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Method for parking reactor

A technology of reactor and oxalate ester, which is applied in chemical instruments and methods, preparation of organic compounds, production of bulk chemicals, etc., can solve the problems of low selectivity of reaction product ethylene glycol and reduction of catalyst activity, etc.

Active Publication Date: 2014-08-13
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 the technical problem that the catalyst activity is reduced during the shutdown process of the reactor and the selectivity of the reaction product ethylene glycol is low in the previous literature.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take by weighing 500 grams of silicon oxide carriers whose specific surface area is 200 square meters per gram, configure the catalyst according to the content of 30% active metal copper and 5% additive metal zinc, and the steps are as follows: select copper nitrate and zinc nitrate, according to Cu and Zn loading The amount was prepared as an impregnating solution, and the silicon oxide carrier was immersed in the solution for 24 hours, and then vacuum-dried at room temperature for 12 hours to obtain a solid. Then the solid was dried at 120°C for 12 hours, and after roasting at 450°C for 4 hours, 200 ml / min of gas containing a hydrogen mixture (hydrogen molar content 20%, nitrogen molar content 80%) was activated at 450°C for 6 hours to obtain required catalyst.

[0021] Weigh 20 grams of the above-mentioned copper-containing solid oxide catalyst sample, put it into a fixed-bed reactor, use dimethyl oxalate as a raw material, and use dimethyl oxalate as a raw material ...

Embodiment 2

[0023] According to the catalyst and various steps and conditions of [Example 1], only the shutdown steps are as follows: (a) keep the temperature at 260 ° C, the pressure at 2.0 MPa, and the hydrogen volume space velocity at 3000 hours -1 Under the conditions, gradually stop the reactor oxalate feed in 20 hours; (b) keep it for 10 hours in the presence of hydrogen; (c) reduce the reactor temperature to 60 °C in 20 hours; (d) use methane gas Displacing reaction gas. After that, dimethyl oxalate is still used as raw material, at a reaction temperature of 210°C, a reaction pressure of 3.0 MPa, and a reaction space velocity of 0.5 hours -1 The reaction was carried out for 10 hours under the condition that the reaction hydrogen / ester molar ratio was 80:1, and the reaction result was that the conversion rate of oxalic acid ester was 100%, and the selectivity of ethylene glycol was 97.1%.

Embodiment 3

[0025] According to the catalyst and various steps and conditions of [Example 1], only the shutdown steps are as follows: (a) keep the temperature at 230 ° C, the pressure at 1.0 MPa, and the hydrogen volume space velocity at 6000 hours -1 Under the conditions, gradually stop the oxalate feed to the reactor in 2 hours; (b) keep it for 4 hours in the presence of hydrogen; (c) reduce the temperature of the reactor to 30 ° C in 15 hours; (d) use argon Displacing reaction gas. After that, dimethyl oxalate is still used as raw material, at a reaction temperature of 210°C, a reaction pressure of 3.0 MPa, and a reaction space velocity of 0.5 hours -1 The reaction was carried out for 10 hours under the condition that the reaction hydrogen / ester molar ratio was 80:1, and the reaction result was that the conversion rate of oxalic acid ester was 100%, and the selectivity of ethylene glycol was 95.8%.

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Abstract

The invention relates to a method for parking a reactor, and mainly solves the technical problems in the prior art that during the parking of the reactor, the activity of a catalyst is reduced, and the selectivity of the hydrogenated product, namely ethylene glycol is low. Through the adoption of the technical scheme that oxalic ester and hydrogen are taken as raw materials, a copper contained solid oxide is taken as a catalyst, and the method comprises the following steps: (a) the temperature is kept to 180 to 260 DEG C, the pressure is 0.2 to 10 MPa, and the volume space velocity of hydrogen is 200 to 8,000 hours<-1>, the feeding of oxalic ester in the reactor is stopped step by step within 0.1 to 40 hours; (b), under the hydrogen atmosphere, the feeding stop is kept for 0.2 to 30 hours; (c) the reaction temperature is reduced to 20 to 100 DEG C within 1 to 60 hours; and (d) reaction gas is replaced with conversion gas, wherein the conversion gas is selected from at least one of nitrogen, methane, helium or argon, and the invention solves the problems, and can be used for parking the reactor in the industrial production of increasing the yield of ethylene glycol.

Description

technical field [0001] The invention relates to a method for shutting down a reactor, in particular to a method for improving the shutting down of a reactor during hydrogenation of dimethyl oxalate or hydrogenation of diethyl oxalate to ethylene glycol. Background technique [0002] Ethylene glycol (EG) is an important organic chemical raw material, mainly used in the production of polyester fiber, antifreeze, unsaturated polyester resin, lubricant, plasticizer, nonionic surfactant and explosives, etc. It can be used in industries such as paint, photographic developer, brake fluid and ink, as a solvent and medium for ammonium perborate, and for the production of special solvents such as glycol ether, etc., and has a wide range of uses. [0003] At present, large-scale ethylene glycol production at home and abroad adopts the process route of direct hydration or pressurized hydration. This process is to prepare a mixed aqueous solution of ethylene oxide and water at a ratio of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/20C07C29/149
CPCY02P20/52
Inventor 刘俊涛孙凤侠王万民
Owner CHINA PETROLEUM & CHEM CORP
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