METHOD OF PREPARING A HYDROGENATION CATALYST
A method of forming a hydrogenation catalyst includes providing a first fluid including a first reagent in a first reagent dispensing device, the first reagent including an organoaluminum compound and providing a second fluid including a second reagent in a second reagent dispensing device, the second reagent including a nickel alkoxylate. The method further includes contemporaneously delivering the first fluid from the first reagent dispensing device and the second fluid from second reagent dispensing device to a reaction vessel at a constant stoichiometry of aluminum in the organoaluminum compound to nickel in the nickel alkoxylate, the organoaluminum compound reacting with the nickel alkoxylate in the reaction vessel to form the hydrogenation catalyst.
1 . A method of forming a hydrogenation catalyst comprising:
providing a first fluid including a first reagent in a first reagent dispensing device, the first reagent including an organoaluminum compound;
providing a second fluid including a second reagent in a second reagent dispensing device, the second reagent including a nickel alkoxylate;
contemporaneously delivering the first fluid from the first reagent dispensing device and delivering the second fluid from the second reagent dispensing device to a reaction vessel at a constant stoichiometry of aluminum in the organoaluminum compound to nickel in the nickel alkoxylate, the organoaluminum compound reacting with the nickel alkoxylate in the reaction vessel to form the hydrogenation catalyst.
2 . The method of claim 1 , wherein at least one of the first fluid and the second fluid further includes a solvent.
3 . The method of claim 2 , wherein the solvent is selected from the group consisting of aliphatic hydrocarbons, aromatic hydrocarbons, cycloaliphatic hydrocarbons and mixtures thereof.
4 . The method of claim 2 , wherein the solvent is selected from the group consisting of hexane, pentane, toluene, benzene, cyclohexane and mixtures thereof.
5 . The method of claim 1 , wherein the organoaluminum compound is represented by Formula I:
where R 1 is selected from alkyl, alkoxy, aryl, alkaryl, arylalkyl and hydrogen;
R 2 is selected from alkyl (including cycloalkyl), aryl, alkaryl, arylalkyl and hydrogen; and
R 3 is selected from alkyl (including cycloalkyl), aryl, alkaryl and arylalkyl.
6 . The method of claim 5 , wherein the organoaluminum compound includes a trialkylaluminum compound.
7 . The method of claim 6 , wherein in the trialkylaluminum compound, R 1 , R 2 and R 3 are each independently a C1 to C18 straight chain or branched alkyl group.
8 . The method of claim 6 , wherein the trialkylaluminum compound is selected from the group consisting of trimethylaluminum, triethylaluminum, tri-n-propylaluminum, triisopropylaluminum, tri-n-butylaluminum, triisobutylaluminum, tripentylaluminum, trihexylaluminum, tricyclohexylaluminum, trioctylaluminum, and dimers and mixtures thereof.
9 . The method of claim 1 , wherein the nickel alkoxylate is derived from a C6 to C18 carboxylic acids.
10 . The method of claim 1 , wherein the nickel alkoxylate is selected from the group consisting of nickel (II) octoate and nickel octanoate.
11 . The method of claim 1 , wherein the constant stoichiometry of aluminum in the organoaluminum compound to nickel in the nickel alkoxylate is fixed within a range of from 2:1 to 3.5:1.
12 . The method of claim 1 , wherein in the contemporaneously delivering the first fluid from the first reagent dispensing device and the second fluid from the second reagent dispensing device to the reaction vessel comprises maintaining the constant stoichiometry of aluminum in the organoaluminum compound to nickel in the nickel alkoxylate for at least two, or at least ten minutes.
13 . The method of claim 1 , wherein the first reagent dispensing device and the second reagent dispensing device comprise syringes that are actuated by respective motors or by a common motor.
14 . The method of claim 1 , wherein the delivery comprises pumping the first and second fluids to a mixing point upstream of the reaction vessel and delivering a mixture of the first and second fluids from the mixing point to the reaction vessel.
15 . The method of claim 1 , wherein the method further includes cooling the reaction vessel during the contemporaneously delivering step.
16 . A hydrogenation catalyst formed by the method of claim 1 .
17 . A rubber composition comprising a hydrogenated elastomer hydrogenated with the hydrogenation catalyst of claim 16 and at least one additive selected from the group consisting of fillers, plasticizers, zinc oxide, and a sulfur-based curing agent.
18 . In combination, an apparatus and reagents for forming a hydrogenation catalyst, comprising:
a first reagent dispensing device which contains a first reagent, the first reagent including an organoaluminum compound;
a second reagent dispensing device which contains a second reagent, the second reagent including a nickel alkoxylate;
a first delivery tube which connects the first reagent dispensing device with a mixing point;
a second delivery tube which connects the second reagent dispensing device with the mixing point;
a reaction vessel;
a common delivery tube which connects the mixing point to the reaction vessel; and
a pressurizing mechanism which pressurizes the first and second reagents so that they are delivered to the reaction vessel at a constant stoichiometry of aluminum in the organoaluminum compound to nickel in the nickel alkoxylate.
19 . The apparatus of claim 18 , wherein the first and second reagent dispensing devices comprise first and second syringes.
20 . The apparatus of claim 19 , wherein the pressurizing mechanism comprises a motor which drives a plunger of at least one of the first and second syringes.