US3887489A — Rhodium catalyst regeneration method

Claim 1

Independent Claim 145 words

A process for the regeneration of a spent catalyst solution containing a soluble rhodium iodocarbonyl complex, hydrogen iodide, water, acetic acid and metallic corrosion products which comprises heating said spent catalyst solution with agitation at a temperature from about 100* to 190*C at a pressure sufficient to boil the solution for a period of time necessary to obtain a rhodium-containing precipitate from said solution and reduce the rhodium content of said solution to a predetermined level, separating the solid rhodium-containing precipitate from said liquid solution, adding a quantity of a solvent selected from the group consisting of water, acetic acid and mixtures thereof and an iodine-containing component selected from the group consisting of iodine, hydrogen iodide, alkyl iodides, aryl iodides and iodine salts to said rhodium-containing precipitate and heating the resulting mixture in contact with carbon monoxide while maintaining constant agitation until solution is effected.

Claim 2

Dependent Claim 145 words

A process for the regeneration of a spent catalyst solution containing a soluble rhodium iodocarbonyl complex, hydrogen iodide, water, acetic acid and metallic corrosion products which comprises heating said spent catalyst solution with agitation at a temperature from about 100* to 190*C at a pressure sufficient to boil the solution for a period of time necessary to obtain a rhodium-containing precipitate from said solution and reduce the rhodium content of said solution to a predetermined level, separating the solid rhodium-containing precipitate from said liquid solution, adding a quantity of a solvent selected from the group consisting of water, acetic acid and mixtures thereof and an iodine-containing component selected from the group consisting of iodine, hydrogen iodide, alkyl iodides, aryl iodides and iodine salts to said rhodium-containing precipitate and heating the resulting mixture in contact with carbon monoxide while maintaining constant agitation until solution is effected.

Claim 3

Dependent Claim 141 words

A PROCESS FOR THE REGENERATION OF A SPENT CATALYST SOLUTION CONTAINING A SOLUBLE RHODIUM IODOCARBONYL COMPLEX, HYDROGEN IODIDE, WATER, ACETRIC ACID AND METALLIC CORROSION PRODUCTS WHICH COMPRISES HEATING SAID SPENT CATALYST SOLUTION WITH AGITATION AT A TEMPERATURE FROM ABOUT 100* TO 190*C AT A PRESSURE SUFFICIENT TO BOIL THE SOLUTION FOR A PERIOD OF TIME NECESSARY TOOBTAIN A RHODIUM-CONTAINING PRECIPITATE FROM SAID SOLUTION AND REDUCE THE RHODIUM CONTENT OF SAID SOLUTION TO A PREDERTERMINED LEVEL, SEPARATING THESOLID RHODIUMCONTAINING PRECIPITATE FROM SAD LIQUID SOLUTION, ADDING A QUANTITY OFA SOLVENT SELECTED FROM THE GROUP CONSISTING OF WATER, ACETIC ACID AND MIXTURESTHEREOF AND AN IODINECONTAINING COMPONENT SELECTED FROM THE GROUP CONSISTING OF IODINE, HYDROGEN IODIDE, ALKYL IODIDES, ARYL IODIDES AND IODINE SALTS TO SAID RHODIUM-CONTAINING PRECIPITATE AND HEATNG THE RESULTING MIXTURE IN CONTACT WITH CARBON MONOXIDE WHILE MAINTAINING CONSTANT AGITATION UNTIL SOLUTION IS EFFECTED.

Claim 4

Dependent Claim 141 words

A PROCESS FOR THE REGENERATION OF A SPENT CATALYST SOLUTION CONTAINING A SOLUBLE RHODIUM IODOCARBONYL COMPLEX, HYDROGEN IODIDE, WATER, ACETRIC ACID AND METALLIC CORROSION PRODUCTS WHICH COMPRISES HEATING SAID SPENT CATALYST SOLUTION WITH AGITATION AT A TEMPERATURE FROM ABOUT 100* TO 190*C AT A PRESSURE SUFFICIENT TO BOIL THE SOLUTION FOR A PERIOD OF TIME NECESSARY TOOBTAIN A RHODIUM-CONTAINING PRECIPITATE FROM SAID SOLUTION AND REDUCE THE RHODIUM CONTENT OF SAID SOLUTION TO A PREDERTERMINED LEVEL, SEPARATING THESOLID RHODIUMCONTAINING PRECIPITATE FROM SAD LIQUID SOLUTION, ADDING A QUANTITY OFA SOLVENT SELECTED FROM THE GROUP CONSISTING OF WATER, ACETIC ACID AND MIXTURESTHEREOF AND AN IODINECONTAINING COMPONENT SELECTED FROM THE GROUP CONSISTING OF IODINE, HYDROGEN IODIDE, ALKYL IODIDES, ARYL IODIDES AND IODINE SALTS TO SAID RHODIUM-CONTAINING PRECIPITATE AND HEATNG THE RESULTING MIXTURE IN CONTACT WITH CARBON MONOXIDE WHILE MAINTAINING CONSTANT AGITATION UNTIL SOLUTION IS EFFECTED.

Claim 5

Dependent Claim 40 words

The process of claim 1 wherein said liquid solution separated from said solid rhodium-containing precipitate is passed through a separator for removal of any finely divided solids contained therein and said finely divided solids are combined with said rhodium-containing precipitate.

Claim 6

Dependent Claim 67 words

The process of claim 1 wherein heating of said spent catalyst solution is effected at a temperature of at least 140* C and in the presence of an alkyl alcohol in which the alkyl group contains 1 to 5 carbon atoms, the amount of said alcohol being sufficient to provide a mole ratio of alcohol to hydrogen iodide in the spent catalyst solution of at least 1:1.

Claim 7

Dependent Claim 66 words

THE PROCESS OF CLAIM 1 WHEREIN HEATING OF SAID SPENT CATALYST SOLUTION IS EFFECTED AT A TEMPERATURE OF AT LEAST 140* C AND IN THE PRESENCE OF AN ALKYL ALCOHOL IN WHICH THE ALKYL GROUP CONTAINS 1 TO 5 CARBON ATOMS, THE AMOUNT OF SAID ALCOHOL BEING SUFFICIENT TO PROVIDE AMOLE RATIO OF ALCOHOL TO HYDROGEN IODIDE IN THE SPENT CATALYST SOLUTION OF AT LEAST 1:1.

Claim 8

Dependent Claim 10 words

The process of claim 3 wherein said alcohol is methanol.

Claim 9

Dependent Claim 23 words

The process of claim 4 wherein the mole ratio of methanol to hydrogen iodide is in the range from about 4:1 to 20:1.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1978-06-02	1978-12-02	1979-06-03	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1982-06-02	1982-12-02	1983-06-03	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1986-06-02	1986-12-02	1987-06-03	$7700.00	Window Closed / Lapsed

Rhodium catalyst regeneration method

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