聚合物/α-磷（膦）酸锆纳米复合材料的制备与结构性能研究
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摘要
α-磷酸锆(α-ZrP)是一种层状无机化合物,不仅在客体插入其层间后能保持稳定的层板,而且还具备离子交换容量大,长径比可有效控制,粒子尺寸分布较窄等优点,很适合应用于制备聚合物／层状无机纳米复合材料。但是,由于α-ZrP结晶度较高,层间距较小,很难在聚合物基体中均匀分散和剥离,本文对如何改善α-ZrP与高聚物基体间的相容性做了如下研究。
1.以溶胶-凝胶回流法合成层状化合物α-ZrP,然后采用正丁胺“层离-插层”的方法对其进行有机修饰。该有机化处理的α-ZrP与聚乙烯醇(PVA)共混制得PVA/α-ZrP纳米复合材料。通过对上述纳米复合材料进行微观结构和形貌表征及一系列性能测试,发现聚乙烯醇和α-ZrP分子间形成了很强的氢键作用,当PVA基体中含有0.8 wt%的α-ZrP时,复合材料的拉伸强度和断裂伸长率分别比纯PVA提高了17.3%,26.6%,热稳定性也显著增强。
2.通过改变反应物磷酸溶液的浓度,制备长径比及比表面积不同的α-ZrP。精确测定α-ZrP的长径比和比表面积大小,探究纳米α-ZrP表面形态及长径比对PVA诸多性能的影响。研究表明,随着α-ZrP长径比的增大,PVA/α-ZrP纳米复合膜的拉伸强度和断裂伸长率显著提高,但当其长径比过大时,对应的高比表面能导致α-ZrP在聚合物基体中的大量团聚,从而破坏了复合材料各方面的性能。
3.通过酸性高锰酸钾的氧化在淀粉的糖环上引入羧基,利用羧基强的电负性来增强氧化淀粉(OST)和聚乙烯醇之间的氢键作用力,改善它们的相容性。此外为了制备性能更加优良的淀粉基材料,本章实验中还用纳米层状磷酸锆(α-ZrP)与氧化淀粉和聚乙烯醇共混,改善复合膜的力学性能和阻水性能。结果表明POST-ZrPn系列复合膜的性能优于PST-ZrPn系列。在POST-ZrPn系列复合薄膜中,随着α-ZrP含量的增加,拉伸强度(σb)和断裂伸长率(εb)也逐渐增加,α-ZrP含量为1.5 wt%时,复合膜的σb和εb同时达到最大值15.1 MPa和53%,同时α-ZrP的加入也增强了复合膜的阻湿性能和热稳定性。
4.采用氟配法合成层状苯膦酸锆(ZrPP),经发烟硫酸磺化后,在ZrPP层间苯环上引入磺酸基团。通过负电荷基团(ZrPP中的磺酸基)和正电基团(壳聚糖的氨基)之间的静电作用增强磺化苯膦酸锆与壳聚糖之间的相互作用和相容性。研究发现随着纳米粒子ZrSP填充量的增加,壳聚糖的拉伸强度(σb)和断裂伸长率(εb)也逐渐增加。ZrSP含量为0.6 wt%时,σb和εb同时达到最大值64 MPa和56%,同时ZrSP的加入也改善了复合膜的阻湿性能和热稳定性。
α-zirconium phosphate (α-ZrP), Zr(HPO_4)_2 H_2O, is kind of layered inorganic, it will still keep its well-ordered structure when the guests are inserted into the interlayers. Because of its high ion-exchange capacity, tunnable aspect ratio and narrow size distribution,α-ZrP is suitable to prepare polymer/layered inorganic nanocomposites. However, higher crystallinity and aspect ratio corresponds to higher particle aggregations and bad dispersions. In order to improve the compatibility betweenα-ZrP and polymers, we have carried out the work as follows:
1. In this work,α-ZrP was prepareded and exfoliated by n-Butylamine at first. And then a series of nanocomposite films that consisted of PVA and layered e-α-ZrP were prepared by a solution casting method. The results from XRD and SEM indicated that the PVA and e-α-ZrP possess good miscibility, which results from hydrogen bonding. Compared to the pure PVA, the tensile strength and elongation at break of the nanocomposite films increased by 17.3%、26.6% respectively.
2. In this work, by controlling the concentration of phosphoric acid, three different aspect ratios crystalline a-ZrP have been prepared. The results indicated that higher concentration of phosphoric acid corresponded to higer crystallinity and aspect ratio ofα-ZrP. Based on the present study, higher aspect ratios can lead to significant improvements in tensile strength, elongation at break and heat distortion temperature, but overhigh aspect ratio would result in bad dispersions ofα-ZrP which can deteriorate the film properties.
3. By introducing the carboxyl on starch sugar-ring, the hydrogen bonding and electrostatic interaction between oxidized starch (OST) and PVA were enhanced. Two series of nanocomposite films (POST-ZrPn and PST-ZrPn) were prepared by a solution casting method. The results from FT-IR, XRD and SEM indicated that the films of POST-ZrPn possessed better miscibility than PST-ZrPn, which resulted in improvement in mechanical properties, thermal stability and water-resistivity. Tensile strength and elongation at break of of the PVA/OST nanocomposite films increased from 6.6 to 15.1 MPa,35% to 63% asα-ZrP content increased from 0 to 1.5 wt%. However, higher loading ofα-ZrP resulted in aggregations ofα-ZrP and theσ_b,ε_b deteriorated. The presence ofα-ZrP also decreased the moisture uptake and increased the degradation temperatures of the nanocomposites.
4. In this paper, zirconium sulphophenyl phosphonate (ZrSP) was synthesized in HF solution and characterized to prepare a series nanocomposites in which ZrSP was used as nanofiller. The results from FT-IR, SEM and XRD indicated that strong interaction between ZrSP and chitosan formed during the film-forming process, and the ZrSP could uniformly dispersed in chitosan matrix when ZrSP loading in the composites was less than 2 wt%. Additionally, because of the enhanced interfacial interaction between the fillers and matrix, the tensile strength, elongation at break, water resistance and thermal stability of the CS based nanocomposites were improved synchronously.
1.以溶胶-凝胶回流法合成层状化合物α-ZrP,然后采用正丁胺“层离-插层”的方法对其进行有机修饰。该有机化处理的α-ZrP与聚乙烯醇(PVA)共混制得PVA/α-ZrP纳米复合材料。通过对上述纳米复合材料进行微观结构和形貌表征及一系列性能测试,发现聚乙烯醇和α-ZrP分子间形成了很强的氢键作用,当PVA基体中含有0.8 wt%的α-ZrP时,复合材料的拉伸强度和断裂伸长率分别比纯PVA提高了17.3%,26.6%,热稳定性也显著增强。
2.通过改变反应物磷酸溶液的浓度,制备长径比及比表面积不同的α-ZrP。精确测定α-ZrP的长径比和比表面积大小,探究纳米α-ZrP表面形态及长径比对PVA诸多性能的影响。研究表明,随着α-ZrP长径比的增大,PVA/α-ZrP纳米复合膜的拉伸强度和断裂伸长率显著提高,但当其长径比过大时,对应的高比表面能导致α-ZrP在聚合物基体中的大量团聚,从而破坏了复合材料各方面的性能。
3.通过酸性高锰酸钾的氧化在淀粉的糖环上引入羧基,利用羧基强的电负性来增强氧化淀粉(OST)和聚乙烯醇之间的氢键作用力,改善它们的相容性。此外为了制备性能更加优良的淀粉基材料,本章实验中还用纳米层状磷酸锆(α-ZrP)与氧化淀粉和聚乙烯醇共混,改善复合膜的力学性能和阻水性能。结果表明POST-ZrPn系列复合膜的性能优于PST-ZrPn系列。在POST-ZrPn系列复合薄膜中,随着α-ZrP含量的增加,拉伸强度(σb)和断裂伸长率(εb)也逐渐增加,α-ZrP含量为1.5 wt%时,复合膜的σb和εb同时达到最大值15.1 MPa和53%,同时α-ZrP的加入也增强了复合膜的阻湿性能和热稳定性。
4.采用氟配法合成层状苯膦酸锆(ZrPP),经发烟硫酸磺化后,在ZrPP层间苯环上引入磺酸基团。通过负电荷基团(ZrPP中的磺酸基)和正电基团(壳聚糖的氨基)之间的静电作用增强磺化苯膦酸锆与壳聚糖之间的相互作用和相容性。研究发现随着纳米粒子ZrSP填充量的增加,壳聚糖的拉伸强度(σb)和断裂伸长率(εb)也逐渐增加。ZrSP含量为0.6 wt%时,σb和εb同时达到最大值64 MPa和56%,同时ZrSP的加入也改善了复合膜的阻湿性能和热稳定性。
α-zirconium phosphate (α-ZrP), Zr(HPO_4)_2 H_2O, is kind of layered inorganic, it will still keep its well-ordered structure when the guests are inserted into the interlayers. Because of its high ion-exchange capacity, tunnable aspect ratio and narrow size distribution,α-ZrP is suitable to prepare polymer/layered inorganic nanocomposites. However, higher crystallinity and aspect ratio corresponds to higher particle aggregations and bad dispersions. In order to improve the compatibility betweenα-ZrP and polymers, we have carried out the work as follows:
1. In this work,α-ZrP was prepareded and exfoliated by n-Butylamine at first. And then a series of nanocomposite films that consisted of PVA and layered e-α-ZrP were prepared by a solution casting method. The results from XRD and SEM indicated that the PVA and e-α-ZrP possess good miscibility, which results from hydrogen bonding. Compared to the pure PVA, the tensile strength and elongation at break of the nanocomposite films increased by 17.3%、26.6% respectively.
2. In this work, by controlling the concentration of phosphoric acid, three different aspect ratios crystalline a-ZrP have been prepared. The results indicated that higher concentration of phosphoric acid corresponded to higer crystallinity and aspect ratio ofα-ZrP. Based on the present study, higher aspect ratios can lead to significant improvements in tensile strength, elongation at break and heat distortion temperature, but overhigh aspect ratio would result in bad dispersions ofα-ZrP which can deteriorate the film properties.
3. By introducing the carboxyl on starch sugar-ring, the hydrogen bonding and electrostatic interaction between oxidized starch (OST) and PVA were enhanced. Two series of nanocomposite films (POST-ZrPn and PST-ZrPn) were prepared by a solution casting method. The results from FT-IR, XRD and SEM indicated that the films of POST-ZrPn possessed better miscibility than PST-ZrPn, which resulted in improvement in mechanical properties, thermal stability and water-resistivity. Tensile strength and elongation at break of of the PVA/OST nanocomposite films increased from 6.6 to 15.1 MPa,35% to 63% asα-ZrP content increased from 0 to 1.5 wt%. However, higher loading ofα-ZrP resulted in aggregations ofα-ZrP and theσ_b,ε_b deteriorated. The presence ofα-ZrP also decreased the moisture uptake and increased the degradation temperatures of the nanocomposites.
4. In this paper, zirconium sulphophenyl phosphonate (ZrSP) was synthesized in HF solution and characterized to prepare a series nanocomposites in which ZrSP was used as nanofiller. The results from FT-IR, SEM and XRD indicated that strong interaction between ZrSP and chitosan formed during the film-forming process, and the ZrSP could uniformly dispersed in chitosan matrix when ZrSP loading in the composites was less than 2 wt%. Additionally, because of the enhanced interfacial interaction between the fillers and matrix, the tensile strength, elongation at break, water resistance and thermal stability of the CS based nanocomposites were improved synchronously.
引文
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