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Method for producing oxalic ester by gas phase CO coupling

A technology of oxalate ester and gas phase method, which is applied in chemical instruments and methods, carbon monoxide or formate reaction preparation, organic chemistry, etc. It can solve the problems of low single-pass conversion rate of raw materials and low selectivity of target product oxalate

Active Publication Date: 2011-03-30
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 selectivity of the target product oxalate in the prior art, and the low problem of raw material single-pass conversion, and a new CO gas-phase method coupling production method for oxalate is provided. It has the characteristics of high single-pass conversion rate of raw materials and good selectivity of oxalate

Method used

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  • Method for producing oxalic ester by gas phase CO coupling
  • Method for producing oxalic ester by gas phase CO coupling
  • Method for producing oxalic ester by gas phase CO coupling

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Experimental program
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Embodiment 1

[0026] according to figure 1 , 2 reactors in series, the diameter of the first tubular fixed-bed reactor RA is 1.5 meters, the diameter of the second tubular fixed-bed reactor RB is 2.5 meters, and the cooling medium in the reactor RA is nitrous acid formazan The raw material gas is composed of ester and CO gas, and the cooling medium in the reactor RB is methyl nitrite. Both the palladium-containing catalyst I and the palladium-containing catalyst II in the two reactors are based on alumina as a carrier, and only palladium is loaded, and the amount of oxides selected from palladium is 0.8% by weight based on the weight of elemental palladium. The molar ratio of the total CO to the total methyl nitrite in the raw material is 1.5:1, and the molar ratio of the second methyl nitrite to the first methyl nitrite material is 0.2:1. according to figure 1 In the flow process, the first stream of raw material gas composed of CO and methyl nitrite with a molar ratio of CO and methyl n...

Embodiment 2

[0028] according to figure 1 , 2 reactors in series, the diameter of the first tubular fixed-bed reactor RA is 3 meters, the diameter of the second tubular fixed-bed reactor RB is 3 meters, and the cooling medium in the reactor RA is nitrite formazan The raw material gas is composed of ester and CO gas, and the cooling medium in the reactor RB is boiler water. The palladium-containing catalyst I in the reactor RA is Pd-Ni / Al 2 o 3 Catalyst, based on the weight of elemental palladium, the amount of oxides selected from metal palladium and palladium is 0.5% by weight, the auxiliary agent Ni is based on the weight of elemental nickel, and the amount of oxides selected from nickel is 0.8% by weight %, the palladium-containing catalyst II in the reactor RB 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 1% by weight, the auxiliary agent Ti is based on the weight of elemental titanium, an...

Embodiment 3

[0030] according to figure 2 , 2 reactors connected in series, the diameter of the first tubular fixed bed reactor RA is 2.5 meters, the diameter of the second tubular reactor RC is 3 meters, and the cooling medium in the reactor RA is Raw material gas composed of ethyl nitrite and CO gas. The palladium-containing catalyst I in the reactor RA is Pd-Ce / Al 2 o 3 Catalyst, by the weight of elemental palladium, the consumption that is selected from the oxide of palladium is that the weight content is 1%, auxiliary agent Ce is by the weight of elemental cerium, and the consumption that is selected from the oxide of cerium is that the weight content is 1.2%, reaction Catalyst II in RC is Pd-Ti / Al 2 o 3 The catalyst is based on the weight of elemental palladium, and the amount of oxides selected from palladium is 1% by weight, and the amount of auxiliary agent Ti is based on the weight of elemental titanium, and the amount selected from metal titanium is 0.1% by weight. The mol...

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Abstract

The invention relates to a method for producing oxalic ester by gas phase CO coupling, which mainly solves the problems of low selectivity of the target product oxalic ester and low conversion per pass of the raw materials in the prior art. In the method, a technical scheme is adopted as follows: CO and nitrous acid ester in mol ratio of 1-5:1 are used as raw materials; a first batch of raw material as a cooling medium passes through tubes of a first tube-type fixed bed reactor, after heat exchange, enters a second fixed bed reactor, contacts with a palladium-containing catalyst II in a catalyst bed II in the reactor for reaction to generate a reaction effluent I containing the oxalic ester; and a gas phase effluent II containing CO is obtained by gas-liquid separation of the reaction effluent I, and is uniformly mixed with a second batch of raw material containing the fresh component nitrous acid ester, and the mixture is returned into the first tube-type fixed bed reactor, contacts with a palladium-containing catalyst I in a catalyst bed I outside the tubes for reaction to generate the reaction effluent containing the oxalic ester, wherein the total mol ratio of CO to nitrous acid ester in the raw material is 1-4:1, the mol ratio of the second batch of nitrous acid ester to the first batch of nitrous acid ester material is 0.2-5:1, and at least two reactors are connected in series. By using the method, the problems can be better solved and the method can be used in the industrial production for increasing the yield of the oxalic ester.

Description

technical field [0001] The present invention relates to a method for producing oxalate by CO gas phase coupling, more specifically, relates to a gas phase reaction of CO and methyl nitrite or ethyl nitrite in a combined fixed bed reactor to produce dioxalate Methyl ester or diethyl oxalate method. Background technique [0002] Oxalate is an important chemical raw material, which can be used to prepare oxalic acid, oxalate, 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 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 important route for C1 chemical production of oxalate. Since the 1980s, fo...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36B01J8/02
Inventor 孙凤侠王万民张惠明蒯骏
Owner CHINA PETROLEUM & CHEM CORP
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