• 专利标题:   Preparing functionalized graphene oxide sponge comprises e.g. reacting p-tert-butylphenol and formaldehyde in a sodium hydroxide solution, filtering and washing with diethyl ether, drying, heating centrifuging and vacuum drying.
  • 专利号:   CN109092259-A
  • 发明人:   LIU S, MA J, LUO J, ZHANG H, LI S, ZHANG Y
  • 专利权人:   UNIV EAST CHINA TECHNOLOGY
  • 国际专利分类:   B01J020/22, B01J020/28, B01J020/30, C02F001/28
  • 专利详细信息:   CN109092259-A 28 Dec 2018 B01J-020/22 201921 Pages: 13 Chinese
  • 申请详细信息:   CN109092259-A CN11209147 17 Oct 2018
  • 优先权号:   CN11209147

▎ 摘  要

NOVELTY - Preparing functionalized graphene oxide sponge comprises e.g. reacting p-tert-butylphenol and formaldehyde in a sodium hydroxide solution to obtain a p-tert-butylcalix(4)arene as product A, reacting product A with anhydrous aluminum chloride to obtain de-t-butylcalix(4)arene as product B, mixing 1 g product B and 10 ml concentrated sulfuric acid, and stirring mixture and heating at 60 degrees C for 4 hours, filtering mixture suction and washing with diethyl ether, drying obtained solid under vacuum at 60 degrees C to obtain a sulfonated cup (4) arene, stirring at high speed for 30 minutes, slowly adding 80-100 ml deionized water and gradually heating up to 98 degrees C for 30 minutes, adding 1.5-3 ml 30% hydrogen peroxide and 30-50 ml deionized water, and washing with a large amount of deionized water, ultrasonically dispersing washed to neutral graphite oxide in water, ultrasonically shaking for 1 hour, and centrifuging, and vacuum drying at 60 degrees C, adding 40-50 mg sulfonated cup (4) arene for 10 minutes. USE - The method is useful for preparing functionalized graphene oxide sponge. ADVANTAGE - The method is simple. The sponge has large surface area and high supramolecular recognition. DETAILED DESCRIPTION - Preparing functionalized graphene oxide sponge comprises (i) reacting p-tert-butylphenol and formaldehyde in a sodium hydroxide solution to obtain a p-tert-butylcalix(4)arene as product A, reacting product A with anhydrous aluminum chloride to obtain de-t-butylcalix(4)arene as product B, mixing 1 g product B and 10 ml concentrated sulfuric acid, and stirring mixture and heating at 60 degrees C for 4 hours, filtering the mixture suction and washing with diethyl ether, drying the obtained solid under vacuum at 60 degrees C to obtain a sulfonated cup (4) arene, and (ii) adding graphene oxide In an ice water bath, adding 2-3 g graphite powder and 1-1.5 g sodium nitrate to 45-70 ml of concentrated sulfuric acid, stirring at high speed for 30 minutes, keeping the reaction temperature below 20 degrees C, slowly adding 6-9 g potassium permanganate, removing the ice bath, slowly heating the solution to 35 degrees C, stirring the reaction for 1 hour, slowly adding 80-100 ml deionized water and gradually heating up to 98 degrees C for 30 minutes, adding 1.5-3 ml 30% hydrogen peroxide and 30-50 ml deionized water, the solution turned bright yellow, filtering the obtained filter cake first washing with 5% hydrochloric acid until the filtrate nearly neutral, and washing with a large amount of deionized water, ultrasonically dispersing the washed to neutral graphite oxide in water, ultrasonically shaking for 1 hour, and centrifuging, and vacuum drying at 60 degrees C, and (iii) ultrasonically dispersing 40-50 mg GO uniformly in 20-30 ml water, 40-50 mg sulfonated cup (4) arene for 10 minutes, carrying out the reaction in a reaction vessel at 160-180 degrees C for 10-12 hours, cooling to room temperature, taking out the graphene hydrogel, washing with deionized water and immersing for 48 hours, and freeze-drying product to obtain S-GOS.