A kind of preparation method of methanol dehydration preparation dimethyl ether catalyst
A methanol dehydration and catalyst technology, which is applied in the direction of ether preparation, dehydration of hydroxyl-containing compounds to prepare ether, chemical instruments and methods, etc., can solve the problems of many by-products, easy deactivation, easy carbon deposition, etc., and achieve high conversion rate and selectivity performance, avoid excessive cracking, and improve the effect of pore structure
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Embodiment 1
[0034] (1) Catalyst preparation:
[0035] Weigh 8.9g of lanthanum nitrate, 13.9g of phosphotungstic acid, 120g of cetyltrimethylammonium bromide and 168.8g of citric acid to form a mixed solution, add 249mL tetraethyl orthosilicate to the mixed solution, and stir for 2 h, then stirred at 70°C until it formed a gel, aged the gel at room temperature for 12 h, dried at 110°C for 8 h, and then calcined at 380°C for 3 h, the resulting solid was added to a C6 alkane solvent and immersed for 10 min, Then filter, dry at room temperature until there is no liquid phase on the surface of the carrier, add it to an aqueous solution containing 6.9g of phosphotungstic acid and 4.4g of lanthanum nitrate, stir at 70°C until the solution is evaporated to dryness, and dry the obtained solid at 110°C for 8.0 h, and then calcined at 450°C for 3.0 h to prepare the catalyst, La 2 o 3 The content is 5wt%, and the content of phosphotungstic acid and ammonium salt is 20%. Wherein the molar ratio of ...
Embodiment 2
[0039]Weigh 13.3g of lanthanum nitrate, 15.6g of phosphotungstic acid, 182.2g of cetyltrimethylammonium bromide and 96g of citric acid to form a mixed solution, add 227mL tetraethyl orthosilicate to the mixed solution, and stir for 2 h, then stirred at 70°C until gelling, aging the gel at room temperature for 12 h, drying at 110°C for 8 h, and then roasting at 400°C for 3 h, adding the obtained solid into a C6 alkane solvent and immersing it for 10 min, Then filter, dry at room temperature until there is no liquid phase on the surface of the carrier, add it to an aqueous solution containing 15.6g of phosphotungstic acid and 13.3g of lanthanum nitrate, stir at 70°C until the solution is evaporated to dryness, and dry the obtained solid at 110°C for 8.0 h, and then calcined at 430°C for 3.0 h to prepare the catalyst, La 2 o 3 The content is 10wt%, and the content of phosphotungstic acid and ammonium salt is 30%. Wherein the molar ratio of cetyltrimethylammonium bromide to sili...
Embodiment 3
[0042] Weigh 13.3g of lanthanum nitrate, 12.1g of phosphotungstic acid, 243g of cetyltrimethylammonium bromide and 48g of citric acid to form a mixed solution, add 189mL tetraethyl orthosilicate into the mixed solution, and stir for 2 h , and then stirred at 70°C until it formed a gel. The gel was aged at room temperature for 12 h, dried at 110°C for 8 h, and then calcined at 420°C for 3 h. The resulting solid was added to a C6 alkane solvent and immersed for 10 min. Then filter, dry at room temperature until there is no liquid phase on the surface of the carrier, add it to an aqueous solution containing 26.6g of phosphotungstic acid and 24.2g of lanthanum nitrate, stir at 70°C until the solution is evaporated to dryness, and dry the obtained solid at 110°C for 8.0 h, and then calcined at 400°C for 3.0 h to prepare the catalyst, La 2 o 3 The content is 15wt%, and the content of phosphotungstic acid and ammonium salt is 35%. Wherein the molar ratio of cetyltrimethylammonium b...
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