A kind of method for preparing ethylene-propylene rubber
A technology of ethylene-propylene rubber and propylene, applied in the field of preparation of ethylene-propylene rubber, can solve problems such as inability to control the performance of ethylene-propylene rubber, and achieve the effect of strong copolymerization catalytic ability
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Embodiment 1
[0045] Synthesis of bridged metallocene complex A1:
[0046] (1) Synthesis of 1-(2,5-dimethylphenyl)-2-methylpropan-1-one: 78.6 grams (0.74mol) of p-xylene, 61 grams (0.45mol) of anhydrous AlCl 3 The mixture of the powder and 500 mL of carbon disulfide was cooled to 0° C., and 79.4 g (0.74 mol) of methacryloyl chloride was slowly added dropwise to the mixture while stirring. After the temperature of the mixture rose to room temperature, stirring was continued for 12 hours. Then add 61 grams (0.45mol) of anhydrous AlCl 3 powder and 250mL carbon disulfide. The mixture was refluxed at 45°C for 3 hours. The reaction mixture was cooled to room temperature and poured into an ice / hydrochloric acid mixture. The organic phase is separated and the carbon disulfide is removed by gas flow. The remaining liquid was extracted with ether and washed with anhydrous Na 2 SO 4 After drying, 93.0 g of 1-(2,5-dimethylphenyl)-2-methylpropan-1-one was obtained, with a yield of 71%. 1 H-NMR (...
Embodiment 2
[0054] Synthesis of bridged metallocene complex A2:
[0055] (1) Synthesis of 1-(2,5-diethylphenyl)-2-methylpropan-1-one: the reaction conditions are the same as those of 1-(2,5-dimethylphenyl)-2 in Example 1 -Synthesis of methylpropan-1-one, only p-xylene was replaced by p-diethylbenzene, 91.3 grams of 1-(2,5-dimethylphenyl)-2-methylpropan-1-one were obtained, Yield 59%. 1 H-NMR (300MHz, CDCl 3 ,δinppm):7.70(s,1H,Ar-H),7.25(s,1H,Ar-H),7.15(s,1H,Ar-H),3.34(sept,1H,CH(CH 3 ) 2 ),2.59(s,4H,Ar-CH 2 ),1.23(d,6H,CHCH 3 ). Elem.Anal.Calcd.ForC 14 h 20 O: C, 82.35%; H, 9.80%; O, 7.84%. Found: C, 82.30%; H, 9.84%; O, 7.86%. ESI-MS: m / z205.10 ([M+H] + ).
[0056] (2) Synthesis of α-bromo-2,5-diethylisobutyrophenone: the reaction conditions are the same as those in Example 1 for the synthesis of α-bromo-2,5-dimethylisobutyrophenone, only 1-( 2,5-Dimethylphenyl)-2-methylpropan-1-one was replaced by 1-(2,5-diethylphenyl)-2-methylpropan-1-one to give 69.9 g of α -Bromo-2,5-di...
Embodiment 3
[0063] Synthesis of bridged metallocene complex A3:
[0064] (1) Synthesis of 1-(2-methoxy-5-methylphenyl)-2-methylpropan-1-one: the reaction conditions are the same as 1-(2,5-dimethylphenyl in Example 1 )-2-methylpropane-1-ketone synthesis, only p-xylene is replaced by p-methyl anisole, 72.8 grams of 1-(2-methoxy-5-methylphenyl)-2- Methylpropan-1-one, 51% yield. 1 H-NMR (300MHz, CDCl 3 ,δinppm):7.58(s,1H,Ar-H),7.13(s,1H,Ar-H),6.73(s,1H,Ar-H),3.73(s,3H,OCH 3 ),3.34(sept,1H,CH(CH 3 ) 2 ),2.35(s,3H,Ar-CH 3 ),1.23(d,6H,CHCH 3 ). Elem.Anal.Calcd.ForC 12 h 16 o 2 : C, 75.0%; H, 8.33%; O, 16.67%. Found: C, 74.95%; H, 8.31%; O, 16.74%. ESI-MS: m / z193.10 ([M+H] + ).
[0065](2) Synthesis of α-bromo-2-methoxy-5-methylisobutyrophenone: the reaction conditions are the same as those in Example 1 for the synthesis of α-bromo-2,5-dimethylisobutyrophenone, only 1-(2,5-Dimethylphenyl)-2-methylpropan-1-one was replaced by 1-(2-methoxy-5-methylphenyl)-2-methylpropane-1- ketone t...
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