Industry share: A solvent based conductive pressure sensitive adhesive preparation method 3

A solvent-based conductive pressure-sensitive adhesive preparation method 3

(1) The expanded graphite was dispersed in an ethanol solution with 20 times the mass fraction of the expanded graphite, stirred at 200rpm for 12h, ultrasonic dispersed at 80kHz for 12h, filtered, and washed with deionized water until the lotion was neutral, and graphite sheets were obtained; The graphite sheet was mixed with sodium hydroxide solution with 10 times the mass fraction of the graphite sheet and 10% of the mass fraction. The graphite sheet was ultrasonically dispersed at 80kHz for 4h, and then the stannous chloride hydrochloric acid solution with 3 times the mass fraction of the graphite sheet was added.

After 1h reaction, Add palladium chloride hydrochloric acid solution (10% mass fraction of graphite sheet) and boric acid solution (0% mass fraction of graphite sheet), continue to react for 3h, filter, and wash with deionized water for 8 times, and transfer to silver ammonia solution (20% mass fraction of graphite sheet).

Formaldehyde solution with a mass fraction of 10% was added at 7ml/min below 100rpm while stirring, and the mass ratio of formaldehyde solution to silver ammonia solution was 5:1. After the drip was finished, it was left to stand for 8h, filtered, washed with deionized water for 5 times, and transferred to a drying oven and dried at 100℃ for 6h to prepare silver-plated nano graphite sheets. Butyl acrylate, isobutyl acrylate, hydroxyethyl acrylate, acrylic acid, methyl methylate acrylate, and silver-plated nano graphite sheets were mixed in a stirring kettle according to a mass ratio of 35:30:1:5:3:3:1:1.5 for mixing and stirring operation. The temperature was adjusted to 30℃ for continuous mixing and stirring for 15min to prepare the pressure-sensitive adhesive mixture.

(2) In the nitrogen atmosphere, heat diamino propyl tetramethyl disiloxane to 95℃, add diamino propyl tetramethyl disiloxane 0.015 times the mass of tetramethyl disiloxane, reaction 1.5 h later, add diamino propyl tetramethyl disiloxane mass of 2.2 times the methyl phenyl siloxane ring body, continue to react for 10h, temperature rise to 140℃.

After 1.5h of reaction, cooling to room temperature, reducing pressure to 10mmHg, warming to 160℃, and holding for 6h, terminal aminopropyl polymethyl phenyl siloxane was prepared. Under a nitrogen atmosphere, ammonia will end with propyl methyl phenyl siloxane and N, N  dimethyl formamide mixed in quality than 1:15 stir until dissolved, after joining the ammonia propyl methyl phenyl siloxane quality 0. 28 times are benzene tetracarboxylic acid two poles, continue to stir until dissolved, after let stand for 30 h, produce self-adhesive;

(3) The mass ratio of phenol, epichlorohydrin, and potassium hydroxide was 5:20: 2 Mixed and heated in a water bath to 80℃, stirred at 100rpm for 8h, added epichlorohydrin with 0.2 times the mass of potassium hydroxide, heated to 90℃, continued to stir for 8h, and filtered with 300 mesh filter while hot and steamed for 2 ~ 3h, then filtered again with 300 mesh filter to obtain aryl epichlorohydrin; The mass ratio of aroxyepichlorohydrin, phenol, formaldehyde, and ammonia water with the mass fraction of 5 ~ 10% is 1:8:3: After stirring at 200rpm for 5h, pressure reduction distillation for 8h was carried out at 0.004mpa at the same temperature. After vacuum distillation, the heating was stopped.

When cooling to 40℃, anhydrous ethyl alcohol with a mass of 0.6 aryl oxyepxychlorohydrin was added, and viscosifying 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 kettle, and the pressure-sensitive glue mixture mass is 0.02 times benzoyl peroxide, the pressure-sensitive glue mixture mass is 0.08 times viscosifying resin, and pressure sensitive glue mixture mass 0.15 times self-made crosslinking agent are added.

The temperature is raised to 80℃. After the reaction for 50min, add pressure-sensitive adhesive mixture A to mix the stirring raw materials, cool down to 75℃, react for 5h, and stand for 1.5h, solvent type conductive pressure-sensitive adhesive is prepared.