Industry share: A solvent based conductive pressure sensitive adhesive preparation method 2

A solvent-based conductive pressure sensitive adhesive preparation method 2

(1)The expanded graphite was dispersed in an ethanol solution with 15 times the mass fraction of the expanded graphite and 55%, stirred at 150rpm for 11h, ultrasonic dispersed at 70kHz for 11h, filtered, and washed with deionized water until the lotion was neutral, and graphite sheets were obtained. The graphite sheet was mixed with a sodium hydroxide solution of 8 times the mass fraction of the graphite sheet, which was 8%, and dispersed by ultrasonic at 70kHz for 3h.

Then, stannous chloride hydrochloric acid solution of 2 times the mass fraction of the graphite sheet, which was 8%, was added. After reaction for 0.5 h, Add palladium chloride hydrochloric acid solution with 2x mass fraction of 8% of graphite sheet and boric acid solution with 2x mass fraction of 8% of graphite sheet, continue to inverse for 2.5 h, filter, and wash with deionized water for 7 times, and transfer to silver ammonia solution with 15x mass fraction of graphite sheet.

Formaldehyde solution with a mass fraction of 7% was added at 6ml/min while stirring at 80rpm, and the mass ratio of formaldehyde solution to silver ammonia solution was 4:1. After the drip was finished, it was left to stand for 6h, filtered, washed with deionized water for 4 times, and transferred to a drying oven and dried at 90℃ for 6h to prepare silver-plated nano graphite sheets. Butyl acrylate, isooctane acrylate, hydroxyethyl acrylate, acrylic acid, methyl methacrylate, and silver-plated nano graphite sheets were mixed in a stirring kettle according to the mass ratio of 20:25:1:2:2:1 for mixing and stirring operation. The temperature was adjusted to 25℃ and continuously mixed and stirred for 13min to prepare the pressure-sensitive adhesive mixture.

(2) In the nitrogen atmosphere, after heating diamino propyl tetramethyl-disiloxane to 90℃, adding diamino propyl tetramethyl-disiloxane 0.01 ~ times the weight of tetramethyl disiloxane, reaction for 1 hour, adding diamino propyl tetramethyl disiloxane weight of 2.1 times the methyl phenyl siloxane ring body, continue to react for 9h, temperature rise to 135℃, reaction for 1h, After cooling to room temperature, reducing pressure to 8mmHg, heating up to 155℃, holding temperature for 5h, the aminopropyl polymethyl phenyl siloxane was prepared.

Under a nitrogen atmosphere, ammonia will end with propyl methyl phenyl siloxane and N, N  dimethylformamide according to the quality than 1:13 mix until dissolved, after joining the ammonia propyl methyl phenyl siloxane quality 0. 27 times are benzene tetracarboxylic acid two poles, continue to stir until dissolved, let stand after 26 ~ 30 h, since the system was made by the adhesive;

(3) The mass ratio of phenol, epichlorohydrin, and potassium hydroxide was 4:18: 1 Mix and heat in a water bath to 75℃, stir at 75 RPM for 6h, add epichlorohydrin 0.15 times the mass of potassium hydroxide, heat up to 85℃, continue to stir for 6h, filter with 300 mesh and steam for 2h, filter again with 300 mesh filter to obtain aryl oxychloropropyl; The mass ratio of aroxyepichlorohydrin, phenol, formaldehyde, and ammonia water with the mass fraction of 8% was 1:7:3: After stirring at 150rpm for 3h, the same temperature was maintained at 0.03MPa for 7h vacuum distillation. After vacuum distillation, the heating was stopped.

When cooling to 35℃, anhydrous ethanol with a mass of 0.5 aryl epichlorohydrin was added, and the viscose resin was prepared by stirring evenly. The pressure-sensitive glue mixture is divided into two parts: pressure-sensitive glue mixture A and pressure-sensitive glue mixture A. The pressure-sensitive glue mixture A is introduced into another stirring tank, and the pressure-sensitive glue mixture mass of 0.01 times benzoyl peroxide, pressure-sensitive glue mixture mass 0.07 times viscosifying resin, and pressure-sensitive glue mixture mass of 0.1 times self-made crosslinking agent are added.

The temperature is raised to 75℃, and the reaction time is 40min. Adding pressure-sensitive adhesive mixture A to mix the stirring raw materials, cooling to 70℃, reacting for 4h, and standing for 1h, solvent-type conductive pressure-sensitive adhesive is prepared.