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
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[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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