Process for producing a catalyst comprising an alkali metal and a transition metal in oxidised form
A technology of transition metals and alkali metals, applied in the direction of metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem of no observed positive impact on yield and selectivity , Methanol conversion rate and methyl mercaptan selectivity decrease, high yield of methyl mercaptan and selectivity duration is not long, etc.
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Embodiment 1
[0070] Embodiment 1 (comparative example):
[0071] As described in Example 2 (Comparative Example) on page 17 of WO 2013 / 092129 A1, when using 17.8% by weight of WO based on the total mass of the catalyst 3 and 17.3 wt% Cs 2 In the three-stage impregnation of O, impregnate 200 g of spherical alumina with a particle size of 2-5 mm (Spheralite 501A from Axens, with a pore volume of 45 ml / 100 g and a bulk density of 815 kg / m 3 ). The procedure adopted is as follows: 62.2g of tungstic acid is suspended in 130.4g of ammonia solution, and dissolved by stirring for about 30 minutes. To this solution was added 89.3 g of cesium hydroxide in water (70%), and the resulting solution was stirred for about 23-24 hours. Alumina was initially fed into a glass vessel evacuated to 150 mbar. The impregnation solution was aspirated off by opening the tap until there was approximately 4.5 cm of supernatant of the impregnation solution over the entire alumina. The glass vessel was vented unde...
Embodiment 2
[0072] Embodiment 2 (comparative example):
[0073] As described in Example 6 on pages 18 and 19 of WO 2013 / 092129 A1, 1.05 kg of powdered alumina (Spheralite 509A from Axens with a specific surface area of 335 m 2 / g, the pore volume is 56ml / 100g, and the bulk density is 840kg / m 3 ) is first mixed with solid tungstic acid, and then the mixture thus obtained is mixed with an aqueous calcium hydroxide solution. The steps it adopts are as follows: 1.05kg Spheralite 509A and 537.9g solid tungstic acid are kneaded at 40 rev / min and 11 rev / min in laboratory batch kneader (Coperion LUK 2.5, Weinheim, Stuttgart, Germany) Back pointing) to mix under the unloading screw, and the barrel of the kneader is cooled to 10°C with a cryostat. Then 740.5 g of a 70% by weight aqueous solution of cesium hydroxide were added over a period of 1 minute of continuous mixing, with a temporary temperature increase of 30-40°C. 10 minutes after the addition was complete, 127.5 grams of deionized wat...
Embodiment 3
[0074] Embodiment 3 (the present invention):
[0075] 150 g of powdered alumina (Spheralite 509A from Axens with a specific surface area of 335 m 2 / g, the pore volume is 56ml / 100g, and the bulk density is 840kg / m 3 ) with the WO of 17.8wt% based on the total mass of the catalyst 3 and 17.3 wt% Cs 2 O impregnation. The steps adopted are as follows: 63.8g of tungstic acid is dissolved in 127.7g of 25% ammonia solution. To this solution was added 121.3 g of cesium hydroxide aqueous solution (50.48%), and the solution was stirred for 24 hours. The solution was then brought to a volume of 243 ml by adding water. The solution thus obtained is called impregnation solution. The impregnation solution was first fed into a glass vessel and the alumina was added with constant stirring. Fifteen minutes after the addition was complete, the suspension was filtered off through a blue ribbon filter in a Nutsche filter. The filter cake was then dried at 120 °C for 3 hours to remove r...
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Abstract
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