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Catalyst start-up method

A catalyst, copper catalyst technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem of low selectivity of ethylene glycol

Active Publication Date: 2011-12-14
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 this invention is that there is a low technical problem of ethylene glycol selectivity in the initial stage of start-up of oxalate ester hydrogenation into ethylene glycol catalyst in previous documents, and a new method of catalyst start-up is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Catalyst preparation:

[0024] Take by weighing 200 grams of a silicon oxide carrier with a specific surface area of ​​280 square meters per gram, configure the catalyst according to the content of 35 parts of active metal copper and 10 parts of metal zinc, the steps are as follows: select copper nitrate, and zinc nitrate, according to Cu and Zn loading Prepare an impregnating solution, impregnate the silicon oxide carrier in the solution for 18 hours, and then vacuum-dry at room temperature for 10 hours to obtain a solid. The solid was then dried at 120°C for 10 hours and calcined at 450°C for 4 hours to obtain the required 30%CuO+10%ZnO / SiO 2 catalyst precursor.

[0025] Weigh the prepared 30%CuO+10%ZnO / SiO 2 The catalyst precursor is 50 grams, which is loaded into a tubular reactor with a diameter of 18 mm, and hydrogen is used as the reducing gas. At a volumetric space velocity of 2000 hours -1 , the reduction pressure is 0.5MPa, and the reduction temperature is 3...

Embodiment 2

[0027] Adopt the same catalyzer of embodiment 1, just the reduction condition of catalyzer is that the volume space velocity is 3500 hours -1 , the reduction pressure is 2.5MPa, and the reduction temperature is 200°C. After 8 hours of reduction, the temperature is lowered to 185°C in a hydrogen atmosphere. At a pressure of 2.5MPa, the weight space velocity of dimethyl oxalate is 0.8 hours. -1 , under the condition that the hydrogen ester molar ratio is 80:1, dimethyl oxalate is put into the reactor, and after being stable for 18 hours, the temperature is raised to the normal reaction temperature of the catalyst at 200°C to continue the reaction. During the whole reaction process, the conversion of dimethyl oxalate The ratios are all 100%, and the selectivity of ethylene glycol is 95.8%.

Embodiment 3

[0029] Prepare 40%CuO+8%ZnO+0.2%CeO according to the various steps and conditions of Example 1 2 / SiO 2 The catalyst precursor is loaded into the reactor with the same loading amount, and the reduction condition of the catalyst is that the volume space velocity is 1000 hours -1 , the reduction pressure is 1.5MPa, and the reduction temperature is 250°C. After reduction for 20 hours, the temperature is lowered to 170°C in a hydrogen atmosphere. At a pressure of 2.8MPa, the weight space velocity of dimethyl oxalate is 0.4 hours. -1 , under the condition that the hydrogen ester molar ratio is 120:1, dimethyl oxalate is put into the reactor, and after being stable for 40 hours, the temperature is raised to the normal reaction temperature of the catalyst at 210°C to continue the reaction. During the whole reaction process, the conversion of dimethyl oxalate The ratios are all 100%, and the selectivity of ethylene glycol is 96.5%.

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PUM

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Abstract

The invention relates to a catalyst starting method for mainly solving the technical problem of low selectivity of ethylene glycol in the initial starting period when oxalate is hydrogenated into the ethylene glycol in the prior art. In a technical scheme adopted by the invention, the catalyst starting method comprises the following steps of: (1) loading a copper-containing catalyst into a reactor, introducing a reducing gas to reduce the catalyst under a reduction condition; (b) placing the reduced catalyst in a hydrogen atmosphere by maintaining the volume velocity of hydrogen to be 50-5000 h<-1>, controlling the temperature to enable the temperature of the reactor to be 5-50 DEG C lower than a design temperature for normal reaction; and (c) maintaining system pressure to be 0.5-5.0MPa, and introducing an oxalate raw material for reaction to generate an effluent containing the ethylene, wherein after the oxalate raw material is introduced for reaction for 4-100 hours, the temperature is raised to a design condition for reaction. By means of the technical scheme, the problem is favorably solved, and the catalyst starting method is suitable for the industrial production of catalyst starting for hydrogenating the oxalate into the ethylene glycol.

Description

technical field [0001] The invention relates to a method for starting a catalyst, in particular to a method for starting a catalyst for hydrogenating dimethyl oxalate or diethyl oxalate into 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, my country has surpassed the United States to become the world's largest consumer of ethylene glycol. From 2001 to 2006, the average annual growth rate of domestic apparent consumption reached 17.4%. Although my country's ethylene glycol production capacity and outpu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/149
Inventor 刘俊涛王万民
Owner CHINA PETROLEUM & CHEM CORP