反应 #70057

ord-70b03b60d66c4e9c88f474373cab2e3a

反应条件

温度
90°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他equipped with an agitator, at room temperature
  2. 2
    workup.ADDITIONwas added
  3. 3
    温度the reaction temperature was maintained at 90° C. overnight
  4. 4
    温度cooled down to room temperature
  5. 5
    其他any reactor pressure was vented
  6. 6
    workup.STIRRINGstirred with 5 g
  7. 7
    其他for half an hour
  8. 8
    过滤filtered
  9. 9
    其他to remove solids

实验过程

A solution of 100 g of purified 1-decene, 1.301 g of a TIBA stock solution (20 mg TIBA/g toluene solution) and 0.445 g of Metallocene A stock solution (1 mg Metallocene A/g toluene solution) was charged into a clean 600 ml autoclave equipped with an agitator, at room temperature. The reactor was then pressurized with 30 psig hydrogen. The mixture was then heated to 90° C. with stirring. A second solution made by adding a) 0.641 g of Activator A stock solution (1 mg Activator A/g toluene solution) and b) 20 g toluene solvent and was added and the reaction temperature was maintained at 90° C. overnight, then cooled down to room temperature, and any reactor pressure was vented. The liquid product was diluted with 50 ml heptane, stirred with 5 g activated alumina for half an hour and filtered to remove solids. The filtrate was analyzed by gas chromatography using an internal standard to obtain the wt % of normal-decane (n-C10) formation from 1-decene hydrogenation, wt % conversion to lubes and wt % lube yield. The lube product was then isolated by flashing the light ends (solvents, unreacted C10 fraction, and any fractions lighter than C30) and distilled at 180° C. under high vacuum (1 millitorr) for two hours to isolate the lube product.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08530712B2uspto-grants-2013_09