• 专利标题:   Preparing flame-retardant conductive composite polyimide film involves adding phosphorus flame retardant material into deoxidizing solvent, performing high power ultrasonic treatment to obtain uniform second filler dispersion, and coating composite polyamic acid solution on substrate.
  • 专利号:   CN115960460-A
  • 发明人:   LIU S, HAN C, TANG Z, LIU C, BEI R
  • 专利权人:   WUXI SHUNYIRUI NEW MATERIAL RES CO LTD, WUXI SHUNXUAN OPTOELECTRONIC TECHNOLOGY, WUXI SHUNXUAN NEW MATERIALS CO LTD
  • 国际专利分类:   C08G073/10, C08J005/18, C08K003/02, C08K003/04, C08L079/08
  • 专利详细信息:   CN115960460-A 14 Apr 2023 C08L-079/08 202342 Chinese
  • 申请详细信息:   CN115960460-A CN10231860 13 Mar 2023
  • 优先权号:   CN10231860

▎ 摘  要

NOVELTY - Preparing flame-retardant conductive composite polyimide film involves mixing carbon-based conductive filler with solvent and dispersant, crushing and grinding to obtain uniform first filler dispersion; adding phosphorus flame retardant material into deoxidizing solvent, carrying out ball milling dispersion, after filtering, performing high power ultrasonic treatment to obtain uniform second filler dispersion; mixing first filler dispersion with second filler dispersion according to proportion, crushing and grinding to obtain composite filler slurry; adding diamine monomer into solvent, stirring and adding composite filler slurry, after uniformly mixing, adding dianhydride monomer, namely preparing composite polyamic acid solution with certain viscosity; coating composite polyamic acid solution on substrate for curing, namely obtaining flame-retardant conductive polyimide film; and directly heating and solidifying program. USE - Method for preparing flame-retardant conductive composite polyimide film. ADVANTAGE - The method enables to have good conductivity and good flame retardant, forms complexation/bonding effect, reduces hydrogen free radical, realizes synergistic flame retardant effect, and improves safety coefficient. DETAILED DESCRIPTION - Preparing flame-retardant conductive composite polyimide film involves mixing carbon-based conductive filler with solvent and dispersant, crushing and grinding to obtain uniform first filler dispersion; adding phosphorus flame retardant material into deoxidizing solvent, carrying out ball milling dispersion, after filtering, performing high power ultrasonic treatment to obtain uniform second filler dispersion; mixing first filler dispersion with second filler dispersion according to proportion, crushing and grinding to obtain composite filler slurry; adding diamine monomer into solvent, stirring and adding composite filler slurry, after uniformly mixing, adding dianhydride monomer, namely preparing composite polyamic acid solution with certain viscosity; coating composite polyamic acid solution on substrate for curing, namely obtaining flame-retardant conductive polyimide film; directly heating and solidifying program; or, peeling pre-cured film from substrate, curing at high temperature by drying tunnel; keeping temperature for 0.2-1 hours at 150-250℃; where technique of high temperature solidifying is to raise temperature to 300-450℃ at speed of 1-8℃/minute; where carbon-based conductive filler is carbon black, carbon nano-tube, graphene, graphite alkyne and fullerene, carbon black is conductive carbon black having particle diameter of 10 nm-10 microns; thickness of graphene 1-50 nm, sheet diameter is 100 nm-10 microns of single-layer graphene or graphene, graphene is pure graphene, reduction oxidation graphene length of carbon nano-tube is 1-50 m, diameter is 2-100 nm, and carbon nano-tube is amination carbon nano-tube, nitrogen-doped carbon nano-tube, carboxylated carbon nano-tube, hydroxylated carbon nano-tube, and carbon nanotube is single-wall carbon nano tube, double-wall carbon nano-tube or multi-wall carbon nano-tube; phosphorus flame retardant material is black phosphorus, phosphate and phosphite ester, black phosphorus is obtained by processing black phosphorus, and size of black phosphorus is 100 nm-50 microns, thickness of sheet layer is 1-100 nm; first filler is 5-60 wt.% polyimide, and dispersant is polyvinyl pyrrolidone, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and 0.1-2 wt.% polyimide filler, and oxygen removing solvent is inert organic solvent bubbling for 2-5 hours; ball milling zirconium ball particle diameter is 0.1-5 mm, ball milling dispersing time is 1-24 hours, frequency of ultrasonic dispersing is 5-40 kHz, power is 500-6000 watt, ultrasonic processing time is 1-24 hours, and ultrasonic processing temperature is 20-30℃. An INDEPENDENT CLAIM is included for a flame-retardant conductive composite polyimide film, which is prepared by preparation method, where limit oxygen index of conductive composite polyimide film reaches 66.2%.