Preparation method of oxalate by CO gas phase coupling synthesis using regular catalyst

A production method and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve problems such as increasing the production cost of oxalate, and achieve improved performance Observation of activity, reduction of reaction pressure, and improvement of mass transfer efficiency

Active Publication Date: 2010-10-06
TIANJIN UNIV +2
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, many scholars at home and abroad have made some progress in the selection of catalysts, activity and carrier effects, and pro

Method used

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Examples

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preparation example Construction

[0022] The method for preparing the above-mentioned regular structure catalyst provided by the present invention includes the following steps:

[0023] (1) Preparation of ball mill sol: mix one or more metal nitrates, hydroxides or oxides, add dilute nitric acid with a concentration of 1-15 wt.%, control the PH value of 1-4, and pass the ball mill ( Planetary ball mill XQM-2L, Nanjing Sunco) After ball milling at 200 rpm for 1-48 hours, the ball mill rubber for coating the carrier is prepared;

[0024] (2) Carrier coating load: use the above ball mill rubber to carry out the carrier coating load on the cordierite ceramic honeycomb carrier or metal honeycomb carrier by a known dip coating method, and then dry at 70-130°C for 2-4 hours, It is fired in a muffle furnace at 900-1200°C for 1-12 hours to form a carrier coating. The coating load is 5-50wt.% of the honeycomb carrier. It must be used multiple times to obtain a high load coating. Dip coating method;

[0025] (3) Loading of ac...

Embodiment 1

[0029] Catalyst preparation

[0030] Weigh 12.5g γ-Al 2 O 3 , 3.5gAlOOH, 6.5gAl(OH) 3 And 8.0gAl(NO 3 ) 3 And 100ml dilute HNO with a mass concentration of 10% 3 The solution was milled by a ball mill for 16 hours to prepare an alumina slurry for later use.

[0031] Put 400 holes / square inch cordierite ceramic honeycomb carrier (Φ25mm×25mm) in a muffle furnace at 700℃ for 2 hours to remove organic impurities, and then use conventional dip coating method to load the alumina coating. The dip coating slurry is the above alumina After uploading the slurry, it was microwave dried and weighed. After 3 dip coating, the alumina loading amount reached 20wt.%, then heated in a muffle furnace to 1200°C for 4 hours, and then exposed to PdCl 2 -FeCl 3 Soak in hydrochloric acid solution for 5 minutes, in which PdCl 2 And FeCl 3 The molar concentrations of are 0.2M and 0.13M respectively, use H after drying 2 Reduced at 500°C for 4 hours to obtain a catalyst 1.0%Pd-Fe / 20%α-Al with a Pd content of ...

Embodiment 2

[0035] Except that the reaction pressure is controlled at 0.6 MPa, everything else is the same as in Example 1. The reaction results are shown in Table 1.

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Abstract

The invention relates to a preparation method of oxalate by CO gas phase coupling synthesis using a regular catalyst. In the method, a fixed bed reactor is adopted, a catalyst bed consists of a regular structural catalyst loaded with noble metal; CO and vaporized nitrite are introduced into a reactor for reacting on the regular catalyst so as to generate the oxalate at the conditions that the pressure is 0.1-2MPa, the reaction temperature is 80-200 DEG C, and N2 is taken as a carrier gas, wherein the volume ratio of the materials is as follows: N2:CO:nitrite is 20-80:5-60:10-40, and the retention time is 0.5-10 hours. The method of the invention improves mass transfer efficiency of the reaction materials between the gas phase and the solid phase or among the gas phase, the liquid phase and the solid phase, increases the contact area of the reaction materials and the catalyst and reduces the usage amount of the catalyst in the noble metal, wherein the usage amount of the catalyst noblemetal Pd is saved by more than 86%. The method of the invention has the characteristics of high catalyst activity, low cost, convenient and fast replacement and the like, and is beneficial for realizing large-scale engineered application.

Description

Technical field [0001] The present invention relates to the synthesis of oxalate, in particular to a production method for synthesizing oxalate by CO gas phase coupling using a regular catalyst. Background technique [0002] In view of the current situation of more coal and less oil in my country, the use of coal or natural gas to replace petroleum ethylene to synthesize ethylene glycol is a major C1 chemical technology with the most scientific raw material route, the most reasonable resource utilization, and significantly better than the petroleum route. As an important intermediate product, the synthesis of oxalate is of great significance to my country's strategic goal of "replacement of petroleum ethylene with coal or natural gas to synthesize ethylene glycol". In addition, oxalate is also an important organic chemical raw material, which is widely used in fine chemicals to prepare various dyes, medicines, important solvents, extractants and various intermediates. [0003] The...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36B01J35/04B01J23/89
Inventor 马新宾赵玉军王保伟吕静王胜平李振花徐艳
Owner TIANJIN UNIV
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