A kind of method of stabilizing phosphite ligand and application thereof
A technology of phosphite and organic phosphite, which is applied in the field of improving the life of the ligand in the catalytic reaction and in the field of improving the life of the phosphite ligand in the catalytic reaction. cheap effect
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Embodiment 1
[0039] Refer to the method for evaluating ligand stability in US 5364950 to simulate the solution of hydroformylation reaction. The solution contained 72 ppm rhodium, 0.6 wt% Ligand A (6,6'-[3,3',5,5'-tetrakis(1,1-dimethylethyl)1,1'-diphenyl -2,2'-diyl]dioxo]bis-dibenzo[d,f][1,3,2]-diphosphine oxygen ligand), about 84 wt% butyraldehyde, about 8.2 wt% tetraethylene glycol Dimethyl ether as solvent and about 7.1 wt% biphenol. Five aliquots of this solution were fill dispensed into nitrogen purged containers. Leave sample A unchanged as a control. To samples B to E were added 0.2 wt% hydroxypentylphosphonic acid and 0.6 wt% water (both based on the total weight of the contents of the container). Nothing was added to sample B, 5 wt% t-butylamine was added to sample C, 5 wt% styrene oxide was added to sample D and 1 wt% beta cyclodextrin was added to sample E. Under the same experimental conditions, the sample solution was regularly taken out to measure the amount of ligand rem...
Embodiment 2
[0045] Referring to the method for evaluating ligand stability by using two-tank series carbonylation reaction in Example 12 of US 5364950, β-cyclodextrin (accounting for 0.7 wt% of the total mixture mass) was used instead of 1,2-epoxydodecane. The reaction continued for 124 days. Compared with the addition of 0.2wt% 1,2-epoxydodecane every three days described in US5364950, no ligand and cyclodextrin were added during the reaction, and other conditions Consistent with US 5364950. figure 2 It shows the change of conversion rate of carbonylation reaction and product isotropic ratio with time, and samples are taken every three days for a total of 124 days. Such as figure 2 As shown in , during the 124-day reaction process, the activity of the catalyst did not change, and the positive-isotropic ratio of the product was basically stable at around 95 (the high positive-isotropic ratio may be due to the shape-selective effect of the cyclodextrin cavity). This constant activity ind...
Embodiment 3
[0047] Except that the equivalent volume of the reaction solvent tetraethylene glycol dimethyl ether was replaced with dimethylimide, and the operating time was changed to 30 days, other process conditions were kept the same as in Example 2.
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