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Method for CO gas phase coupling production of oxalate

A gas-phase coupling, oxalate technology, applied in chemical instruments and methods, heterogeneous catalyst chemical elements, carbon monoxide or formate reaction preparation, etc., can solve the problem of low space-time yield, low dispersion, The problem of large grain size of active component Pd, etc., achieves the effect of high space-time yield, stable pH value, and strong stability

Active Publication Date: 2014-10-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is that the particle size of the active component Pd grains of the catalyst in the prior art is relatively large, and the degree of dispersion is low, resulting in the problem of low space-time yield of oxalate. A new CO gas-phase coupling method is provided. Method for producing oxalate

Method used

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  • Method for CO gas phase coupling production of oxalate
  • Method for CO gas phase coupling production of oxalate
  • Method for CO gas phase coupling production of oxalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Take 60g Al 2 o 3 Put it in a muffle furnace and bake it at 1100°C for 4 hours to get modified α-Al 2 o 3 carrier. Prepare 50 milliliters of palladium chloride concentration and be 0.056 mol / liter solution, adjust pH with 10% (weight) sodium carbonate to be 3.0, and add complexing agent A to obtain impregnation solution I, the mol ratio of complexing agent and Pd is 2. Add impregnation solution I to the above α-Al 2 o 3 in the carrier, and the carrier is turned over to make the solution impregnated evenly, so as to obtain the catalyst precursor. The catalyst precursor was aged in the air for 2 hours, dried at 60°C, and then roasted in a muffle furnace at 300°C to obtain a CO coupling oxalate catalyst.

[0039]The catalyst is loaded into the reaction tube, and hydrogen gas is introduced at a volume space velocity of 500 hours -1 , the temperature was programmed to 200°C for 6 hours for reduction. Then, at a reaction temperature of 120°C, a reaction pressure of 0~...

Embodiment 2

[0042] Take 60g Al 2 o 3 Put it in a muffle furnace and bake at 1100°C for 6 hours to obtain modified α-Al 2 o 3 carrier. Prepare 50 milliliters of palladium chloride concentration and be 0.112 mol / liter solution, adjust pH with 10% (weight) sodium carbonate to be 4.0, and add complexing agent B to obtain impregnation solution I, the mol ratio of complexing agent and Pd is 0.05. Add impregnation solution I to the above α-Al 2 o 3 in the carrier, and the carrier is turned over to make the solution impregnated evenly, so as to obtain the catalyst precursor. The catalyst precursor was aged in the air for 8 hours, dried at 100°C, and then baked in a muffle furnace at 400°C to obtain a CO coupling oxalate catalyst.

[0043] The catalyst is loaded into the reaction tube, and hydrogen gas is introduced at a volume space velocity of 500 hours -1 , the temperature was programmed to 200°C for 6 hours for reduction. Then, at a reaction temperature of 140°C, a reaction pressure of...

Embodiment 3

[0046] Take 60g Al 2 o 3 Put it in a muffle furnace and bake at 1100°C for 8 hours to obtain modified α-Al 2 o 3 carrier. Prepare 50 milliliters of palladium chloride concentration and be 0.0033 mol / liter solution, adjust pH with 10% (weight) sodium carbonate to be 4.0, and add complexing agent C to obtain impregnation solution I, the mol ratio of complexing agent and Pd is 1. Add impregnation solution I to the above α-Al 2 o 3 in the carrier, and the carrier is turned over to make the solution impregnated evenly, so as to obtain the catalyst precursor. The catalyst precursor was aged in the air for 12 hours, dried at 130°C, and then roasted in a muffle furnace at 450°C to obtain a CO coupling oxalate catalyst.

[0047] The catalyst is loaded into the reaction tube, and hydrogen gas is introduced at a volume space velocity of 500 hours -1 , the temperature was programmed to 200°C for 6 hours for reduction. Then, at a reaction temperature of 140°C, a reaction pressure o...

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Abstract

The invention relates to a method for CO gas phase coupling production of oxalate, and mainly solves the problem of low space time yield of oxalate due to the large particle size and low dispersion of an active component Pd crystal grain in catalysts in the prior art. A technical scheme adopted in the invention is characterized in that carbon monoxide and organic nitrite raw materials contact with a palladium-containing catalsty under coupling reaction conditions, and a complexation additive is added into a dipping during the preparation of the catalyst. The technical scheme well solves the problem, and the method can be used in the industrial for the carbon monoxide gas phase coupling production of oxalate.

Description

technical field [0001] The invention relates to a method for producing oxalate through CO gas-phase coupling, in particular to a method for synthesizing dimethyl oxalate or diethyl oxalate through CO gas-phase coupling. Background technique [0002] Oxalate is an important organic chemical raw material, which is widely used in fine chemical industry to prepare various dyes, medicines, solvents, extractants and various intermediates. In addition, hydrogenation of oxalate can produce ethylene glycol, a very important chemical raw material, and this route can replace the current method of producing ethylene glycol by the petroleum route with high cost. [0003] Traditional oxalate production routes include starch nitric acid oxidation method, cellulose alkali fusion method, sodium formate method, ethylene glycol one-step oxidation method, propylene oxidation method and oxalate alcohol esterification reaction method, but the above-mentioned traditional processes have high cost a...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36B01J23/44
CPCB01J23/002B01J23/44B01J23/63B01J2523/00C07C67/36B01J2523/31B01J2523/3706B01J2523/3712B01J2523/3737B01J2523/824C07C69/36
Inventor 龚海燕刘俊涛刘国强
Owner CHINA PETROLEUM & CHEM CORP
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