硼酸根插层的Ca-A1LDHs的制备、改性与应用研究
发布时间：2019-04-12 11:45
【摘要】：水滑石、类水滑石和插层水滑石等统称为水滑石类插层材料(LDHs)。目前有关Zn-Al-BO3-LDHs、Mg-Al-BO3-LDHs和Zn-Al-CO3-LDHs、Mg-Al-CO3-LDHs等LDHs的合成已有报道,并证明这些LDHs具有比较好的阻燃性。本文在前人研究工作的基础上,首先以四水硝酸钙、九水硝酸铝、氢氧化钠以及硼酸或硼砂为原料,探索适宜的合成方法和最佳的合成条件,合成硼酸根插层的Ca-Al-BO3-LDHs;其次使用表面改性剂和偶联剂对硼酸根插层的Ca-Al-BO3-LDHs表面进行有机化修饰；最后将改性后的硼酸根插层的Ca-Al-BOs-LDHs添加到EVA中,测试不同填充量下的EVA复合材料的力学性能和燃烧氧指数,考察硼酸根插层的Ca-Al-BO3-LDHs的阻燃效果。具体内容如下：(1)以四水硝酸钙、九水硝酸铝、氢氧化钠以及硼酸或硼砂为原料,首先采用常用的共沉淀的方法,在室温下将硼酸溶液和氢氧化钠溶液同时滴加到四水硝酸钙和六水硝酸铝的混合盐溶液中,然后将形成的乳白色浆液置于65℃的油浴中进行晶化,晶化时间控制为10h,晶化完成后再将该浆液在室温下静置13h。为探究该方法的最佳合成条件,又分别改变晶化温度和晶化时间,并对不同反应条件下的产物进行了XRD和FT-IR表征。通过分析发现该方法虽能获得硼酸根插层的Ca-Al-LDHs,但同时会有大量的副产物生成,并且获得产物的晶相不是很好。为此改变合成方法,即采用离子交换法来合成硼酸根插层的Ca-Al-LDHs,通过对该法合成产物的FT-IR和XRD分析表征,发现利用该方法可以得到比较纯净的硼酸根插层的Ca-Al-LDHs,最终确定离子交换法为硼酸根插层的Ca-Al-LDHs的适宜合成方法。(2)以上述合成方法和合成条件合成的产物为原料,对其先用硬脂酸进行表面改性,再加入钛酸酯偶联剂对其进一步进行表面改性,提高其与高聚物分子的相容性；对改性产物进行XRD. FT-IR表征,悬浮性能和活化指数测试,当偶联剂添加量为1%NDZ-311时,活化指数可达到97.86%。将改性粉体与EVA基体共混,获得硼酸根插层Ca-Al-LDHs/EVA复合材料。对其进行力学性能和氧指数测试表明：当1%NDZ-311改性的硼酸根插层的Ca-Al-LDHs与EVA以2：5的比例共混,混合后的复合材料平均拉伸强度为9.68MPa,平均断裂伸长率为663.3%；氧指数为27.8%；
[Abstract]:Hydrotalcite, hydrotalcite-like and intercalated hydrotalcite are collectively known as hydrotalcite-like intercalation materials (LDHs). At present, the synthesis of LDHs such as Zn-Al-BO3-LDHs,Mg-Al-BO3-LDHs and Zn-Al-CO3-LDHs,Mg-Al-CO3-LDHs has been reported, and it has been proved that these LDHs have good flame retardancy. On the basis of previous research work, first of all, calcium nitrate tetrahydrate, aluminum nitrate nine water, sodium hydroxide, boric acid or borax as raw materials, to explore the appropriate synthesis method and the best synthetic conditions, Synthesis of borate intercalation Ca-Al-BO3-LDHs; Secondly, the surface of borate intercalated Ca-Al-BO3-LDHs was organically modified by surface modifier and coupling agent. At last, the modified borate intercalated Ca-Al-BOs-LDHs was added to EVA, and the mechanical properties and combustion oxygen index of EVA composites were tested under different fillings. The flame retardant effect of Ca-Al-BO3-LDHs intercalated with borate ions was investigated. The main contents are as follows: (1) using calcium nitrate tetrahydrate, aluminum nitrate nine water, sodium hydroxide and boric acid or borax as raw materials, the common coprecipitation method is adopted firstly. The boric acid solution and sodium hydroxide solution were added simultaneously to the mixed salt solution of calcium nitrate tetrahydrate and aluminum nitrate hexahydrate at room temperature, and then the milk white slurry was crystallized in oil bath at 65 鈩，
本文编号：2456982
[Abstract]:Hydrotalcite, hydrotalcite-like and intercalated hydrotalcite are collectively known as hydrotalcite-like intercalation materials (LDHs). At present, the synthesis of LDHs such as Zn-Al-BO3-LDHs,Mg-Al-BO3-LDHs and Zn-Al-CO3-LDHs,Mg-Al-CO3-LDHs has been reported, and it has been proved that these LDHs have good flame retardancy. On the basis of previous research work, first of all, calcium nitrate tetrahydrate, aluminum nitrate nine water, sodium hydroxide, boric acid or borax as raw materials, to explore the appropriate synthesis method and the best synthetic conditions, Synthesis of borate intercalation Ca-Al-BO3-LDHs; Secondly, the surface of borate intercalated Ca-Al-BO3-LDHs was organically modified by surface modifier and coupling agent. At last, the modified borate intercalated Ca-Al-BOs-LDHs was added to EVA, and the mechanical properties and combustion oxygen index of EVA composites were tested under different fillings. The flame retardant effect of Ca-Al-BO3-LDHs intercalated with borate ions was investigated. The main contents are as follows: (1) using calcium nitrate tetrahydrate, aluminum nitrate nine water, sodium hydroxide and boric acid or borax as raw materials, the common coprecipitation method is adopted firstly. The boric acid solution and sodium hydroxide solution were added simultaneously to the mixed salt solution of calcium nitrate tetrahydrate and aluminum nitrate hexahydrate at room temperature, and then the milk white slurry was crystallized in oil bath at 65 鈩，
本文编号：2456982
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