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Molecular Sieve Patent

 

Thermactivation of catalysts comprising catalytic metals-free crystalline zeolitic molecular sieve particles dispersed in a gel matrix

Molecular sieve abstract

Method of activating a catalyst composite comprising particles of a catalytic metals-free crystalline zeolitic molecular sieve dispersed in a gel matrix comprising silica-alumina, a Group VI hydrogenating component and a Group VIII hydrogenating component, which method comprises heating said catalyst composite in an oxygen-containing gas stream at 1200.degree. to 1600.degree.F. for 0.25 to 48 hours, and the catalyst composite so activated.

Molecular sieve claims

What is claimed is:

1. A catalyst composite comprising:

A. a gel matrix comprising:

a. at least 15 weight percent silica,

b. alumina, in an amount providing an alumina-to-silica weight ratio of 15/85 to 80/20

c. nickel or cobalt, or the combination thereof, in the form of metal, oxide, sulfide, or any combination thereof, in an amount of 1 to 10 weight percent of said matrix, calculated as metal,

d. molybdenum or tungsten, or the combination thereof, in the form of metal, oxide, sulfide, or any combination thereof, in an amount of 5 to 25 weight percent of said matrix, calculated as metal;

B. a crystalline zeolitic molecular sieve substantially in the ammonia or hydrogen form, substantially free of any catalytic loading metal or metals, said sieve further being in particulate form and being dispersed through said matrix;

said catalyst composite being further characterized by an average pore diameter below 100 Angstroms and a surface area above 200 square meters per gram;

said catalyst composite being further characterized by hydrocracking activities and stabilities developed therein by heating said catalyst composite in an oxygen-containing gas stream at temperatures in the range 1200.degree.F. to 1600.degree.F. for 0.25 to 48 hours.

2. A catalyst composite as in claim 1 wherein said gel matrix further comprises titania.

3. A catalyst comprising a silica-alumina matrix having dispersed in it particles of a low-sodium molecular sieve zeolite, the silica-alumina matrix having dispersed in it a Group VI metal or metal compound and a Group VIII metal or metal compound and the zeolite being substantially free of chemically or physically bonded metals or metal compounds having appreciable catalytic activity for hydrogenation; said catalyst being further characterized by hydrocracking activities and stabilities developed therein by heating said catalyst in an oxygen-containing gas stream at temperatures in the range 1200.degree. to 1600.degree.F. for 0.25 to 48 hours.

4. A catalyst comprising a crystalline zeolitic molecular sieve of the ammonia or hydrogen form and substantially free of metals or metal compounds having catalytic activity for hydrogenation dispersed in a hydrocracking catalyst matrix comprised of silica-alumina having dispersed in it 1 to 10% by weight of nickel in the formm of metal, metal oxide or metal sulfide and 5 to 25% by weight of molybdenum or tungsten in the form of metal, metal oxide or metal sulfide, said catalyst being further characterized by hydrocracking activities and stabilities developed therein by heating said catalyst in an oxygen-containing gas stream at temperatures in the range 1200.degree. to 1600.degree.F. for 0.25 to 48 hours.

Molecular sieve description

INTRODUCTION

In Joseph Jaffe copending application Ser. No. 749836 filed Aug. 2 1968 for "Hydrotreating Catalyst and Process," there is described a novel and unusually effective hydrofining-hydrocracking catalyst. Said catalyst comprises a crystalline zeolitic molecular sieve component substantially free of any catalytic metal or metals, a silica-containing gel component, a Group VI hydrogenating component, and a component selected from titanium, zirconium, thorium, hafnium, and compounds thereof. It has now been found that catalysts of this general type, either with or without a Group IV component, can be even further improved in various respects by a novel heat treatment procedure, which serves both to activate and stabilize the catalyst. Said heat treatment procedure, hereinafter for convenience called an activation or thermactivation treatment or procedure, is applied to the total catalyst composite, following dispersion of the crystalline zeolitic molecular sieve component in the gel matrix.

STATEMENT OF INVENTION

In accordance with the present invention catalysts of the aforesaid type are thermactivated in an oxygen-containing gas stream at temperatures in the range 1200.degree. to 1600.degree.F., preferably 1250.degree. to 1400.degree.F., for 0.25 to 48 hours. The oxygen-containing gas stream, which may be air, preferably is as dry as practicable. The improved results obtainable with the process of the present invention are optimized as the gas stream becomes extremely dry; although for most practical purposes the gas stream need be only as dry as ambient air, greater dryness is preferred. Those skilled in the art will be aware of various methods for drying the gas stream to any desired extent.

Although the process of the present invention is applicable to activation of catalysts of the aforesaid type with a wide range of silica content, it is especially useful with such catalysts that contain less than 40 weight percent silica in the total catalyst, and less than 35 weight percent silica in the catalyst matrix.

Further in accordance with the present invention there is provided the method of activating a catalyst composite comprising:

A. A gel matrix comprising:

A. at least 15 weight percent silica,

B. alumina, in an amount providing an aluminum-to-silica weight ratio of 15/85 to 80/20

C. nickel or cobalt, or the combination thereof, in the form of metal, oxide, sulfide or any combination thereof, in an amount of 1 to 10 weight percent of said matrix, calculated as metal,

D. molybdenum or tungsten, or the combination thereof, in the form of metal, oxide, sulfide or any combination thereof, in an amount of 5 to 25 weight percent of said matrix, calculated as metal;

B. A crystalline zeolitic molecular sieve substantially in the ammonia or hydrogen form, substantially free of any catalytic loading metal or metals, said sieve further being in particulate form and being dispersed through said matrix;

said catalyst composite being further characterized by an average pore diameter below 100 Angstroms and a surface area above 200 square meters per gram;

which method comprises heating said catalyst composite in an oxygen-containing gas stream at temperatures in the range 1200.degree. to 1600.degree.F. for 0.25 to 48 hours.

Further in accordance with the present invention there is provided a catalyst composite comprising:

A. A gel matrix comprising:

a. at least 15 weight percent silica,

b. alumina, in an amount providing an alumina-to-silica weight ratio of 15/85 to 80/20

c. nickel or cobalt, or the combination thereof, in the form of metal, oxide, sulfide or any combination thereof, in an amount of 1 to 10 weight percent of said matrix, calculated as metal,

d. molybdenum or tungsten, or the combination thereof, in the form of metal, oxide, sulfide or any combination thereof, in an amount of 5 to 25 weight percent of said matrix, calculated as metal;

B. A crystalline zeolitic molecular sieve substantially in the ammonia or hydrogen form, substantially free of any catalytic loading metal or metals, said sieve further being in particulate form and being dispersed through said matrix;

said catalyst composite being further characterized by an average pore diameter below 100 Angstroms and a surface area above 200 square meters per gram; said catalyst composite being further characterized by hydrocracking activities and stabilities developed therein by heating said catalyst composite in an oxygen-containing gas stream at temperatures in the range 1200.degree.to 1600.degree.F. for 0.25 to 48 hours.

The gel matrix of the aforesaid catalyst composite additionally may comprise titanium, zirconium, thorium, hafnium, or any combination thereof, in the form of the metal, oxide, sulfide or any combination thereof, in an amount of 1 to 10 weight percent of said matrix, calculated as metal.

The reference to a crystalline zeolitic molecular sieve "substantially free of any catalytic loading metal or metals" means that the molecular sieve contains no more than 0.5 weight percent of catalytic metal or metals, based on the sieve. The catalytic metal or metals include the Group VI and VIII metals, excluding sodium.


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