• 专利标题:   Preparing high flame retardant polyurethane composite material comprises mixing ethanol with water, adding phosphorus oxychloride into N, N-dimethyl formamide, mixing, adding pyridine, Ziegler-Natta catalyst, reacting, adding the cobalt chloride, centrifuging and cooling.
  • 专利号:   CN113512284-A, CN113512284-B
  • 发明人:   WANG L, SHI R
  • 专利权人:   JUNNENG CHEM LONGNAN CO LTD
  • 国际专利分类:   C08K013/06, C08K007/06, C08K003/22, C08K007/00, C08K005/5313, C08K003/32, C08K005/00, C08K009/12, C08K003/04, C08K009/06, C08L075/04
  • 专利详细信息:   CN113512284-A 19 Oct 2021 C08L-075/04 202207 Chinese
  • 申请详细信息:   CN113512284-A CN10457323 27 Apr 2021
  • 优先权号:   CN10457323

▎ 摘  要

NOVELTY - Method comprises (i) mixing ethanol with water, adjusting the pH value, adding silane coupling agent KH-570 and isocyanate propyl triethoxy silane, performing hydrolysis, reacting, filtering, washing, drying to obtain material A, (ii) adding phosphorus oxychloride into N, N-dimethyl formamide, mixing uniformly, adding triethylamine, dropping N, N dimethyl formamide solution of hydroxyethyl acrylate, adding pyridine, dropping N, N-dimethyl formamide solution of 4,4'-diamino diphenyl ether, reacting, filtering, water washing, drying to obtain the material B, (iii) adding cyclohexane, stirring material A and Ziegler-Natta catalyst, adding material B, reacting, washing, drying to obtain material C, (iv) adding the cobalt chloride into the mixed solution of N, N-dimethyl formamide and water, adding material C, centrifuging, washing, drying to obtain material D, (v) adding e.g. thermoplastic polyurethane elastomer and carbon fiber, banburying, and cooling to room temperature. USE - The method is useful for preparing high flame retardant polyurethane composite material. DETAILED DESCRIPTION - Preparing high flame retardant polyurethane composite material comprises (i) mixing ethanol with water, adjusting the pH value to 5-6, adding silane coupling agent KH-570 and isocyanate propyl triethoxy silane, performing hydrolysis, adding graphene, then stirring and reacting for 3.5-5.5 hours at 65-75degrees Celsius, finishing reaction, filtering, washing, drying to obtain material A, (ii) adding phosphorus oxychloride into N, N-dimethyl formamide at the temperature of 0 to -5degrees Celsius under the protection of nitrogen, mixing uniformly, adding triethylamine, dropping N, N dimethyl formamide solution of hydroxyethyl acrylate, finishing dropping, preserving temperature and reacting for 7-11 hours at 0 to -5degrees Celsius, adding pyridine, dropping N, N-dimethyl formamide solution of 4,4'-diamino diphenyl ether, finishing dropping, raising the temperature to 70-80degrees Celsius, reacting for 3-6 hours, filtering, water washing, drying to obtain the material B, (iii) adding cyclohexane in a sealed reactor, stirring the material A and Ziegler-Natta catalyst, replacing by argon gas, adding material B, reacting at 55-65degrees Celsius for 30-150 minutes under the condition of 1-1.5 MPa, adding hydrochloric acid, separating solid and liquid, washing, drying to obtain material C, (iv) adding the cobalt chloride into the mixed solution of N, N-dimethyl formamide and water, adding material C and mixing uniformly, then adding triethylene diamine and stirring uniformly to obtain the reaction liquid, adding the reaction liquid in a hydrothermal reaction kettle for hydrothermal reaction, centrifuging, washing, drying to obtain material D, (v) adding thermoplastic polyurethane elastomer, ammonium polyphosphate, aluminium diethyl phosphinate, material D, cerium(iv) oxide nano sheet, carbon fiber and 1-ethyl-3-methyl imidazole hexafluorophosphate, banburying, taking out, cooling to room temperature to obtain the high flame retardant polyurethane composite material.