Pyrenylated hyperbranched polyethylene and its application in the preparation of graphene
A technology of hyperbranched polyethylene and graphene, which is applied in the field of graphene preparation, can solve problems such as difficulty in obtaining wide application, difficulty in removing surfactants, and decline in electrical properties of graphene, so as to improve the strength of non-covalent interaction and maintain the original There are performance advantages and the effect of improving dispersion stability
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Embodiment 1
[0053] Embodiment 1, comparative example 1
[0054] 1. Sample preparation
[0055] (1) The preparation of embodiment 1 sample is carried out as follows:
[0056] Step 1: Under nitrogen protection, add 1-pyrenemethanol (5.0g / 0.022mol), triethylamine (18mL / 0.13mol) and anhydrous grade THF (230mL) in sequence in a 250mL Schlenk reaction flask, at room temperature Stirred at low temperature for 10 min to form a solution, then added dropwise acryloyl chloride (10.5 mL / 0.13 mol) previously dissolved in 30 mL of anhydrous THF within 4 h under the control of an ice bath, and continued stirring at room temperature for 24 h after the addition was complete. After the reaction was finished, the salt and by-products generated by the reaction were removed by filtration, and the obtained filtrate was concentrated to obtain an oily product. After dissolving in 100 mL of dichloromethane, it was successively passed through hydrochloric acid aqueous solution (mass concentration 1%), saturated a...
Embodiment 2
[0069] Embodiment 2, comparative example 2
[0070] 1. Sample preparation
[0071] (1) The preparation of embodiment 2 sample is carried out as follows:
[0072] Step 1: Under nitrogen protection, add 1-pyrenemethanol (5.0g / 0.022mol), triethylamine (18mL / 0.13mol) and anhydrous grade THF (200mL) in sequence in a 500mL Schlenk reaction flask, at room temperature Stir at low temperature for 20 min to form a solution, then dropwise add acryloyl chloride (10.5 mL / 0.13 mol) previously dissolved in 50 mL of anhydrous THF under the control of an ice bath within 4 h, and continue stirring at room temperature for 24 h after the addition is complete. After the reaction was over, the salt and by-products generated by the reaction were removed by filtration, and the obtained filtrate was concentrated to obtain an oily product. After being dissolved in 100 mL of dichloromethane, it was washed 18 times with aqueous hydrochloric acid (mass concentration 1%), and saturated aqueous sodium bica...
Embodiment 3
[0087] Embodiment 3, comparative example 3
[0088] 1. Sample preparation
[0089] (1) The preparation of embodiment 3 sample is carried out as follows:
[0090] Step 1: For the synthesis steps and process of pyrenylated HBPE, refer to Steps 1 and 2 in Example 2.
[0091] Step 2: Add natural flake graphite (120mg), analytically pure THF (60mL) and pyrenylated HBPE (120mg) obtained in the first step above into a 100mL cylindrical glass bottle, seal it and place it in a 250W ultrasonic The total ultrasonic time was 132 hours at constant temperature in the pool at 25°C. Sampling was carried out at 12h, 24h, 32h, 48h, 72h and 132h respectively during the period, each sampling volume was 10mL, and the graphene initial dispersion liquid corresponding to each time was obtained, and further centrifuged at 4000rpm at a low speed for 45min, and then stood still for 8h to obtain A series of corresponding graphene dispersions containing excess pyrenylated HBPE (note: the feeding concen...
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