• 专利标题:   Preparation of graphene oxide surface-modified carbon fiber involves adding 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride to aqueous solution of graphene oxide, activating, adding e.g. aminated carbon fiber, and reacting.
  • 专利号:   CN105040412-A
  • 发明人:   HAN W, HONG C, HU P, ZHAO G, ZHANG X, CHENG Y, AN J, DU H, ZHOU S
  • 专利权人:   HARBIN INST TECHNOLOGY
  • 国际专利分类:   C01B031/04, D06M101/40, D06M011/74
  • 专利详细信息:   CN105040412-A 11 Nov 2015 D06M-011/74 201628 Pages: 16 Chinese
  • 申请详细信息:   CN105040412-A CN10523168 24 Aug 2015
  • 优先权号:   CN10523168

▎ 摘  要

NOVELTY - Preparation of graphene oxide surface-modified carbon fiber involves diluting aqueous solution of graphene oxide to concentration of 0.1-0.5 mg/mL in a round bottom flask with stirring, adding 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride, activating for 15 minutes, obtaining solution (B), adjusting pH of solution (B) to 7.2-7.5, adding N-hydroxysuccinimide, vibrating for 1 minute, adding alkali, uniformly dispersing, adding aminated carbon fiber, reacting at room temperature for 24 hours and vacuum-drying. USE - Preparation of graphene oxide surface-modified carbon fiber (claimed). ADVANTAGE - The method enables preparation of graphene oxide surface-modified carbon fiber with excellent surface wettability, adhesiveness, roughness, interface property, damage resistance, mechanical property and thermal stability. DETAILED DESCRIPTION - Preparation of graphene oxide surface-modified carbon fiber involves extracting carbon fiber in a Soxhlet extractor using acetone as a solvent, reflux-condensing at 70 degrees C for 48 hours, drying, adding dried carbon fiber to 69% concentrated nitric acid, heating at 80-100 degrees C for 3-4 hours in an oil bath, washing resultant fiber with water to neutral, vacuum-drying, placing obtained acidified carbon fiber in a round bottom flask, adding deionized water, stirring, adjusting pH to 4-6, adding 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride, activating for 15 minutes, obtaining solution (A), adding polyethyleneimine to a beaker, adding deionized water, ultrasonically processing for 5 minutes, obtaining polyethyleneimine aqueous dispersion, adjusting pH of solution (A) to 7.2-7.5, adding N-hydroxysuccinimide and polyethyleneimine aqueous dispersion, reacting at room temperature for 24 hours, vacuum-drying, obtaining aminated carbon fiber, diluting aqueous solution of graphene oxide to concentration of 0.1-0.5 mg/mL in a round bottom flask with stirring, adding 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride, activating for 15 minutes, obtaining solution (B), adjusting pH of solution (B) to 7.2-7.5, adding N-hydroxysuccinimide, vibrating for 1 minute, adding alkali, uniformly dispersing, adding aminated carbon fiber, reacting at room temperature for 24 hours and vacuum-drying. The content ratio of acidified carbon fiber and deionized water is 1 mg:0.25-0.55 mL. The mass ratio of acidified carbon fiber and 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride is 1-3:1. The content ratio of carbon fiber and acetone is 1 g:4-8 mL. The content ratio of carbon fiber and 69% concentrated nitric acid is 1 g:4-8 mL. The aqueous solution of graphene oxide is prepared by adding graphite powder, 98% concentrated sulfuric acid (S1), sodium nitrate and potassium permanganate (P1) to a round bottom flask under ice cooling condition, heating at 35 degrees C for 7 hours, cooling the reaction mixture, placing the round bottom flask in an ice-water bath, adding 98% concentrated sulfuric acid (S2) and potassium permanganate (P2), heating at 35 degrees C for 12 hours, adding ice water to the round bottom flask, stirring, adding hydrogen peroxide solution such that color is changed from black-brown to bright yellow, and ultrasonically washing resultant product with 5% hydrochloric acid and deionized water to pH of 4-6 for 2-3 hours. The mass ratio of graphite powder and 98% concentrated sulfuric acid (S1) is 1:40-5. The mass ratio of graphite powder and sodium nitrate is 2:1. The mass ratio of graphite powder and potassium permanganate (P1) is 1:3. The mass ratio of graphite powder and 98% concentrated sulfuric acid (S2) is 1:8-11. The mass ratio of graphite powder and potassium permanganate (P2) is 1:1-1.5. The mass ratio of polyethyleneimine and acidified carbon fiber is 1:1-8. The content ratio of polyethyleneimine and deionized water is 20-160 mg:1 mL. The mass ratio of 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and N-hydroxysuccinimide is 4-10:1. The mass ratio of graphene oxide aqueous solution and 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride is 1-3:1. The mass ratio of graphene oxide solution and aminated carbon fiber is 0.01-0.1:1.