• 专利标题:   Manufacture of sulfonated graphene oxide/high-solid-content aqueous polyurethane emulsion involves reacting dimethylolpropionic acid, sulfonated graphene oxide dispersion and oligomer diol-isophorone diisocyanate prepolymer, and emulsifying.
  • 专利号:   CN107383302-A
  • 发明人:   FENG J, WANG X, LUO X, WANG Y, BAI P
  • 专利权人:   UNIV SHAANXI SCI TECHNOLOGY
  • 国际专利分类:   C01B032/23, C08G018/10, C08G018/12, C08G018/34, C08G018/44, C08G018/48, C08G018/66, C08G018/75, C08K003/04, C08K009/04, C08L075/04, C08L075/08
  • 专利详细信息:   CN107383302-A 24 Nov 2017 C08G-018/10 201806 Pages: 14 Chinese
  • 申请详细信息:   CN107383302-A CN10570823 13 Jul 2017
  • 优先权号:   CN10570823

▎ 摘  要

NOVELTY - Manufacture of sulfonated graphene oxide/high-solid-content aqueous polyurethane emulsion involves mixing 15-20 g oligomeric diol and 5-10 g isophorone diisocyanate, adding organotin catalyst, reacting at 80-90 degrees C for 1-2 hours to prepare a prepolymer, adding 30-100 ml dimethylolpropionic acid and sulfonated graphene oxide-acetone dispersion and/or sulfonated graphene oxide-aqueous dispersion to the prepolymer, reacting for 2-4 hours, cooling to 60 degrees C, adding dimethylolpropionic acid and low-molecular amine, neutralizing, adding deionized water, emulsifying, and distilling acetone. USE - Manufacture of sulfonated graphene oxide/high-solid-content aqueous polyurethane emulsion (claimed). ADVANTAGE - The method enables efficient manufacture of sulfonated graphene oxide/high-solid-content aqueous polyurethane emulsion with excellent mechanical property and hydrolysis resistance, and high solid content. DETAILED DESCRIPTION - Manufacture of sulfonated graphene oxide/high-solid-content aqueous polyurethane emulsion involves mixing 15-20 g oligomeric diol and 5-10 g isophorone diisocyanate in ratio of (3-5):1, adding organotin catalyst, reacting at 80-90 degrees C for 1-2 hours to prepare a prepolymer, adding 30-100 ml dimethylolpropionic acid and sulfonated graphene oxide-acetone dispersion and/or sulfonated graphene oxide-aqueous dispersion to the prepolymer, reacting for 2-4 hours, cooling to 60 degrees C, adding dimethylolpropionic acid and low-molecular amine, neutralizing for 30 minutes, adding 20-40 ml deionized water, emulsifying under high shear force for 30 minutes, and distilling acetone. The solid content of the sulfonated graphene oxide/high-solid-content aqueous polyurethane emulsion is 40-55%. The sulfonated graphene oxide dispersion is sulfonated graphene oxide-acetone dispersion obtained by dispersing sulfonated graphene oxide in acetone, and ultrasonically processing under power of 300-600 W for 0.5-2 hours, or sulfonated graphene oxide aqueous dispersion obtained by dispersing sulfonated graphene oxide in acetone, and ultrasonically processing under power of 300-600 W for 0.5-2 hours. The sulfonated graphene oxide-acetone dispersion has sulfonated graphene oxide concentration of 0.5-5 mg/ml. The sulfonated graphene oxide aqueous dispersion has sulfonated graphene oxide concentration of 0.5-10 mg/ml. The sulfonated graphene oxide is obtained by mixing 0.2-2 g graphite oxide, 1.6-16 g sodium hydroxide, 200-1000 ml deionized water and 3-30 g sodium 2-chloroethanesulfonate, ultrasonically treating at 20 degrees C and power of 300-1000 W for 1-5 hours, adding nitric acid, reacting for 20-40 minutes, adjusting pH to 6.5-7.5, centrifuging at rate of 5000-10000 rpm for 5-10 minutes, washing with ethanol 3-5 times, and drying. The graphite oxide is obtained by mixing expanded graphite, sodium nitrate, and concentrated sulfuric acid in an ice water bath, reacting for 1 hour, adding potassium permanganate, reacting for 6 hours, diluting the mixture with deionized water, adding hydrogen peroxide, stirring until no bubbles, separating, adding 0.01 mol/L hydrochloric acid to the supernatant, centrifuging, washing the precipitate with ethanol, dialyzing for 48-72 hours, adjusting pH to 6.5-7, adding barium chloride, and freeze-drying.