1-Octene → 1-Octene t-butylstyrene divinylbenzene

HRID 516195Notes

Reaction equation

HRID 516195 reaction equation
[CH2:1]=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[C:9]([CH:13]=[CH:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([CH3:12])([CH3:11])[CH3:10]>C1(C)C=CC=CC=1>[CH2:1]=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[C:9]([CH:13]=[CH:14][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)([CH3:12])([CH3:10])[CH3:11].[CH:2]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH:9]=[CH2:10])=[CH2:1]

Participants

4

Reactant 2

HCID 81251-OcteneHCID 138033tert-Butylstyrene

Product 1

HCID 866624871-Octene t-butylstyrene divinylbenzene

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

The polymerization reaction was conducted in a 300 ml stainless autoclave equipped with a mechanical stirrer. In an argon filled dry-box, the reactor was charged with 50 ml of toluene, 0.2 ml of DVB, and various volume ratios of 1-octene and tert-butylstyrene (Oct/BSt=7/3, 6/4, 5/5, 6/4, and 7/3 ml). The reactor was then sealed and then moved from the dry box and purged with nitrogen gas at 30° C. About 0.101 g of TiCl3(AA) and 1 ml of AlCl2Et in 10 ml of toluene, after mixing for 20 minutes by stirring, were introduced to the reactor under nitrogen pressure to initiate the polymerization. After about 1 hour, the reaction was terminated by adding 100 ml of dilute HCl solution in methanol to the reactor. The 1-octene/t-butylstyrene/divinylbenzene terpolymers were isolated by filtration and washed completely with methanol and dried under vacuum for about 8 hours. The resulting terpolymers were completely soluble in common organic solvents, including toluene and decalin. Before absorption measurement, the resulting terpolymers were divided into ½ inch sized particles and heated in an oven at about 220° C. for about 2 hours to obtain fully cross-linked samples. Table 3 provides absorption capacity data for the samples in toluene after 5 hours and 16 hours.

Workup

  1. customThe polymerization reaction
  2. customequipped with a mechanical stirrer
  3. customThe reactor was then sealed
  4. custompurged with nitrogen gas at 30° C
  5. additionAbout 0.101 g of TiCl3(AA) and 1 ml of AlCl2Et in 10 ml of toluene, after mixing for 20 minutes
  6. additionwere introduced to the reactor under nitrogen pressure
  7. customthe polymerization
  8. customthe reaction was terminated
  9. additionby adding 100 ml of dilute HCl solution in methanol to the reactor

Sources & evidence

ORD record
ord-436597a392bb4bc08ca9aa3a8b13d267
Source dataset
uspto-grants-2015_08
Patent number
US09109057B2

Reaction notes

Loading…