Method for synthesizing biformyl by means of glycol catalytic oxidation and using lanthanum phosphate mosaic etectric crystal silver as catalyst
A technology of catalytic oxidation and silver catalyst, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carbon-based compounds, etc., can solve the problem of unsatisfactory high temperature resistance and activity stability of catalysts, easy loss of components, and insufficient restriction of catalysts. good question
Inactive Publication Date: 2002-09-04
FUDAN UNIV
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[0003] Silver-catalyzed production of glyoxal is the most important method for producing glyoxal in the world, and Russian patent RU136,352 describes the use of Al 2 o 3 Be the loaded silver (40%Ag) of carrier as catalyzer, glyoxal yield 61%, this method catalyzer prepares complicatedly, ethylene glycol must be diluted, and catalyzer is easily poisoned
U.S. Patent No. 4,242,282 describes the method for the synthesis of glyoxal by catalytic oxidation of ethylene glycol, using electrocrystallized silver as a catalyst, the catalyst is made into particles, layered and paved, and the yield of glyoxal is 66%. The shortcoming of this method is that Catalyst restriction is still not good enough, and the high temperature resistance of the catalyst is poor
Russian patent RU2,119,385 describes the use of phosphorus-modified silver catalysts. Phosphorus modification can effectively improve the limitation of the catalyst. The disadvantage of this method is that phosphorus is easy to lose, and the high temperature resistance and activity stability of the catalyst are not satisfactory.
The addition of phosphorus is beneficial to improve the selectivity of the catalytic oxidation of ethylene glycol, and the addition of lanthanum helps to improve the thermal stability of crystalline silver, but these additives are easy to be lost by the conventional impregnation method, and can only be loaded on the surface, which is harmful to heat. The improvement in stability has no obvious effect
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[0017] 1. Prepare 3% silver nitrate solution as the electrolyte; add 5g / L of lanthanum phosphate with a particle size of 1μm to the electrolyte; electrolyze metallic silver with a content of 99.99% as the anode, the electrolysis temperature is 35°C, and the current density is 3A / dm 2 , the air is strongly stirred, and the electrocrystallized silver catalyst embedded with lanthanum phosphate is prepared.
[0018] Put 5 grams of lanthanum phosphate-embedded electrocrystallized silver catalyst into a stainless steel reactor with a diameter of 14mm, inject the ethylene glycol aqueous solution into the gasifier with a metering pump, mix it with the preheated air, and then enter the The catalytic bed reacts, and the liquid hourly space velocity of ethylene glycol is 8hr -1 , the air feed flow rate is 0.014M 3 / h, the reaction temperature is 410°C, the product is quenched and absorbed by spraying after quenching, and the supplementary water quantity of spraying is controlled to obta...
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Abstract
The present invention relates to a method for synthesizing biformyl by catalytic oxidation of glycol. In the presence of lanthanum phosphate mosaic electrocrystal silver catalyst, the glycol can be air-oxidated to produce 40% biformly by means of one-step process. Tests show that the said invented silver catalyst high-temp. resistance and catalytic activity stability are greatly raised.
Description
technical field [0001] The invention relates to a method for synthesizing glyoxal by catalytic oxidation of ethylene glycol. Background technique [0002] Glyoxal has two adjacent carbonyl groups in its structure. In addition to its generality of aldehydes and ketones, it can also perform many special reactions and is widely used in organic synthesis, medicine and biochemistry. The invention provides an improved method for synthesizing glyoxal by air oxidation of ethylene glycol catalyzed by silver. An electrocrystallized silver catalyst is prepared by using lanthanum phosphate mosaic composite electrolysis, so that the catalyst has better high temperature resistance and stability. [0003] Silver-catalyzed production of glyoxal is the most important method for producing glyoxal in the world, Russian patent RU136,352 describes the use of Al 2 o 3 The supported silver (40% Ag) as the carrier is used as the catalyst, and the yield of glyoxal is 61%. The preparation of the ca...
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IPC IPC(8): C07C45/32C07C47/127
Inventor 徐华龙沈伟
Owner FUDAN UNIV