Method for preparing octylene-1 by ethylene tetramerization reaction
A technology for tetramerization and reaction of ethylene, applied in chemical instruments and methods, hydrocarbons, organic compounds/hydrides/coordination complex catalysts, etc. low sex issues
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Embodiment 1
[0039] 1. Preparation of (diphenyl) phosphorus nitrogen (isopropyl) phosphorus (diphenyl) ligand (C 27 h 27 NP 2 )
[0040] (1) Preparation of N, N-diisopropyl dichlorophosphoramide
[0041] in the N 2 Add dehydrated toluene (100mL) into a fully replaced stirred 250mL reactor, add PCl 3 (21.87mL, 0.25mol), and cooled to -20°C. Diisopropylamine (70 mL, 0.5 mol) was slowly added while stirring at room temperature, stirred for 3 hours, raised to room temperature and continued to react for 2 hours, then filtered and dried to obtain 38.1 g (0.19 mol, 74%) of the product.
[0042] (2) Preparation of phenylmagnesium bromide lattice reagent
[0043] in the N 2 Add dehydrated THF (100 mL) and magnesium powder (9.11 g, 0.375 mol) into a fully replaced stirred 250 mL reactor, cool down in an ice bath and slowly add bromobenzene (11.775 g, 0.075 mol) dropwise. After 2 hours, heat to reflux and continue the reaction for 2 hours to obtain the lattice reagent.
[0044] (3) Preparati...
Embodiment 2
[0055] 1. Preparation of (diphenyl) phosphorus nitrogen (isopropyl) phosphorus (diphenyl) ligand (C 27 h 27 NP 2 ) with embodiment 1.
[0056] 2. Preparation of modified active agent
[0057] At -78°C, under vigorous stirring, slowly add 0.81 mL of twice distilled water (45 mmol) dropwise into 6.84 mL (50 mmol) of AlEt 3 In toluene (50mL) solution, after the dropwise addition, the system was naturally returned to room temperature, and the reaction was continued for 12h to obtain a toluene solution of EAO. [Ph 3 C][Al(OC(CF 3 ) 3 ) 4 ] (10mmol) of toluene solution 50mL, kept at room temperature for 6 hours after the dropwise addition, to obtain a modified activator.
[0058] 3. Preparation of catalyst
[0059] With embodiment 1. The modified activator added is the modified activator prepared in this example.
[0060] 4. Ethylene oligomerization
[0061] With embodiment 1. Obtain 6.38g of oligomerization product, catalyst activity is 3.87×10 5 g oligomer / mol Cr.h. ...
Embodiment 3
[0063] 1. Preparation of (diphenyl) phosphorus nitrogen (isopropyl) phosphorus (diphenyl) ligand (C 27 h 27 NP 2 ) with embodiment 1.
[0064] 2. Preparation of modified active agent
[0065] With embodiment 1. The difference is that the added modifier containing at least two heteroatoms is sodium tetrafluoroborate compound.
[0066] 3. Preparation of catalyst
[0067] With embodiment 1.
[0068] 4. Ethylene oligomerization
[0069] With embodiment 1. Obtain 8.5g of oligomerization product, catalyst activity is 5.15×10 5 g oligomer / molCr.h. The distribution of the oligomerization products is shown in Table 1.
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