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Catalyzer for CO low-voltage gas-phase synthesizing of oxalic ester and method of preparing the same

A low-pressure gas phase, oxalate ester technology, used in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of low space-time yield, etc. Effect

Inactive Publication Date: 2008-03-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Subsequently, many patents have successively reported that Mo, Ni, Ti, Fe, Ga, Cu, Na 2 O, and SiO 2 Catalysts composed of additives such as CO and nitrite are used in the gas phase synthesis of dimethyl oxalate, diethyl oxalate and diisopropyl oxalate, but the space-time yield is still low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 20g specific surface area is 15m 2 / g of α-Al 2 o 3 Two parts of the carrier, one part modified (denoted as Al 2 o 3 (M)), one unmodified treatment (denoted as Al 2 o 3 (W). According to 1.2wt%Pd+0.4wt%Ti+0.2%wtCe / α-Al 2 o 3 Content preparation catalyst, its steps are as follows: choose tetrabutyl titanate, prepare impregnating liquid according to Ti loading amount, loading amount is formulated into impregnating liquid, in order to prevent titanium from being hydrolyzed, dissolve and prepare ethanol solution with absolute ethanol dried through molecular sieves, The prepared modified α-Al 2 o 3 After the carrier was soaked in the solution for 24 hours, it was vacuum-dried for 8 hours to obtain a solid. Select Ce(NO 3 ) 3 According to the amount of Ce loading, the impregnating solution was formulated. In order to prevent metal ions from hydrolyzing to form hydroxide or oxide precipitation, a small amount of nitric acid was added to the impregnating solut...

Embodiment 2

[0019] Weigh 20g specific surface area is 30m 2 / g modified α-Al 2 o 3 Two parts of carrier, according to 1wt%Pd+0.2wt%Ti+0.2wt%Ce / α-Al 2 o 3 Content preparation catalyst, its steps are as follows: choose tetrabutyl titanate, prepare impregnating liquid according to Ti loading amount, loading amount is formulated into impregnating liquid, in order to prevent titanium from being hydrolyzed, dissolve and prepare ethanol solution with absolute ethanol dried through molecular sieves, The prepared modified α-Al 2 o 3 After the carrier was immersed in the solution for 10 hours, it was vacuum-dried for 6 hours to obtain a solid. Select Ce(NO 3 ) 3 According to the amount of Ce loading, the impregnating solution was formulated. In order to prevent metal ions from hydrolyzing to form hydroxides or oxides, a small amount of nitric acid was added to the impregnating solution to make the pH of the impregnating solution = 6.5, and then the α-Al 2 o 3Soak in the soaking solution fo...

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Abstract

The present invention belongs to the oxalate preparation technical field and aims to provide a catalyst for synthesis of low pressure, high activity and high selectivity oxalate in a CO low-pressure gas phase, and a preparation method for the catalyst. The catalyst mainly uses the palladium metal as a main activated component, titanium and cerium as a promoter, and modified Alfa-Al2O3 as a carrier. The select content of palladium metal is 0.1 to 3.0 percent of the carrier weight, the content of the titanium metal is 0.02 to 1.5 percent of the carrier weight, and the content of the cerium metal is 0.01 to 0.75 percent of the carrier weight. The catalyst is manufactured with the method of immersion. The catalyst is manufactured with the method of immersion. Proven by experiments, the catalyst of the present invention is provided with the very high reaction activity and oxalate selectivity in the reaction to synthesize dimethyl oxalate or diethyl oxalate with carbon monoxide and nitrite. Moreover, the catalyst can resist affection by oxygen, hydrogen, water steam and other impurities. The catalyst is provided with the long usable life and the stable reaction performance, and can be easily controlled.

Description

technical field [0001] The invention belongs to the technical field of oxalate preparation, and further relates to a catalyst for CO low-pressure gas-phase synthesis of oxalate and a preparation method thereof. Background technique [0002] Oxalate is an important chemical raw material, which can be used to prepare oxalic acid, ethylene glycol, carbonate, oxalamide, oxalyl chloride, intermediates of drugs and dyes, plastic accelerators and solvents, etc. [0003] At present, the method of esterification and dehydration of oxalic acid and alcohol (methanol, ethanol, etc.) with toluene as a dehydrating agent is still used in China to produce dialkyl oxalate (dimethyl oxalate, diethyl oxalate). One of its main raw materials, oxalic acid, is produced by the sodium formate method. Sodium formate is synthesized by CO and sodium hydroxide at 160°C and a pressure of 1.56-1.96MPa, and then concentrated and dehydrogenated at 400°C to form sodium oxalate, which is then reacted with lea...

Claims

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Application Information

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IPC IPC(8): B01J23/63C07C69/36C07C67/00
Inventor 王保伟马新宾许根慧
Owner TIANJIN UNIV
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