• 专利标题:   Preparation of graphene modified flame retardant and light resistant aqueous polyurethane coating used e.g. for walls, by reacting sodium carboxymethyl cellulose and ethanol into sulfonyl chloride, distilling solvent, cooling and filtering.
  • 专利号:   CN106366896-A, CN106366896-B
  • 发明人:   DUAN B, DI Z
  • 专利权人:   DUAN B, HEBEI CYSO IND TRADE GROUP CO LTD
  • 国际专利分类:   C08G018/10, C08G018/34, C08G018/48, C08G018/66, C08G018/75, C08K003/04, C08K003/26, C08K003/30, C08K003/32, C08K005/092, C08K005/098, C08K005/5419, C08K007/00, C08K009/02, C08K009/04, C09D175/08, C09D005/18, C09D007/12, C09D007/61, C09D007/62, C09D007/63
  • 专利详细信息:   CN106366896-A 01 Feb 2017 C09D-175/08 201730 Pages: 14 Chinese
  • 申请详细信息:   CN106366896-A CN10775497 31 Aug 2016
  • 优先权号:   CN10775497

▎ 摘  要

NOVELTY - A graphene modified flame retardant and light resistant aqueous polyurethane coating is prepared by adding 3-hydroxyl-7-methoxy-2-naphthoic acid, sodium carboxymethyl cellulose, ethanol, magnesium ethoxide, zinc acetate, diethanolamine and N-bromosuccinimide into ketone and sulfonyl chloride, reacting, distilling solvent, cooling and filtering, washing filter cake with hot potassium bicarbonate solution, water washing to neutral, drying, and re-crystallizing using tetrahydrofuran with methanol and acetone to obtain powder catalyst. USE - Method for preparing graphene modified flame retardant and light resistant aqueous polyurethane coating (claimed) used for walls, furniture, metal tool surface, plastics, glass, paper and textile. ADVANTAGE - The coating is environment-friendly, and has low cost. DETAILED DESCRIPTION - A graphene modified flame retardant and light resistant aqueous polyurethane coating is prepared by: (A) adding 2.2 g 3-hydroxyl-7-methoxy-2-naphthoic acid, 4.1 g sodium carboxymethyl cellulose, 1.6 g ethanol, 0.6 g magnesium ethoxide, 5.3 g zinc acetate, 4.5 g diethanolamine and 3.2 g N-bromosuccinimide into 30 ml methyl ethyl ketone and 2 ml sulfonyl chloride, reacting at 90 degrees C for 3 hours, distilling solvent, cooling and filtering, washing filter cake with hot potassium bicarbonate solution, water washing to neutral, drying, and re-crystallizing using tetrahydrofuran with methanol and acetone to obtain powder catalyst; (B) stirring 3 g sodium sulfite, 0.9 g sodium metasulfite, 3.5 g trimeric sodium phosphate, 6.2 g tea polyphenol, 4.5 g citric acid and 1.3 g dibutyl hydroxy toluene at 60 degrees C for 1 hour, adding 4.2 g aluminum carbonate and 1.6 g aluminum stearate, mixing at 70 degrees C for 2 hours, adding 2.5 g methyltriethoxysilane and 3.2 g dimethyl formamide, and stirring at 80 degrees C for 3 hours to obtain light fastness agent; (C) adding 0.05 g graphene sheet with 400 ml concentrated sulfuric acid, 0.4 g 4-(diphenylamino)phenylboronic acid and 0.3 g 3,4,5-trifluorobenzene boric acid, mixing, reacting at 70 degrees C, condensing and refluxing for 3 hours at 500 W and 100 KHz, diluting using 450 mL deionized water, filtering through 0.2 mu m microporous filtering film, washing using deionized water to neutral, drying at 80 degrees C for 8 hours, and grinding to fine powder to obtain carboxylated graphene sheets; (D) adding 0.6 g (A) and 80 g polytetrahydrofuran diol with 40 g isophorone diisocyanate into 500 ml four-mouth flask stirring paddle, reacting to 70 degrees C 1 hour, adding 0.2 g 2-sulfobenzoic acid anhydride and 0.05 g (C), and reacting to 80 degrees C for 2 hours to obtain polyurethane pre-polymer A; and (E) reacting with 1.2 g amino benzene sulfonic acid and 20 g acetone, reacting to 75 degrees C for 2 hours, adding 1 g 2,4,6-trihydroxybenzoic acid and 1.2 g (B), reacting to 85 degrees C for 0.5 hours, adding 12 g triethylamine, reacting for 30 minutes, adding 110 g water, and stirring to emulsify. The graphene is chemical vapor deposited to length of 0.1-10 mu m, width of 0.1-10 mu m, thickness of 1-10 nm, purity of 99.5 wt.% and specific surface area of 500-2600 m2/g.