PDF | Data on the activity, selectivity, and reaction conditions for the selective oligomerization of ethylene to octene-1 mediated by chromium-containing organic. MAO is requisite in forming active species for ethylene tetramerization toward 1- octene. TCE shows significant promotion effect to assist. higher catalytic activity and longer lifetime for ethylene tetramerization in the presence ethylene tetramerization, 1-octene, trinuclear, diphenylphosphinoamine.
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Otherwise, the reaction process and product treatment processes were conducted as in Example 1. Meanwhile, 95 g of recrystallized triphenylphosphorus and mi of dried tetrahydrofuran THF were put into a 1 L three-neck flask equipped with a funnel for dropping, a condenser for reflux cooling, and a nitrogen injector to form a solution.
In order to analyze the liquid using GC-FBD, nonane, serving as an internal standard substance, was added thereto. The mixed solution was slowly heated to room temperature and then stirred for 30 minutes. A phenyl 2 PCH 2 P phenyl 2 ligand was prepared by reacting diphenylphosphine with 2 equivalents of dibromoalkyl in dimethylfluoromethylene DMF and cesium hydroxide atmospheres, as disclosed in the document “R. Tetramerization of ethylene using CrChftefrahvdrofuranK R.
Comparative Catalyst Preparation Example 4: The catalyst system for tetramerizing ethylene according to claim 1, wherein, in the P- C-C-P backbone structure ligand represented by Formula 1 above, R 5 and R 6 are each independently selected from the group consisting of alkyl, substituted alkyl, aryl, substituted aryl, aryloxy, substituted aryloxy, alkoxycarbonyl, carbonyloxy, alkoxy, aminocarbonyl, carbonylamino, dialkylamino, silyl, derivatives thereof, and aryl substituted with these arbitrary substituents.
Ethylene tetramerization: a new route to produce 1-octene in exceptionally high selectivities.
Separation of components from a multi-component hydrocarbon stream which includes ethylene. Further, German Patent No.
The slurry solution was cooled to form it into a solid, and then the solid was washed with 25 mi of water twice and then rapidly cooled using ethanol, cooled using ice, to form a beige solid containing impurities. Thereafter, simultaneously, LiP 4-OMe-Ph 2 1-oxtene formed in the solution, heat was generated in the solution, and the solution became dark reddish yellow.
1-otcene reaction mixture was further stirred for 24 hours, and was then filtered to remove triethylammonium salts therefrom.
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It was found that the weight of the product, determined through GC, was 9. A mixed heteroatomic PNP ligand was prepared by reacting amine with phosphine chloride R 2 PClas disclosed in the theses: The mixture reacted strongly, and was then refluxed and heated for 2 hours to obtain a Grignard reagent. Highly active and highly selective ethylene tetrameization catalyst, and preparation method of hexene or octene using same.
The oily product was extracted twice using mi of ether, and was then dried by Na 2 SO 4 to form an ether extract. Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art, and an object of the present invention is to provide a method of preparing 1-octene at high activity and high selectivity while stably maintaining reaction activity by tetramerizing ethylene using a chromium-based catalyst system comprising a transition metal or a transition metal precursor, a cocatalyst, and a P-C-C-P backbone structure ligand represented by the following Formula 1: Examples of the reactors may include, but are not limited to, tetrameriztion batch reactor, a semibatch reactor, and a continuous reactor.
Chromium-Based Catalyst for Ethylene Tetramerization to 1-Octene
Further, in the P-C-C-P backbone structure ligand represented by Formula 1 above, R and R 6 are not hydrogen but each independently a hydrocarbyl group and substituted hydrocarbyl group.
Species Ethylene tetramerization catalyst compositions and tetramerization process of ethylene. JP Kind code of ref document: C-C-P backbone structure ligand represented by Formula 1 above, R 1R 2R 3 and R 4 are each independently selected from the group consisting of phenyl, benzyl, naphthyl, anthracenyl, mesityl, xylyl, methyl, ethyl, ethylenyl, propyl, propenyl, propynyl, butyl, cyclohexyl, A- methylcyclohexyl, 4-ethylcyclohexyl, 4-isopropylcyclohexyl, tolyl, 4-methylphenyl, 4- ethylphenyl, 4-isopropylphenyl, 4-t-butylphenyl, 4-methoxyphenyl, 4-isopropoxyphenyl, cumyl, methoxy, ethoxy, phenoxy, tolyloxy, dimethylamino, thiomethyl, trimethylsilyl, and dimethylhydrazyl.
Comparative Catalyst Preparation Example 5: Kind code of ref document: An ethylene tetramerization catalyst composition and method of Ethylene tetramerization. The reaction mixture was stirred for 30 minutes, and then impurities were removed therefrom. Comparative Catalyst Preparation Example 3: US USB2 en Bosnich et al, J.
Comparative Examples 14 to Thus, the nickel complex was slowly dissolved, and was thus formed into a red solution, [Ni S,S -chiraphos 2 CN 3 ] “and then the red solution changed into a turbid beige solution.
Subsequently, ethylene was charged in the reactor at a pressure of 30 bar, and was then stirred at a stirring speed of rpm. Examples 9 to 12 and Comparative Examples 14 to 17 were conducted to compare the 1-octene production yields of the P-C-C-P backbone structure ligand of the present invention with those of the conventional hetero atom structure PNP ligand depending on reaction times.
After 30 minutes, the supply of ethylene and the stirring thereof were stopped, and the reactor was cooled to a temperature of less than lOt.
The catalyst system according to the present invention may be manufactured through a process of forming a ligand coordination complex using transition metal compounds and the P- C-C-P backbone structure ligand. The solution was reacted for 60 hours at room temperature, and 60 ml of distilled water was added ethylnee, and the solution was extracted three times 1octene 60 ml of DMC to form an organic layer. Ethylne was found that the weight of the product, determined through GC, was Tetramerization of ethylene using Cr IID acetylacetonate j.
Highly active and selective ethylene oligomerization catalyst and method of preparing hexene or octene using the same. EP Kind code of ref document: Further, it was found that the total weight of the reaction mixture, determined through GC, was