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Production method of catalyst dilution loading oxalate

A production method and catalyst technology, applied in the direction of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve the problems of low oxalate selectivity, low single-pass conversion rate of raw materials, etc., and achieve the effect of good technical effect

Inactive Publication Date: 2014-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is the low single-pass conversion rate of raw materials in the prior art and the low selectivity of oxalate esters. A new method for producing oxalate esters with catalyst dilution and loading is provided. High, good oxalate selectivity characteristics

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The reactor for CO coupling production of dimethyl oxalate is a fixed-bed reactor with tubes, the catalyst is installed inside the tubes, and the cooling medium is outside the tubes. The molar ratio of CO and methyl nitrite entering the reactor is 1.5:1, the feed temperature is 100°C, the pressure is 0.3MPa, and the catalyst is Pd / Al 2 o 3 The catalyst only supports palladium, based on the weight of elemental palladium, the amount of oxides selected from palladium is 0.8% by weight. The tubes contain two stages of catalyst beds, the height of the upper and lower catalyst beds is H 2 / H 1 =2:1, the upper catalyst bed is a homogeneous mixture of catalyst and inert alumina carrier, the volume ratio of inert alumina carrier to catalyst is 0.5:1, and the lower catalyst bed only contains catalyst. Under the above conditions, according to the present invention, the CO coupling synthesis of dimethyl oxalate is designed, the single-pass conversion rate of methyl nitrite is 85...

Embodiment 2

[0019] The reactor for CO coupling to produce dimethyl oxalate is a tubular fixed-bed reactor with a catalyst outside the tube and a cooling medium inside the tube. The form of the reactor is the same as that in Chinese patent 200910057857.6. The molar ratio of CO and methyl nitrite entering the reactor is 1.2:1, the feed temperature is 70°C, the pressure is 0.1MPa, and the catalyst is Pd-Ti / Al 2 o 3 Catalyst, based on the weight of elemental palladium, the amount of oxides selected from metal palladium and palladium is 2% by weight, the auxiliary agent Ti is based on the weight of elemental titanium, and the amount of oxides selected from titanium is 0.2% by weight %. The tubes contain three catalyst beds, and the height ratio of the three catalyst beds is H 3 / H 2 / H 1 =3:1.5:1, the first catalyst bed is a homogeneous mixture of catalyst and inert alumina carrier, the volume ratio of inert alumina carrier to catalyst is 2:1, the second catalyst bed is catalyst and inert ...

Embodiment 3

[0022] The reactor for CO coupling to produce diethyl oxalate is a fixed-bed reactor with tubes, the catalyst is installed inside the tubes, and the cooling medium is outside the tubes. The molar ratio of CO and ethyl nitrite entering the reactor was 5:1, the feed temperature was 140°C, the pressure was 1.0MPa, and the catalyst was Pd-Ni / (Al 2 o 3 +SiO2 2 ) catalyst, based on the weight of elemental palladium, the amount selected from the oxide of palladium is 0.15% by weight, the additive Ni is based on the weight of elemental nickel, and the amount selected from metal nickel is 2% by weight, in the tube Contains three-stage catalyst bed, the height ratio of the three-stage catalyst bed is H 3 / H 2 / H 1 =5:3:1, the first catalyst bed is a homogeneous mixture of catalyst and inert alumina and inert silica mixture carrier, the volume ratio of inert filler to catalyst is 3:1, the second catalyst bed is catalyst and Uniform mixture of inert alumina carrier, the volume ratio ...

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Abstract

The invention relates to a production method of catalyst dilution loading oxalate, which mainly solves the problems of low raw material per-pass conversion and low oxalate selectivity in the prior art. With the adoption of the technical scheme that CO and nitrite at a mole ratio of (1-5):1 are introduced to a fixed bed reactor as raw materials at the feed temperature of 60-160 DEG C, and perform contact reaction with a palladium-bearing catalyst at the pressure of 0-1.5MPa, heat generated by the reaction is removed by heat exchange timely, the reactor comprises at least two catalyst bed layers, the height of each catalyst bed layer is Hn, Hn / H1 is equal to (1-5):1 by taking the height H1 of the first bed layer at the upper part as a reference, a volume ratio of inert filler without catalyst activity to a catalyst is (0-4):1, and the volume ratios of the catalyst in the bed layers from the top down are gradually increased, the problems are better solved, and the method can be used for industrial production of oxalate.

Description

technical field [0001] The present invention relates to a kind of oxalate ester production method of catalyst dilution packing, more specifically, relate to a kind of gas phase method CO and methyl nitrite or ethyl nitrite react in the tubular fixed-bed reactor of catalyst dilution packing Process for producing dimethyl oxalate or diethyl oxalate. Background technique [0002] Oxalate is an important chemical raw material, which can be used to prepare oxalic acid, ethylene glycol, carbonate, oxamide, intermediates of drugs and dyes, plastic accelerators and solvents, etc. [0003] The traditional production route of oxalate is the method of esterification and dehydration of oxalic acid and alcohol with toluene as the dehydrating agent. The production process is long, the energy consumption is high, the pollution is serious, and the cost is high. It is urgent to find a new process route. The gas-phase catalyzed synthesis of oxalate from CO and nitrite opens up a new and impo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/36C07C67/36
CPCC07C67/36
Inventor 孙凤侠蒯骏赵焱
Owner CHINA PETROLEUM & CHEM CORP
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