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双子磷酸酯改性硼酸锌晶须及其在聚 乙烯中的阻燃增强研究
论文作者:童鞋论文网  论文来源:www.txlunwenw.com  发布时间:2019/10/26 13:28:26  

摘要:防水透汽膜是一种具有防水、透汽的功能型薄膜,通常存在易燃、易破损等不足,限制其广泛应用,目前对于阻燃型防水透汽膜的研究报道很少。防水透汽膜常用聚乙烯(PE)作为基质材料,主要是因为聚乙烯具有毒性低,电绝缘性好,机械性能优异,化学稳定性好,易加工成型等优点。但聚乙烯极限氧指数(LOI)仅为17.4%,非常易燃。因此,如何提高其阻燃性成为一大挑战。硼酸锌作为一种无卤阻燃剂,具有无毒、抑烟等优点,但硼酸锌微粒尺寸较大,在聚合物材料中容易团聚,分散性较差。纳米晶须可以在高分子材料中具有较好的分散性和补强性,在提高高聚物阻燃性的基础上,还能增加材料的机械强度;但是硼酸锌晶须是极性物质,填充在聚合物中时,存在相界面,需要对硼酸锌晶须进行表面改性,增加其在聚合物中的相容性。本论文以纳米硼酸锌晶须作为基质材料,采用自制的双子磷酸酯对其进行改性,利用改性后硼酸锌晶须的良好分散性和较低极性,将其与聚乙烯材料复合,制备成防水透汽膜,以期得到高效阻燃、高强度的防水透汽膜。

以六水合硝酸锌和硼酸为原料,采用水热合成工艺,通过简单可控的方法,成功制备出4ZnO•B2O3•H2O结构的纳米硼酸锌晶须。考察原料摩尔比,反应温度,反应时间和反应pH对晶须生长的影响,得出最佳的晶须生长工艺条件是在原料Zn(NO3)2•6H2O:H3BO3:NaOH的摩尔比为2:3:4、反应温度为240 °C、反应时间为22 h,反应pH在8~9,此时硼酸锌晶须具有良好的微观形貌以及最佳的长径比49。硼酸锌晶须的直径达到60~100 nm,长度为2~3 μm,长径比为20~50。

以三氯氧磷和乙二醇为原料,成功制备双子磷酸酯改性剂。将制备得到的双子磷酸酯改性剂用于硼酸锌晶须的改性。通过FT-IR、XRD、SEM、1H-NMR等表征手段得出,双子磷酸酯改性硼酸锌晶须是在硼酸锌的表面形成牢固化学键,但改性前后并未改变硼酸锌的晶体结构和晶须的微观形貌;通过水接触角、亲油化度值和活化指数表征改性效果,可以得出双子磷酸酯改性剂用量在1%时,硼酸锌晶须具有最佳的改性效果,此时硼酸锌晶须由亲水性向疏水性转变,水接触角达到159.8°,亲油化度值达到60.8%,活化度达到99.5%。

以改性后硼酸锌晶须和低密度聚乙烯为原料,制备复合材料,探究改性硼酸锌晶须对复合材料的阻燃增强效果,并与市售硼酸锌进行对比。结果表明,当改性硼酸锌晶须在聚乙烯中的添加量达到10%时,复合材料的拉伸强度和弯曲强度得到明显提升,拉伸强度达到19.1 N/mm2,弯曲强度达到10.9 N/mm2。当改性硼酸锌晶须添加量在50%时,复合材料氧指数达到27.6%,材料属于难燃级别,垂直燃烧等级达到V-1级别。之后将改性硼酸锌晶须、聚磷酸铵添加至聚乙烯中复配,制备防水透汽膜。结果表明硼酸锌晶须与聚磷酸铵的协同阻燃作用,有利于提升防水透汽膜的阻燃效果;由于硼酸锌晶须的存在,防水透汽膜的力学性能同时得到提升。当聚乙烯中聚磷酸铵和改性硼酸锌晶须的掺杂比例达到30%时,防水透汽膜的拉伸强度达到9.94 N/mm2,断裂伸长率达到270.01%。当聚乙烯中聚磷酸铵和改性硼酸锌晶须的掺杂比例达到50%时,防水透汽膜材料的极限氧指数达到29.4%,属于难燃级别,达到B1等级。防水透汽膜具有良好的的透汽性能,透汽性能可达到1813 g/(m2•24h)。

Vapor-permeable waterproofing membrane wasa functional membrane with waterproof and vapor permeability. Due to theflammability and damage of the vapor-permeable waterproofing membrane, it wasfurther limited to its wide application. At present, the research reported onthe flame retardant vapor-permeable waterproofing membrane was very less.Polyethylene (PE) was commonly used as a matrix material for vapor-permeablewaterproofing membrane. That was because polyethylene had the advantages of lowtoxicity, good electrical insulation, excellent mechanical properties, goodchemical stability, and easy processing. However, the limiting oxygen index(LOI) of polyethylene was only 17.4% and the polyethylene was very burned.Therefore, it became a major challenge on how to improve its flame retardancy.As a halogen-free flame retardant, zinc borate had the advantages ofnon-toxicity and smoke suppression. But the zinc borate particles were large insize. It was easy to agglomerate and had poor dispersibility in polymermaterials. Nanowhiskers had a good dispersibility and reinforcement in thepolymer material. It could increase the mechanical strength of the material onthe basis of improving the flame retardancy of the polymer. Zinc borate whiskerwas a polar substance. When it was added to the polymer, there was a phaseinterface. It was necessary to modify the surface of zinc borate whisker. Itcould increase its compatibility in the polymer. Zinc borate nanowhiskers wasused as matrix material in this paper. The self-made gemini phosphatesurfactant was used for the modification of zinc borate whiskers. The modifiedzinc borate nanowhiskers had good dispersibility and low polarity. Thevapor-permeable waterproofing membrane was synthesized by using zinc boratenanowhiskers and polyethylene as raw materials in order to obtainhigh-efficiency flame and high-strength vapor-permeable waterproofing membrane.

The zinc borate whiskers with 4ZnO•B2O3•H2Ostructure were synthesized by using zinc nitrate hexahydrate and boracic acidas raw materials with the hydrothermal synthesis process. The zinc borate wassynthesized by choosing four factors including the molar ratio of rawmaterials, reaction temperature, reaction time, and reaction pH. The bestwhisker growth process were obtained when the molar ratio of raw materialsZn(NO3)2•6H2O:H3BO3:NaOH was 2:3:4, the reaction temperature was 240 °C, thereaction time was 22 h, and the reaction pH was 8~9. At this time, the zincborate whiskers had good microscopic morphology and the best aspect ratio 49.The diameter of zinc borate whiskers was up to 60~100 nm, the length was 2~3μm, and the aspect ratio was 20~50.

The gemini phosphate surfactant wassynthesized by using phosphorus oxychloride and ethylene glycol as rawmaterials. The gemini phosphate surfactant was used for the modification ofzinc borate whiskers. The FT-IR, XRD, SEM and 1H-NMR characterization methodsshowed that the gemini phosphate modified zinc borate whiskers formed a strongchemical bond on the surface of zinc borate. But the crystal structure of zincborate and the microscopic morphology of whiskers were not changed withmodification. When the modification effect was characterized by water contactangle, lipophilicity value and activation index. It showed that the zinc boratewhisker had the best modification effect when the amount of the geminiphosphate surfactant was up to 1%. It had changed from hydrophilic tohydrophobic. The water contact angle reached 159.8 °. The lipophilicity valuereached 60.8%. The activation degree reached 99.5%.

The composite materials were synthesized byusing modified zinc borate whiskers and low-density polyethylene as rawmaterials. The modified zinc borate was used to explore the flame retardantenhancement effect in polyethylene materials. The effect of flame retardant wasalso compared with the commercial zinc borate.

关键词:硼酸锌晶须;双子磷酸酯;聚乙烯;阻燃;防水透汽膜

Zinc borate whiskers; Gemini phosphate;Polyethylene; Flame retardant; Vapor-permeable waterproofing membrane

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