Invista North America S.a.r.l.

Inv Nylon Chemicals Americas, LLC

Invista Textiles Limited

Vinay Medhekar

Keith Whiston

Joan Fraga-Dubreuil

Thomas A Micka

John Joseph Ostermaier

Colin S Slaten

John Arthur Turner

Michael C Quinn, Iii

The present invention relates to heterogeneous catalysts and methods of making and using the same. In various embodiments, the present invention provides a method of making a hydrogenation catalyst including particulate nickel metal (Ni(0)). The method includes calcining first nickel(II)-containing particles in an atmosphere including oxidizing constituents to generate second nickel(II)-containing particles. The method also includes reducing the second nickel(II)-containing particles in a reducing atmosphere while rotating or turning the second nickel(II)-containing particles at about 275&#xb0; C. to about 360&#xb0; C. for a time sufficient to generate the particulate nickel metal (Ni(0)), wherein the particulate nickel metal (Ni(0)) is free flowing.

Heterogeneous catalyst process and nickel catalyst

Methods are described herein that involve rotating or gently mixing nickel(II)-containing particles in a reaction vessel while heating the particles and flowing a reducing atmosphere through the reaction vessel for a time sufficient to generate free-flowing nickel metal (Ni(0)) from the nickel(II)-containing particles.

Nickel metal particle production

Disclosed are nickel-containing complexation precursors having high complexation activity for bidentate phosphite ligands. Also disclosed are methods of making the complexation precursors. The disclosed method of generating the nickel-containing complexation precursor includes including contacting a nickel starting material with a reductant under conditions sufficient to generate a nickel-containing complexation precursor having at least about 1,500 ppmw sulfur in the form of sulfide.

Nickel having high ligand-complexation activity and methods for making the same

As described herein, nickel treated with sulfur provides a surprisingly effective source of nickel atoms for generating nickel-phosphorus-containing ligand complexes useful as hydrocyanation catalysts.

Metal-ligand catalyst formation

A novel nickel particulate form is provided that efficiently forms a zero-valent nickel complex with a phosphorus-containing ligands in an organic liquid to form a hydrocyanation catalyst. Particles in the nickel particulate form comprise nickel crystallites. For example, the nickel particulate form can have a BET Specific Surface Area of at least about 1 m/gm; an average crystallite size less than about 20-25 nm, the nickel particulate form can have at least 10% of the crystallites in the nickel form can have can have a diameter (C10) of less than about 10 nm, and/or there are on average at least about 10surface crystallites per gram nickel. A ratio of BET SSA to C50 for the nickel particulate form can be at least about 0.1&#xd7;10m/gm and preferably at least about 0.4&#xd7;10m/gm. Methods of preparation and use are also provided.

Nickel form for preparation of catalytic nickel-ligand complexes

A novel nickel particulate form is provided that efficiently forms a zero-valent nickel complex with a phosphorus-containing ligands in an organic liquid to form a hydrocyanation catalyst. Particles in the nickel particulate form comprise nickel crystallites. For example, the nickel particulate form can have a BET Specific Surface Area of at least about 1 m/gm; an average crystallite size less than about 20-25 nm, the nickel particulate form can have at least 10% of the crystallites in the nickel form can have a diameter (C10) of less than about 10 nm, and/or there are on average at least about 10surface crystallites per gram nickel. A ratio of BET SSA to C50 for the nickel particulate form can be at least about 0.1&#xd7;10m/gm and preferably at least about 0.4&#xd7;10m/gm. Methods of preparation and use are also provided.

These disclosures relate to preparing nickel metal (Ni(0)) suited for use in catalyst systems, such as nickel complexes with phosphorus-containing ligands, useful to catalyze the hydrocyanation of ethylenically unsaturated compounds. The methods described herein can include use of steam during reduction of nickel.

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Beaumont, TX, United States of America

Vinay Medhekar