Method for production of isoolefin polymers using tertiary ether
A technology of isoolefins and polymers, applied in the field of isoolefin polymers, can solve problems such as economic infeasibility
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Embodiment 1
[0168] Example 1 AlCl 3 : Initiator solution preparation
[0169] Prepare fresh AlCl daily 3 Initiator solution was used for all experiments performed that day. In the glove box, a 100 mL Erlenmeyer flask was charged with AlCl dissolved in MeCl (100 mL) 3 (0.30 g, 2.25 mmol) and cooled to -30°C. The solution was stirred using a mechanical stirrer at -30 °C at 450 rpm for 30 min. Stirring was stopped, the flask was sealed, and the solution was cooled to -95°C until use.
Embodiment 2
[0170] Example 2: General Slurry Polymerization Procedure
[0171] A 500 mL stainless steel beaker equipped with a temperature probe was placed in a pentane bath cooled to -95 °C and charged with pre-cooled methyl chloride (MeCl, 180 mL). Isobutene (20 mL, 14.24 g, 25.0 mmol) was condensed as a liquid into a pre-cooled graduated cylinder and transferred to the reaction flask. Isoprene (0.8 mL, 0.54 g, 7.92 mmol) was transferred to the reaction by pipette. The solution was stirred mechanically at 800 rpm until the temperature stabilized. Pre-prepared AlCl 3 The reaction was initiated by transferring initiator solution (3 mL, 0.0090 g, 0.0675 mmol) to the reaction via a pre-cooled pipette. Polymerizations were stirred at 800 rpm for 5 minutes unless otherwise stated. Polymerization was terminated by adding NaOH (1.0 mL, 1 wt%, 0.01 mmol) ethanol solution. The polymer cement was removed from the glove box, diluted with hexane (approximately 300 mL) and antioxidant (1.0 mL,...
Embodiment 3
[0174] Embodiment 3: MTBE solution preparation
[0175] A 100 mL Erlenmeyer flask was placed in a pentane bath cooled to -95 °C and charged with pre-cooled MeCl (100 mL). Methyl tert-butyl ether (MTBE, 5 L, 0.0037 g, 0.042 mmol) was transferred to the flask by micropipette. The flask was stirred to disperse the MTBE into the MeCl, then sealed and the solution was stored at -95 °C until use.
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