Large scale synthesis of oxidative dehydrogenation catalyst

A precalcined catalyst composition comprising molybdenum, vanadium, tellurium, niobium, oxygen, and sulfur, wherein:

• the molar ratio of molybdenum to vanadium is from 1:0.05 to 1:0.60;
• the molar ratio of molybdenum to tellurium is from 1:0.01 to 1:0.30;
• and
• the molar ratio of molybdenum to niobium is from 1:0.05 to 1:0.40;
• and
• wherein oxygen is present at least in an amount to satisfy the valency of any present metal oxides and sulfur comprises 0.001 wt. % to 0.25 wt. % of the composition;
• and
• wherein the composition is prepared by a method comprising:
• hydrothermally reacting an aqueous mixture comprising molybdenum, vanadium, tellurium, and niobium to provide a prewashed ODH catalyst precursor comprising more than 0.5 wt. % sulfur;
• and
• washing the prewashed ODH catalyst precursor with a solution comprising a water to provide the ODH catalyst precursor comprising less than 1.0 wt. % sulfur.

A method of preparing a catalyst composition comprising molybdenum, vanadium, tellurium, niobium, oxygen, and, optionally, sulfur wherein:

• the molar ratio of molybdenum to vanadium is from 1:0.05 to 1:0.60;
• the molar ratio of molybdenum to tellurium is from 1:0.01 to 1:0.30;
• and
• the molar ratio of molybdenum to niobium is from 1:0.05 to 1:0.40;
• and
• wherein oxygen is present at least in an amount to satisfy the valency of any present metal oxides and sulfur, when present, comprises less than 0.25 wt. % of the composition;
• and
• wherein the method comprises:
• hydrothermally reacting an aqueous mixture comprising molybdenum, vanadium, tellurium, and niobium to provide a prewashed catalyst composition comprising more than 0.5 wt. % sulfur;
• and
• washing the prewashed catalyst composition with a solution comprising a polar solvent to provide the catalyst composition comprising less than 0.25 wt. % sulfur.

A catalyst material comprising molybdenum, vanadium, tellurium, niobium, and oxygen, wherein:

• the molar ratio of molybdenum to vanadium is from 1:0.12 to 1:0.49;
• the molar ratio of molybdenum to tellurium is from 1:0.01 to 1:0.30;
• and
• the molar ratio of molybdenum to niobium is from 1:0.01 to 1:0.30;
• and
• wherein oxygen is present at least in an amount to satisfy the valency of any present metal oxides, and wherein the catalyst material comprises from 0.001 wt. % to 0.01 wt. % sulfur.

A method of preparing a catalyst material comprising molybdenum, vanadium, tellurium, niobium, oxygen, and, optionally, sulfur, the method comprising, the method comprising:

• hydrothermally reacting an aqueous mixture comprising molybdenum, vanadium, tellurium, and niobium to provide a prewashed composition comprising more than 0.5 wt. % sulfur;
• washing the prewashed composition with a solution comprising a polar solvent to provide a catalyst composition comprising molybdenum, vanadium, tellurium, niobium, oxygen, and, optionally, sulfur wherein:
• the molar ratio of molybdenum to vanadium is from 1:0.05 to 1:0.60;
• the molar ratio of molybdenum to tellurium is from 1:0.01 to 1:0.30;
• and
• the molar ratio of molybdenum to niobium is from 1:0.01 to 1:0.40;
• wherein oxygen is present at least in an amount to satisfy the valency of any present metal oxides and sulfur, when present, comprises less than 0.25 wt. % of the composition;
• and
• calcining the catalyst composition to provide the catalyst material, and wherein the molar ratio of molybdenum to vanadium is from 1:0.12 to 1:0.49, the molar ratio of molybdenum to tellurium is from 1:0.01 to 1:0.30, and the molar ratio of molybdenum to niobium is from 1:0.01 to 1:0.30;
• and wherein oxygen is present at least in an amount to satisfy the valency of any present metal oxides and sulfur, when present, comprises less than 0.01 wt. % of the catalyst material.