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申请号:201811071075.3 公开号:CN110903485A 主分类号:C08G79/04
申请人:【中文】天津科技大学【EN】Tianjin University of Science and Technology 申请日:2018.09.14 公开日:2020.03.24
摘要:【中文】本发明涉及一种高磷含量超支化氧化磷聚膦酸酯无卤阻燃剂及其制备方法,制备方法为:在氮气保护下,将定量的三氯氧磷和二羟基甲基氧化磷50℃‑90℃反应6‑10h,然后在100‑130℃进行减压反应0.5‑1.5h,冷却室温,经纯化处理,即可得到超支化氧化磷聚膦酸酯无卤阻燃剂。本高磷含量超支化氧化磷聚膦酸酯为聚合物,分子质量高、热稳定性能好,且磷含量高;本结构中还有大量的活性羟基官能团可以更好的与高分子材料相容,不易迁移;且能与高分子材料结合成为本体阻燃材料;适用范围广,适合用作皮革、环氧树脂、聚氨酯不饱和树脂等的阻燃剂,而且该产品的工艺流程简单,易于工业化,设备投资少,效益高。 【EN】The invention relates to a hyperbranched phosphorus oxide polyphosphonate halogen-free flame retardant with high phosphorus content and a preparation method thereof, wherein the preparation method comprises the following steps: reacting a certain amount of phosphorus oxychloride with dihydroxymethyl phosphorus oxide at 50-90 ℃ for 6-10h under the protection of nitrogen, then carrying out reduced pressure reaction at 100-130 ℃ for 0.5-1.5h, cooling to room temperature, and carrying out purification treatment to obtain the hyperbranched phosphorus oxide polyphosphonate halogen-free flame retardant. The hyperbranched phosphorus oxide polyphosphonate with high phosphorus content is a polymer, has high molecular quality, good thermal stability and high phosphorus content; a large number of active hydroxyl functional groups in the structure can be better compatible with high polymer materials and are not easy to migrate; and can be combined with high polymer materials to form a body flame retardant material; the flame retardant has wide application range, is suitable for being used as flame retardants of leather, epoxy resin, polyurethane unsaturated resin and the like, and has the advantages of simple process flow, easy industrialization, low equipment investment and high benefit.
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申请号:201811266085.2 公开号:CN111100166A 主分类号:C07F9/6574
申请人:【中文】天津科技大学【EN】Tianjin University of Science and Technology 申请日:2018.10.29 公开日:2020.05.05
摘要:【中文】本发明涉及一种高磷含量季鏻型磷酸酯三聚氰胺盐无卤阻燃剂及其制备方法,制备方法为:将定量的磷酸和二羟甲基甲基氧化磷100℃‑130℃反应2‑5h;然后在上述体系中加入定量的三聚氰胺,80‑100℃反应4‑6小时;经纯化处理后加入一定的四羟甲基硫化磷,调节至一定PH,70‑80℃反应1‑3小时,得到季鏻型磷酸酯三聚氰胺盐无卤阻燃剂。本高磷含量季鏻型磷酸酯三聚氰胺盐热稳定性好,且含磷氮量高;广泛适用于环氧树脂、皮革、不饱和树脂、聚丙烯等的阻燃剂;该结构还带有较多的活性官能团,与有机高分子材料结合性好,不易迁移;而且该阻燃剂为高含磷量的膨胀型阻燃剂,阻燃效率高。 【EN】The invention relates to a quaternary phosphonium type phosphate melamine salt halogen-free flame retardant with high phosphorus content and a preparation method thereof, wherein the preparation method comprises the following steps: reacting quantitative phosphoric acid with dimethylol methyl phosphorus oxide at 100-130 ℃ for 2-5 h; then adding quantitative melamine into the system, and reacting for 4-6 hours at 80-100 ℃; after purification treatment, certain tetrakis hydroxymethyl phosphonium sulfide is added, the pH is adjusted to a certain value, and the reaction is carried out for 1 to 3 hours at the temperature of between 70 and 80 ℃ to obtain the quaternary phosphonium type phosphate melamine salt halogen-free flame retardant. The quaternary phosphonium phosphate melamine salt with high phosphorus content has good thermal stability and high phosphorus and nitrogen content; widely applicable to flame retardants of epoxy resins, leather, unsaturated resins, polypropylene and the like; the structure also has more active functional groups, has good bonding property with organic polymer materials and is not easy to migrate; and the flame retardant is an intumescent flame retardant with high phosphorus content, and has high flame retardant efficiency.
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