethylene glycol air oxidation catalysts has been going on for decades. German patent DE1,967,147 uses crystalline silver as a catalysis, and the yield of synthesizing glyoxal can reach 70%, but the conversion rate is still not ideal, and the space velocity of raw materials is also relatively low. U.S. Patent No. 4,242,282 uses crystalline silver with a particle size of 0.1-2.5 mm as the catalyst. The catalyst is loaded with a thick bottom of several centimet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/127C07C45/38B01J23/89C22F1/14C23C18/48
CPCY02P20/584C07C45/38B01J23/8926B01J37/035B01J37/348C23C18/1827C23C18/48C07C47/127
Inventor 徐华龙尹国平邓支华晏浩哲秦枫沈伟
Owner FUDAN UNIV
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