• 专利标题:   Preparing epoxy side chain liquid crystal grafted graphene oxide comprises reacting functionalized graphene oxide and epoxypropyl 4-((4'-acryloyloxy)benzoyloxy)benzoate liquid crystal monomer, precipitating, filtering, washing and drying.
  • 专利号:   CN103539911-A, CN103539911-B
  • 发明人:   LU S, YU J, QI B, YUAN Z
  • 专利权人:   UNIV GUILIN TECHNOLOGY
  • 国际专利分类:   C08F220/32, C08F292/00, C08L051/10, C08L063/00, C09K019/38
  • 专利详细信息:   CN103539911-A 29 Jan 2014 C08F-292/00 201431 Pages: 7 Chinese
  • 申请详细信息:   CN103539911-A CN10353234 14 Aug 2013
  • 优先权号:   CN10353234

▎ 摘  要

NOVELTY - Preparing epoxy side chain liquid crystal grafted graphene oxide comprises adding 0.1-1 g functionalized graphene oxide and 3-30 g epoxypropyl 4-((4'-acryloyloxy)benzoyloxy)benzoate liquid crystal monomer into 250 ml three-necked flask, adding 20-100 ml N,N-dimethylformamide and 0.05-0.5 g azobisisobutyronitrile, under nitrogen protection, reacting by heating to 20-80 degrees C and stirring for 10-30 hours, completing the reaction, precipitating with water, filtering, washed and drying to obtain gray and black product. USE - The method is useful for preparing epoxy side chain liquid crystal grafted graphene oxide (claimed). ADVANTAGE - The preparation method has easy-to-get raw materials, simple process flow, good reproducibility and low pollution. The obtained epoxy resin has improved mechanical properties and thermal properties. DETAILED DESCRIPTION - Preparing epoxy side chain liquid crystal grafted graphene oxide comprises (i) adding 1.5-15 g p-hydroxybenzoic acid and 20-70 ml N,N-dimethylformamide into 250 ml three-necked flask, stirring to dissolve, adding 2-15 ml pyridine, dropwise adding 1.5-15 ml acryloyl chloride under ice-cooling condition into the above solution, stirring the mixture at 20-70 degrees C for 15-30 hours, completing the reaction, precipitating with water, filtering, washing and drying; (ii) adding 2-20 g dried product into 250 ml three-necked flask, adding 5-25 ml thionyl chloride and 2-10 drops of N,N-dimethylformamide, under nitrogen protection, stirring at room temperature for 4-12 hours, heating to 30-75 degrees C for 2-10 hours, completing the reaction, vacuum distilling to remove excess thionyl chloride, adding 10-30 ml N,N-dimethylformamide, and formulating into mixed solution; (iii) adding 1.5-15 g p-hydroxybenzoic acid and 20-70 ml N,N-dimethylformamide into 250 ml three-necked flask, stirring to dissolve, dropwise adding 10-30 ml N,N-dimethylformamide, mixing, adding 3-15 ml pyridine, under nitrogen protection, reacting by heating to 20-70 degrees C, and stirring for 10-20 hours, precipitating with water, filtering, washing, re-crystallizing and drying to obtain pale yellow unsaturated bond-containing 4-(4-acryloyloxy)benzoyloxy benzoate liquid crystal monomer; (iv) adding 4-(4-acryloyloxy)benzoyloxy benzoate liquid crystal monomer into 250 ml three-necked flask, adding 5-25 ml thionyl chloride and 2-10 drops N,N-dimethylformamide, under nitrogen protection, reacting by stirring at room temperature for 5-12 hours, heating to 30-75 degrees C for 2-10 hours, completing the reaction, vacuum distilling to remove excess thionyl chloride, adding 10-50 ml N,N-dimethylformamide and formulating into mixed solution; (v) adding 0.8-8 ml glycidol and 5-15 ml pyridine into the mixed solution, reacting by heating to 20-70 degrees C and stirring for 10-30 hours, completing the reaction, precipitating with water, filtering, washing and drying to obtain pale yellow unsaturated bond-containing epoxypropyl 4-((4'-acryloyloxy)benzoyloxy)benzoate liquid crystal monomer; (vi) adding 0.1-1 g graphite oxide and 20-80 ml N,N-dimethylformamide into 250 ml three-necked flask, ultrasonicating for 30-120 minutes and uniformly dispersing and oxidizing graphene to obtain mixed solution; (vii) adding 2-20 ml acryloyl chloride and 5-15 ml pyridine into the mixed solution, magnetically stirring to react at 20-70 degrees C for 10-30 hours, completing the reaction, centrifuging and washing to obtain functionalized graphene oxide; (viii) adding 0.1-1 g functionalized graphene oxide and 3-30 g epoxypropyl 4-((4'-acryloyloxy)benzoyloxy)benzoate liquid crystal monomer into 250 ml three-necked flask, adding 20-100 ml N,N-dimethylformamide and 0.05-0.5 g azobisisobutyronitrile, under nitrogen protection, reacting by heating to 20-80 degrees C and stirring for 10-30 hours, completing the reaction, precipitating with water, filtering, washed and drying to obtain gray and black product. The graphite oxide is chemically pure flake graphite, the oxidation is Hummers oxidation method, and p-hydroxybenzoic acid is of industrial grade; and acryloyl chloride, thionyl chloride, glycidol, pyridine and N,N-dimethylformamide are of analytical grade.