co vapor phase synthesis of oxalate
A gas-phase synthesis and oxalate ester technology, which is applied in the direction of chemical instruments and methods, heterogeneous catalyst chemical elements, carbon monoxide or formate reaction preparation, etc., can solve the problems of low utilization rate of precious metals, high cost of catalysts, high content of precious metals in catalysts, etc. problems, to achieve the effects of shortened residence time, high combustion activity, and high effective utilization
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Embodiment 1
[0038] Take 60g from Al 2 o 3 For the coating and the cordierite honeycomb ceramic as the carrier of the inert core, the thickness of the coating is 80 μm. Take 0.03g of palladium chloride and 0.56g of lanthanum nitrate to prepare a 30ml solution as impregnation solution Ⅰ. Slowly add the impregnating solution I into the carrier, and turn the carrier to make the solution impregnate evenly, so as to prepare the catalyst precursor. The catalyst precursor was aged in the air for 20 hours, dried at 80°C, and then roasted in a muffle furnace at 450°C. After roasting, a carbon monoxide gas-phase synthesis oxalate catalyst was obtained. The catalyst composition was tested to be 0.03%Pd+0.3%La +80μm thick Al 2 o 3 The coating and cordierite honeycomb ceramics are the carrier of the inert core, and the distribution depth of Pd and La is 80 μm.
[0039] Get 40g and make catalyst and pack in reaction tube, feed hydrogen at volume space velocity and be 500 hours -1 , the temperature...
Embodiment 2
[0041] According to the preparation method of [Example 1], except that the catalyst composition is 0.01%Pd+1%Ce+150μm thick TiO 2 The coating and cordierite honeycomb ceramics are the carrier of the inert core, and the distribution depth of Pd and Ce is 150 μm.
[0042] Take 40 g of the prepared catalyst and put it into a reaction tube, feed hydrogen gas at a volume space velocity of 500 h −1 , and program the temperature to 200° C. for reduction for 6 hours. Then at a reaction temperature of 130°C, a reaction pressure of 0.2 MPa, a molar ratio of CO to methyl nitrite of 1.5, and a volumetric space velocity of 3000 h -1 Under the conditions of carbon monoxide gas phase synthesis of oxalate, the space-time yield of oxalate is 746g / L.cat.H, and the catalyst stability is 7000 hours.
Embodiment 3
[0044] According to the preparation method of [Example 1], except that the catalyst composition is 0.05%Pd+1%Sm+150μm thick SiO 2 The coating and cordierite honeycomb ceramics are the carrier of the inert core, and the distribution depth of Pd and Sm is 40 μm.
[0045] Take 40 g of the prepared catalyst and put it into a reaction tube, feed hydrogen gas at a volume space velocity of 500 h −1 , and program the temperature to 200° C. for reduction for 6 hours. Then, at a reaction temperature of 120°C, a reaction pressure of 0.5 MPa, a molar ratio of CO to methyl nitrite of 1.5, and a volumetric space velocity of 1000 h -1 Under the conditions of carbon monoxide gas phase synthesis of oxalate, the space-time yield of oxalate is 720g / L.cat.H, and the catalyst stability is 9500 hours.
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