硼酸根插層的Ca-A1LDHs的制備、改性與應用研究
發(fā)布時間:2019-04-12 11:45
【摘要】:水滑石、類水滑石和插層水滑石等統(tǒng)稱為水滑石類插層材料(LDHs)。目前有關Zn-Al-BO3-LDHs、Mg-Al-BO3-LDHs和Zn-Al-CO3-LDHs、Mg-Al-CO3-LDHs等LDHs的合成已有報道,并證明這些LDHs具有比較好的阻燃性。本文在前人研究工作的基礎上,首先以四水硝酸鈣、九水硝酸鋁、氫氧化鈉以及硼酸或硼砂為原料,探索適宜的合成方法和最佳的合成條件,合成硼酸根插層的Ca-Al-BO3-LDHs;其次使用表面改性劑和偶聯(lián)劑對硼酸根插層的Ca-Al-BO3-LDHs表面進行有機化修飾;最后將改性后的硼酸根插層的Ca-Al-BOs-LDHs添加到EVA中,測試不同填充量下的EVA復合材料的力學性能和燃燒氧指數(shù),考察硼酸根插層的Ca-Al-BO3-LDHs的阻燃效果。具體內容如下:(1)以四水硝酸鈣、九水硝酸鋁、氫氧化鈉以及硼酸或硼砂為原料,首先采用常用的共沉淀的方法,在室溫下將硼酸溶液和氫氧化鈉溶液同時滴加到四水硝酸鈣和六水硝酸鋁的混合鹽溶液中,然后將形成的乳白色漿液置于65℃的油浴中進行晶化,晶化時間控制為10h,晶化完成后再將該漿液在室溫下靜置13h。為探究該方法的最佳合成條件,又分別改變晶化溫度和晶化時間,并對不同反應條件下的產(chǎn)物進行了XRD和FT-IR表征。通過分析發(fā)現(xiàn)該方法雖能獲得硼酸根插層的Ca-Al-LDHs,但同時會有大量的副產(chǎn)物生成,并且獲得產(chǎn)物的晶相不是很好。為此改變合成方法,即采用離子交換法來合成硼酸根插層的Ca-Al-LDHs,通過對該法合成產(chǎn)物的FT-IR和XRD分析表征,發(fā)現(xiàn)利用該方法可以得到比較純凈的硼酸根插層的Ca-Al-LDHs,最終確定離子交換法為硼酸根插層的Ca-Al-LDHs的適宜合成方法。(2)以上述合成方法和合成條件合成的產(chǎn)物為原料,對其先用硬脂酸進行表面改性,再加入鈦酸酯偶聯(lián)劑對其進一步進行表面改性,提高其與高聚物分子的相容性;對改性產(chǎn)物進行XRD. FT-IR表征,懸浮性能和活化指數(shù)測試,當偶聯(lián)劑添加量為1%NDZ-311時,活化指數(shù)可達到97.86%。將改性粉體與EVA基體共混,獲得硼酸根插層Ca-Al-LDHs/EVA復合材料。對其進行力學性能和氧指數(shù)測試表明:當1%NDZ-311改性的硼酸根插層的Ca-Al-LDHs與EVA以2:5的比例共混,混合后的復合材料平均拉伸強度為9.68MPa,平均斷裂伸長率為663.3%;氧指數(shù)為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,
本文編號: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,
本文編號:2456982
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