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Synthesis of prepolymers and characterization

 

Thermal polyesterification of itaconic acid (IA), polyethylene glycol 400 (PEG-400)

 

 

Polymers were prepared in dependence on the experimental procedures of Barrett et al.^[1]

The procedure requires exact masses. Therefore an analytical balance (4 decimal places) was used and if not otherwise stated PEG as well as itaconic acid were pre-dried before use on a high vacuum line (< 10^-3 mbar) overnight.

To avoid contamination with oxygen during the reaction and to remove produced water, common Schlenk technique was applied. As inert gas argon was used.

 

A1

Date: 02/06/15 – 03/06/15

Lab members: AW, SZ

 

Preparation process:

A 50 mL Schlenk flask was loaded with 1.213 g (3.033 mmol, 1 eq.) PEG-400 and 0.395 g (3.032 mmol, 1 eq.) itaconic acid and flushed with argon. Within 20 minutes the mixture was heated up to 100 °C with an oil bath and stirred under argon atmosphere. As a colorless melt had formed the vacuum was applied (3·10^-2 mbar) and the mixture was stirred at 100 °C for 17 h. The slightly yellow viscous liquid was cooled down to room temperature. 

For a picture of A1 see appendix.

 

Analysis:

No further analyses were performed.

 

A2

Date: 09/06/15 – 10/06/15

Lab members: FR, SJ

 

Preparation process:

A 25 mL Schlenk tube was loaded with 2.169 g (5.422 mmol, 1 eq.) PEG-400, 0.705 g (5.420 mmol, 1 eq.) itaconic acid and capped with a septum. Within an hour the mixture was heated up to 145 °C with an oil bath and stirred under argon atmosphere. As a colorless melt had formed the vacuum was applied (< 10^-3 mbar) and the mixture was stirred at 145 °C for 24 h. The slightly yellow viscous liquid was cooled down to room temperature.

For a picture of A2 see appendix.

 

Visual Observations:

During the reaction itaconic acid recrystallised on the flask surface which wasn’t dipped into the oil bath. Therefore the ratio between itaconic acid and PEG-400 has changed.

 

Analysis:

The product was analyzed by differential scanning calorimetry DSC to identify the glass transition (T_g) temperature.

The T_g of A2 is -4.7 °C.

 

Figure 1: DSC- Plot of A2. The T_g of A2 is -4.7 °C