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Catalyst reduction method

A catalyst and auxiliary technology, applied in molecular sieve catalysts, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problems of low conversion rate of raw materials, low selectivity of target products, easy to fly over temperature of catalyst bed, etc. The effect of technical effects

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 that in the past literature, in the reduction process of oxalate ester hydrogenation into ethylene glycol catalyst, there is a catalyst bed layer that is easy to fly over temperature, which leads to low conversion rate of raw materials in the reaction process of the catalyst after reduction, and the target product selection In order to solve the technical problem of low stability, a new method for catalyst reduction is provided, which has the advantages of stable catalyst bed temperature during the reduction process of oxalate ester hydrogenation into ethylene glycol catalyst, and the conversion rate of raw materials in the reaction process of the reduced catalyst High, high selectivity of the target product, etc.

Method used

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Experimental program
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Effect test

Embodiment 1

[0024] Catalyst preparation:

[0025] Weigh 200 grams of silica carrier with a specific surface area of ​​280 square meters / g, and configure the catalyst according to the content of 35 parts of active metallic copper and 10 parts of metallic zinc. The steps are as follows: select copper nitrate and zinc nitrate, according to the Cu and Zn loadings Prepare an impregnation solution, immerse the silica carrier in the solution for 18 hours, and then vacuum dry at room temperature for 10 hours to obtain a solid. Dry the solid at 120°C for 10 hours, and calcinate at 450°C for 4 hours to obtain the required 30%CuO+10%ZnO / SiO 2 The catalyst precursor is referred to as A-I.

[0026] Weigh the 30%CuO+10%ZnO / SiO to be prepared 2 The catalyst precursor A-I is 50 grams, and the required amount is charged into two tubular reactors with a diameter of 24 mm. A mixed gas with a hydrogen volume content of 60% and a nitrogen volume content of 40% is used as the reduction feed gas. The restoration me...

Embodiment 2

[0031] Prepare 40% CuO + 8% Zn O + 0.2% CeO according to the steps and conditions of Example 1 2 / SiO 2 The catalyst precursor, denoted as B-I.

[0032] Weigh the 40% CuO + 8% Zn O + 0.2% CeO that will be prepared 2 / SiO 2 The catalyst precursor B-I is 50 grams, and the required amount is charged into two tubular reactors with a diameter of 24 mm, and a mixed gas with a volume content of hydrogen of 60% and a volume of nitrogen of 40% is used as the reduction feed gas. The restoration method is shown in Table 2:

[0033] Table 2

[0034]

[0035] The catalyst obtained after reduction by the above reduction scheme is referred to as catalyst B.

Embodiment 3

[0037] 30%CuO+2%BaO+0.2%La were prepared according to the steps and conditions of Example 1 2 O 3 / SiO 2 The catalyst precursor of, denoted as C-I.

[0038] Weigh the 30%CuO+2%BaO+0.2%La to be prepared 2 O 3 / SiO 2 The catalyst precursor C-I is 50 grams, and the required amount is charged into a two-tube reactor with a diameter of 24 mm. A mixed gas with a volume content of hydrogen of 70% and a volume of nitrogen of 30% is used as the reduction feed gas. The restoration method is shown in Table 3:

[0039] table 3

[0040]

[0041] The catalyst obtained after reduction by the above reduction scheme is referred to as catalyst C.

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Abstract

The invention relates to a catalyst reduction method, which mainly solves the technical problems in traditional technology that the catalyst beds are liable to temperature runaway in the reduction process of hydrogenating oxalic ester to ethylene glycol catalyst so that the reduced catalyst has low conversion rate of raw materials in the reaction process and the target product is low in selectivity. The method solves the above problems favorably by adopting the following technical proposal that, the raw materials containing hydrogen or CO gas come into contact with the catalyst under the conditions that the hourly space velocity is 1000 to 10000hr-1, the pressure of reduction reaction is 0 to 6.0MPa, the reduction temperature is 20 to 450 DEG C, the reduced heating is staged with the heating rate controlled to be less than 50 DEG C per hour, and the temperature difference of beds is less than 40 DEG C, high valence metallic elements in the catalyst are reduced to low valence active metallic elements or metal elements; thus the method can be used for the industrial production of ethylene glycol by hydrogenated oxalic ester.

Description

Technical field [0001] The invention relates to a catalyst reduction method, in particular to a catalyst reduction method for hydrogenating dimethyl oxalate or 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, non-ionic surfactant and explosives, etc. It can be used in coatings, photographic developer, brake fluid, ink and other industries, used as a solvent and medium for ammonium perborate, and used in the production of special solvent glycol ethers. It has a wide range of uses. [0003] At present, my country has surpassed the United States to become the world's largest ethylene glycol consumer. The average annual growth rate of domestic apparent consumption from 2001 to 2006 reached 17.4%. Although my country's ethylene glycol production capacity and output have grown rapidly, due ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/18B01J37/16B01J23/80B01J23/83B01J23/889B01J29/48B01J29/68B01J23/835C07C31/20C07C29/149
CPCY02P20/52
Inventor 刘俊涛李斯琴张惠明蒯骏
Owner CHINA PETROLEUM & CHEM CORP