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Structured catalyst for synthesizing oxalate by CO gaseous-phase coupling and preparation method thereof

A catalyst and oxalate technology, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, carbon monoxide or formate reaction preparation, etc., can solve the problems of increasing the production cost of oxalate, and achieve saving process operation costs, The preparation method is simple and the effect of reducing the amount of use

Active Publication Date: 2012-07-18
TIANJIN UNIV +2
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  • Summary
  • Abstract
  • Description
  • 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 process operating conditions, and believe that α-Al 2 o 3 etc. are more suitable catalyst supports, but the use of noble metal Pd as the active component of the catalyst increases the production cost of oxalate

Method used

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  • Structured catalyst for synthesizing oxalate by CO gaseous-phase coupling and preparation method thereof
  • Structured catalyst for synthesizing oxalate by CO gaseous-phase coupling and preparation method thereof
  • Structured catalyst for synthesizing oxalate by CO gaseous-phase coupling and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Preparation of coating precursor slurry

[0036] Weigh 12.5g γ-Al 2 O 3, 3.5gAlOOH, 6.5gAl(OH) 3 and 8.0gAl(NO 3 ) 3 and 100ml of 10wt.% dilute HNO 3 The solution was ball milled by a ball mill (planetary ball mill XQM-2L, Nanjing Shunchi) at a rotational speed of 200 rpm for 16 hours to obtain an alumina sol for later use.

[0037] catalyst preparation

[0038] A 400-hole / square inch cordierite ceramic honeycomb carrier (Φ25mm×25mm) was placed in a muffle furnace for calcination at 700°C for 2 hours to remove organic impurities, and then a conventional dip coating method was used to load the alumina coating, and the dip coating slurry was the above alumina The slurry was microwave-dried and weighed after uploading. After 3 dip-coating, the alumina loading reached 20 wt. 2 -FeCl 3 Immersion in hydrochloric acid solution for 5 minutes in which PdCl 2 and FeCl 3 The molar concentrations of 0.2M and 0.13M were used after drying with H 2 Reduction at 500°C for 4 ...

Embodiment 2

[0042] The process is the same as that of Example 1, except that the skeleton carrier adopts a cordierite ceramic honeycomb carrier with 600 pores / square inch. A catalyst with a Pd content of 1.0 wt.% (relative to the alumina coating) and a Pd / Fe atomic ratio of 1.5:1 was obtained 1.0%Pd-Fe / 20%α-Al 2 O 3 / Cordierite. The reaction results are shown in Table 1.

Embodiment 3

[0044] Except that the ball milling time of the ball mill is 4.5 hours, other processes are the same as in Example 1, and the catalyst 1.0%Pd-Fe / 20%α-Al is obtained 2 O 3 / Cordierite (Pd / Fe atomic ratio 1.5:1). The reaction results are shown in Table 1.

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Abstract

The invention provides a structured catalyst for synthesizing oxalate by CO gaseous-phase coupling and a preparation method thereof. In the catalyst, a ceramic honeycomb or metal honeycomb is used as a skeletal carrier, the aluminum oxide, silicon oxide and titanium oxide and the like are used as carrier coatings, precious metals such as Pt, Pd, Ir, Rh and the like are used as active ingredients,and Fe, CO, Ni and the like are used as additives, wherein the carrier coating accounts for 5 to 50 percent of the weight of the honeycomb carrier; the active ingredients of the catalyst account for 0.1 to 5 percent of the weight of the carrier coating; the additives of the catalyst account for 0.3 to 10 percent of the weight of the carrier coating; and the atomic ratio of the active ingredients to the additives is 0.1 to 3. In the structured catalyst of the invention, the active ingredients are limited in the carrier coating, so that the using amount of the precious metal Pd is reduced. Meanwhile, the structured catalyst and the preparation method thereof reduce the loss of the catalyst caused by wear in the processes of catalyst filling and using, reduce the using cost of the catalyst and the production cost of the oxalate, and contribute to realize the large-scale industrial production.

Description

technical field [0001] The invention relates to the synthesis of oxalate, in particular to a regular catalyst for synthesizing oxalate by gas-phase coupling of CO and a preparation method thereof. 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 instead of 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 obviously superior to the petroleum route. Oxalate is an important intermediate product, and its synthesis is of great significance to our country's strategic goal of "replacing 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] T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J35/04B01J23/89C07C69/36C07C67/36
Inventor 马新宾高晓晨赵玉军王保伟王胜平吕静李振花徐艳
Owner TIANJIN UNIV