耐热抗冲PVC复合材料的制备、结构与性能
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摘要
PVC树脂具有良好的综合性能,但耐热及抗冲击性能的不足大大限制了其应用。PVC的耐热改性往往导致材料的加工性能和力学性能劣化,而其增塑和抗冲改性提高了PVC材料韧性的同时,却牺牲了PVC材料的耐热性。如果将增塑剂分子通过化学反应或物理作用固定在无机粒子表面形成核-壳结构的粒子,将这种粒子与PVC复合,一方面可限制增塑剂的迁移,另一方面可提高无机粒子的分散性,可同时实现增塑、增强、增韧和提高耐热性的目的。本文采用类流体技术、插层镶嵌技术以及包覆交联技术制备出含增塑剂的具有核壳结构的高岭土粒子和碳酸钙粒子,用这两类核壳结构的无机粒子与PVC复合,制备出了高耐热抗冲PVC复合材料。
本论文的主要研究内容与结果如下：
(1)用3-(三甲氧基硅丙基)二甲基十八烷基氯化铵(DC5700)对高岭土进行表面修饰,用壬基酚聚氧乙烯醚硫酸钠(NPES)进行离子子交换,制备出高岭土类流体(SFKF)。用傅里叶红外光谱(FTIR)、 X射线衍射(XRD)、热重分析(TG)和透射电镜(TEM)分析了SFKF的结构,用电磁流变仪研究了SFKF的流变性能。结果发现所制备的SFKF表面接枝了43%的长链有机物,在加热至65℃时具有流动性,高岭土处于插层和部分剥离形态。
(2)用机械共混技术将SFKF与PVC复合,制备出PVC/SFKF复合材料。用转矩流变仪、紫外光谱(UV-vis)、扫面电镜(SEM)、动态粘弹谱仪(DMA)和万能力学试验机研究了PVC/SFKF复合体系的加工性能,PVC/SFKF复合材料的微观结构、动态粘弹行为和力学性能。结果发现,SFKF对PVC具有很强的增塑作用,可抑制加工过程中PVC的降解；SFKF在PVC基体中分散均匀,且与PVC基体的界面粘结提高,PVC/SFKF复合材料的缺口冲击强度(4.08kJ/m2)较纯PVC的缺口冲击强度(3.07kJ/m2)提高33%,Tg达到93.6℃。
(3)用一端富含腈基的液态高分子增塑剂(LMM-1)对高岭土进行表面插层镶嵌,制备了具有核-壳结构的高岭土(LKL)。用机械共混法将LKL与PVC进行熔融复合,制备出PVC/LKL复合材料。用转矩流变仪、UV-vis、SEM、DMA和万能力学试验机研究了PVC/LKL复合体系的加工性能,PVC/LKL复合材料的微观结构、动态粘弹行为和力学性能。结果表明,LKL对PVC具有较好的增塑作用,可抑制加工过程中PVC的降解；LMM-1插层镶嵌提高了LKL在PVC基体中的分散,LKL与PVC的界面粘结提高,PVC/LKL复合材料的缺口冲击强度(4.0kJ/m2)较纯PVC的缺口冲击强度(3.07kJ/m2)提高29%,Tg达到95.2℃,较纯PVC材料提高了6℃。
(4)用LMM-1对粒状碳酸钙表面进行包覆,制备出了具有核-壳结构的碳酸钙(LCC)。用机械共混法将LCC与PVC进行熔融复合,制备出PVC/LCC复合材料。用转矩流变仪、UV-vis、SEM、DMA和万能力学试验机研究了PVC/LCC复合体系的加工性能,PVC/LCC复合材料的微观结构、动态粘弹行为和力学性能。结果发现,LMM-1与碳酸钙一起对PVC具有很好的协同增塑作用,且可抑制加工过程中PVC的降解；LMM-1包覆改性提高了LCC在PVC基体中的分散,LCC与PVC的界面粘结提高,PVC/LCC复合材料的缺口冲击强度(4.95kJ/m2)较纯PVC的缺口冲击强度(3.07kJ/m2)提高59.7%,Tg达到93.0℃。
(5)用白度测试、UV-vis、SEM和万能力学试验机对添加碳酸钙及LCC的PVC材料紫外光老化实验后的结构和性能进行研究。结果表明,LCC作为紫外光屏蔽剂加入PVC基体,显著提高了体系的抗紫外老化性能。LMM-1对碳酸钙的包覆促进了其在PVC基体中的分散,LCC对紫外光的屏蔽效果较碳酸钙颗粒优异,经紫外光老化实验后的PVC/LCC复合材料表现出较PVC/CaCO3(PVC/CC)复合材料高的白度保持率和力学性能保持率。
(6)用一端富含双键的液态高分子改性剂(LMM-2)对碳酸钙进行包覆,同时添加交联剂对包覆于碳酸钙表面的LMM-2进行交联,制备出表面交联包覆的核-壳结构碳酸钙颗粒(CLCC)。用机械共混法将CLCC与PVC进行熔融复合,制备出PVC/CLCC复合材料。用转矩流变仪、UV-vis、白度测试、SEM、 DMA和万能力学试验机研究了PVC/CLCC复合体系的加工性能,PVC/CLCC复合材料的微观结构、动态粘弹行为和力学性能。结果发现,CLCC对PVC具有很好的增塑作用,可抑制加工过程中PVC的降解; CLCC显著提高了PVC材料的抗冲击性能和耐热性。当体系中CLCC颗粒含量达一最佳值时,交联的LMM-2在PVC基体中形成三维的网络状结构,复合材料的抗冲性能和耐热性达最佳,PVC/CLCC复合材料的缺口冲击强度(5.8kJ/m2)较纯PVC的缺口冲击强度(3.07kJ/m2)提高87.1%,Tg达到104.6℃,较纯PVC材料提高了15.4℃。
(7)用Pukanszky方程研究了碳酸钙包覆前后与PVC基体界面的相互作用,用Friedman方程和Kissinger方程对添加了LCC和CLCC的PVC材料的热降解机理和降解行为进行了研究。结果表明,LMM-1及LMM-2的加入,显著提高了碳酸钙颗粒与PVC基体间的界面作用；在降解第一阶段,PVC、PVC/LCC及PVC/CLCC复合材料的降解机理是一致的。LCC及CLCC的加入只是改变了PVC的热降解速度,并没有改变PVC的热降解机理。
Although the comprehensive performance of PVC resin is promising, the relatively low heat resistance and impact strength restrict its application. The attempts to promote the heat resistant property of PVC material usually deteriorate its processability and mechanical properties. The plasticization and toughening of PVC material can enhance the toughness, but meanwhile, sacrifice its heat resistant property. If the plasticizing molecules can be anchored on the surface of inorganic particles to form a core-shell structure and incorporated into the PVC matrix, their mobility in host material can be hampered and the dispensability of inorganic particles can be promoted. Additionally, such strategy can realize a simultaneous plasticizing, reinforcing and toughening, and enhance the heat resistance of PVC material. In this thesis, the kaolin and calcium carbonate particles with core-shell structure are prepared by liquid-like technique, intercalation inset technique and coating crosslink technique. These core-shell structured inorganic particles are mixed with PVC matrix to produce PVC/inorganic particle composites with high impact strength and heat resistance.
The main contents and results are listed as follows:
1. The dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride (DC5700) is used to modify the surface of kaolin. Then sodium nonylphenol polyoxyethylene ether sulfate (NPES) is used to achieve ion exchange reaction with kaolin organic ion salt to produce solvent-free kaolin fluid (SFKF). The Fourier Infrared Spectrometer analysis (FTIR), X-ray Diffraction (XRD), thermogravimetric analysis (TG) and transmission electron microscope (TEM) are used to analyze the structure of SFKF. The rheological property of SFKF is studied by electromagnetic rheometer. The results show that the surface of SFKF grafts43wt%long chain organic species. It can flow when the temperature achieves65℃, at which the kaolin particles are intercalated and partially exfoliated.
2. The PVC/SFKF composites are prepared by mechanically mixing SFKF with PVC materials. The processability, micro-structure, dynamic mechanical behavior and mechanical properties of PVC/SFKF composites are studied by using torque rheometer, ultraviolet-visible spectroscopy (UV-vis), scanning electron microscope (SEM), dynamic mechanical analysis (DMA) and universal mechanical testing machine, respectively. The results show that SFKF has fine plasticization effect on PVC materials, and restrains the decomposition of PVC materials during melting process. SFKF can uniformly disperse in PVC matrix, and the interface adhesion between kaolin and PVC matrix is enhanced. The notched impact strength of the PVC/SFKF composite achieves4.08kJ/m2, which is33%higher than that of neat PVC materials. The Tg of the PVC/SFKF composite is93.6℃, which is4.4℃higher than that of neat PVC materials.
3. The liquid macromolecular plasticizer (LMM-1) with nitrile end-group is used to intercalate kaolin on the surface, and thus the core-shell structured kaolin (LKL) is obtained. The PVC/LKL composites are prepared by melt blending LKL with PVC materials. The processability, micro-structure, dynamic mechanical behavior and mechanical properties of PVC/LKL composites are studied by employing torque rheometer, UV-vis, SEM, DMA and universal mechanical testing machine. The results show that LKL has good plasticization effect on PVC materials, and can restrain the decomposition of PVC materials during melting process. The intercalation of LMM-1can improve the dispersion of LKL in PVC matrix and the interface adhesion between LKL and PVC matrix is enhanced. The notched impact strength and Tg of the PVC/LKL composites achieve4.0kJ/m2and95.2℃, respectively, which are enhanced29%and6℃with respect to neat PVC materials.
4. The core-shell structured CaCCO3(LCC) particles are prepared by coating LMM-1on the surface of CaCO3particles. The PVC/LCC composites are also prepared through melt blending LCC with PVC materials. The processability, micro-structure, dynamic mechanical behavior and mechanical properties of PVC/LCC composites are studied by using torque rheometer, UV-vis, SEM, DMA and universal mechanical testing machine. The results show that LMM-1and CaCO3particles have good synergistic plasticization effect on PVC materials, and can restrain the decomposition of PVC materials during melting process. The dispersion of LCC in PVC matrix is improved when the CaCO3particles are modified by LMM-1. The notched impact strength of PVC/LCC composite incorporated with optimum amount of LCC particles is4.95kJ/m2, which is59.7%higher than that of neat PVC materials. The Tg of the composite is93.0℃, which is3.8℃higher than that of neat PVC materials.
5. The structure and properties of PVC material incorporated with CaCO3and LCC particles after UV aging are characterized using whiteness test, UV-vis, SEM and universal mechanical testing machine. The results show that LCC particles used as ultraviolet light screening agents can effectively improve the anti-aging properties of PVC matrix. Due to the coating of LMM-1on the surface of CaCO3particles, the compatibility between CaCO3particles and PVC matrix is significantly improved. The LCC particles can uniformly disperse in PVC matrix and effectively reflect ultraviolet light. Based on these premises, the LCC particles have better anti-aging properties than CaCO3particles for PVC matrix. The PVC/LCC composite has higher whiteness and mechanical property retention than PVC/CaCO3(PVC/CC) composite.
6. The liquid macromolecular plasticizer (LMM-2) with double bond end-groups is used to modify CaCO3particles, and then the crosslinking agent is added to crosslink the LMM-2. The core-shell structured CaCO3particles with crosslinked coating layer (CLCC) are obtained. The PVC/CLCC composites are also prepared through melt blending CLCC with PVC materials. The processability, micro-structure, dynamic mechanical behavior and mechanical properties of PVC/CLCC composites are studied by using torque rheometer, UV-vis, whiteness test, SEM, DMA and universal mechanical testing machine. The results show that CLCC has fine plasticization effect on PVC materials, and can restrain the decomposition of PVC materials during melting process. CLCC significantly enhances the toughness and heat resistance of PVC materials. When the CLCC content reaches an optimum value, the crosslinked LMM-2forms three-dimensional network structure in PVC matrix, and the notched impact strength and Tg of the composite achieve5.8kJ/m2and104.6℃, respectively, which are much higher than that of neat PVC materials.
7. The interface interaction between PVC matrix and CaCO3particles before and after modification is studied by using Pukanszky equation. The degradation mechanism and behavior of PVC/LCC and PVC/CLCC composites are investigated by using Friedman equation and Kissinger equation. The results show that the interface adhension between CaCO3particles and PVC matrix significantly enhances after the addition of LMM-1and LMM-2. The degradation mechanism of PVC, PVC/LCC and PVC/CLCC composites are consistent at the first stage of degradation. The addition of LCC and CLCC particles only changes the decomposition speed of PVC materials, but does not alter its degradation mechanism.
本论文的主要研究内容与结果如下：
(1)用3-(三甲氧基硅丙基)二甲基十八烷基氯化铵(DC5700)对高岭土进行表面修饰,用壬基酚聚氧乙烯醚硫酸钠(NPES)进行离子子交换,制备出高岭土类流体(SFKF)。用傅里叶红外光谱(FTIR)、 X射线衍射(XRD)、热重分析(TG)和透射电镜(TEM)分析了SFKF的结构,用电磁流变仪研究了SFKF的流变性能。结果发现所制备的SFKF表面接枝了43%的长链有机物,在加热至65℃时具有流动性,高岭土处于插层和部分剥离形态。
(2)用机械共混技术将SFKF与PVC复合,制备出PVC/SFKF复合材料。用转矩流变仪、紫外光谱(UV-vis)、扫面电镜(SEM)、动态粘弹谱仪(DMA)和万能力学试验机研究了PVC/SFKF复合体系的加工性能,PVC/SFKF复合材料的微观结构、动态粘弹行为和力学性能。结果发现,SFKF对PVC具有很强的增塑作用,可抑制加工过程中PVC的降解；SFKF在PVC基体中分散均匀,且与PVC基体的界面粘结提高,PVC/SFKF复合材料的缺口冲击强度(4.08kJ/m2)较纯PVC的缺口冲击强度(3.07kJ/m2)提高33%,Tg达到93.6℃。
(3)用一端富含腈基的液态高分子增塑剂(LMM-1)对高岭土进行表面插层镶嵌,制备了具有核-壳结构的高岭土(LKL)。用机械共混法将LKL与PVC进行熔融复合,制备出PVC/LKL复合材料。用转矩流变仪、UV-vis、SEM、DMA和万能力学试验机研究了PVC/LKL复合体系的加工性能,PVC/LKL复合材料的微观结构、动态粘弹行为和力学性能。结果表明,LKL对PVC具有较好的增塑作用,可抑制加工过程中PVC的降解；LMM-1插层镶嵌提高了LKL在PVC基体中的分散,LKL与PVC的界面粘结提高,PVC/LKL复合材料的缺口冲击强度(4.0kJ/m2)较纯PVC的缺口冲击强度(3.07kJ/m2)提高29%,Tg达到95.2℃,较纯PVC材料提高了6℃。
(4)用LMM-1对粒状碳酸钙表面进行包覆,制备出了具有核-壳结构的碳酸钙(LCC)。用机械共混法将LCC与PVC进行熔融复合,制备出PVC/LCC复合材料。用转矩流变仪、UV-vis、SEM、DMA和万能力学试验机研究了PVC/LCC复合体系的加工性能,PVC/LCC复合材料的微观结构、动态粘弹行为和力学性能。结果发现,LMM-1与碳酸钙一起对PVC具有很好的协同增塑作用,且可抑制加工过程中PVC的降解；LMM-1包覆改性提高了LCC在PVC基体中的分散,LCC与PVC的界面粘结提高,PVC/LCC复合材料的缺口冲击强度(4.95kJ/m2)较纯PVC的缺口冲击强度(3.07kJ/m2)提高59.7%,Tg达到93.0℃。
(5)用白度测试、UV-vis、SEM和万能力学试验机对添加碳酸钙及LCC的PVC材料紫外光老化实验后的结构和性能进行研究。结果表明,LCC作为紫外光屏蔽剂加入PVC基体,显著提高了体系的抗紫外老化性能。LMM-1对碳酸钙的包覆促进了其在PVC基体中的分散,LCC对紫外光的屏蔽效果较碳酸钙颗粒优异,经紫外光老化实验后的PVC/LCC复合材料表现出较PVC/CaCO3(PVC/CC)复合材料高的白度保持率和力学性能保持率。
(6)用一端富含双键的液态高分子改性剂(LMM-2)对碳酸钙进行包覆,同时添加交联剂对包覆于碳酸钙表面的LMM-2进行交联,制备出表面交联包覆的核-壳结构碳酸钙颗粒(CLCC)。用机械共混法将CLCC与PVC进行熔融复合,制备出PVC/CLCC复合材料。用转矩流变仪、UV-vis、白度测试、SEM、 DMA和万能力学试验机研究了PVC/CLCC复合体系的加工性能,PVC/CLCC复合材料的微观结构、动态粘弹行为和力学性能。结果发现,CLCC对PVC具有很好的增塑作用,可抑制加工过程中PVC的降解; CLCC显著提高了PVC材料的抗冲击性能和耐热性。当体系中CLCC颗粒含量达一最佳值时,交联的LMM-2在PVC基体中形成三维的网络状结构,复合材料的抗冲性能和耐热性达最佳,PVC/CLCC复合材料的缺口冲击强度(5.8kJ/m2)较纯PVC的缺口冲击强度(3.07kJ/m2)提高87.1%,Tg达到104.6℃,较纯PVC材料提高了15.4℃。
(7)用Pukanszky方程研究了碳酸钙包覆前后与PVC基体界面的相互作用,用Friedman方程和Kissinger方程对添加了LCC和CLCC的PVC材料的热降解机理和降解行为进行了研究。结果表明,LMM-1及LMM-2的加入,显著提高了碳酸钙颗粒与PVC基体间的界面作用；在降解第一阶段,PVC、PVC/LCC及PVC/CLCC复合材料的降解机理是一致的。LCC及CLCC的加入只是改变了PVC的热降解速度,并没有改变PVC的热降解机理。
Although the comprehensive performance of PVC resin is promising, the relatively low heat resistance and impact strength restrict its application. The attempts to promote the heat resistant property of PVC material usually deteriorate its processability and mechanical properties. The plasticization and toughening of PVC material can enhance the toughness, but meanwhile, sacrifice its heat resistant property. If the plasticizing molecules can be anchored on the surface of inorganic particles to form a core-shell structure and incorporated into the PVC matrix, their mobility in host material can be hampered and the dispensability of inorganic particles can be promoted. Additionally, such strategy can realize a simultaneous plasticizing, reinforcing and toughening, and enhance the heat resistance of PVC material. In this thesis, the kaolin and calcium carbonate particles with core-shell structure are prepared by liquid-like technique, intercalation inset technique and coating crosslink technique. These core-shell structured inorganic particles are mixed with PVC matrix to produce PVC/inorganic particle composites with high impact strength and heat resistance.
The main contents and results are listed as follows:
1. The dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride (DC5700) is used to modify the surface of kaolin. Then sodium nonylphenol polyoxyethylene ether sulfate (NPES) is used to achieve ion exchange reaction with kaolin organic ion salt to produce solvent-free kaolin fluid (SFKF). The Fourier Infrared Spectrometer analysis (FTIR), X-ray Diffraction (XRD), thermogravimetric analysis (TG) and transmission electron microscope (TEM) are used to analyze the structure of SFKF. The rheological property of SFKF is studied by electromagnetic rheometer. The results show that the surface of SFKF grafts43wt%long chain organic species. It can flow when the temperature achieves65℃, at which the kaolin particles are intercalated and partially exfoliated.
2. The PVC/SFKF composites are prepared by mechanically mixing SFKF with PVC materials. The processability, micro-structure, dynamic mechanical behavior and mechanical properties of PVC/SFKF composites are studied by using torque rheometer, ultraviolet-visible spectroscopy (UV-vis), scanning electron microscope (SEM), dynamic mechanical analysis (DMA) and universal mechanical testing machine, respectively. The results show that SFKF has fine plasticization effect on PVC materials, and restrains the decomposition of PVC materials during melting process. SFKF can uniformly disperse in PVC matrix, and the interface adhesion between kaolin and PVC matrix is enhanced. The notched impact strength of the PVC/SFKF composite achieves4.08kJ/m2, which is33%higher than that of neat PVC materials. The Tg of the PVC/SFKF composite is93.6℃, which is4.4℃higher than that of neat PVC materials.
3. The liquid macromolecular plasticizer (LMM-1) with nitrile end-group is used to intercalate kaolin on the surface, and thus the core-shell structured kaolin (LKL) is obtained. The PVC/LKL composites are prepared by melt blending LKL with PVC materials. The processability, micro-structure, dynamic mechanical behavior and mechanical properties of PVC/LKL composites are studied by employing torque rheometer, UV-vis, SEM, DMA and universal mechanical testing machine. The results show that LKL has good plasticization effect on PVC materials, and can restrain the decomposition of PVC materials during melting process. The intercalation of LMM-1can improve the dispersion of LKL in PVC matrix and the interface adhesion between LKL and PVC matrix is enhanced. The notched impact strength and Tg of the PVC/LKL composites achieve4.0kJ/m2and95.2℃, respectively, which are enhanced29%and6℃with respect to neat PVC materials.
4. The core-shell structured CaCCO3(LCC) particles are prepared by coating LMM-1on the surface of CaCO3particles. The PVC/LCC composites are also prepared through melt blending LCC with PVC materials. The processability, micro-structure, dynamic mechanical behavior and mechanical properties of PVC/LCC composites are studied by using torque rheometer, UV-vis, SEM, DMA and universal mechanical testing machine. The results show that LMM-1and CaCO3particles have good synergistic plasticization effect on PVC materials, and can restrain the decomposition of PVC materials during melting process. The dispersion of LCC in PVC matrix is improved when the CaCO3particles are modified by LMM-1. The notched impact strength of PVC/LCC composite incorporated with optimum amount of LCC particles is4.95kJ/m2, which is59.7%higher than that of neat PVC materials. The Tg of the composite is93.0℃, which is3.8℃higher than that of neat PVC materials.
5. The structure and properties of PVC material incorporated with CaCO3and LCC particles after UV aging are characterized using whiteness test, UV-vis, SEM and universal mechanical testing machine. The results show that LCC particles used as ultraviolet light screening agents can effectively improve the anti-aging properties of PVC matrix. Due to the coating of LMM-1on the surface of CaCO3particles, the compatibility between CaCO3particles and PVC matrix is significantly improved. The LCC particles can uniformly disperse in PVC matrix and effectively reflect ultraviolet light. Based on these premises, the LCC particles have better anti-aging properties than CaCO3particles for PVC matrix. The PVC/LCC composite has higher whiteness and mechanical property retention than PVC/CaCO3(PVC/CC) composite.
6. The liquid macromolecular plasticizer (LMM-2) with double bond end-groups is used to modify CaCO3particles, and then the crosslinking agent is added to crosslink the LMM-2. The core-shell structured CaCO3particles with crosslinked coating layer (CLCC) are obtained. The PVC/CLCC composites are also prepared through melt blending CLCC with PVC materials. The processability, micro-structure, dynamic mechanical behavior and mechanical properties of PVC/CLCC composites are studied by using torque rheometer, UV-vis, whiteness test, SEM, DMA and universal mechanical testing machine. The results show that CLCC has fine plasticization effect on PVC materials, and can restrain the decomposition of PVC materials during melting process. CLCC significantly enhances the toughness and heat resistance of PVC materials. When the CLCC content reaches an optimum value, the crosslinked LMM-2forms three-dimensional network structure in PVC matrix, and the notched impact strength and Tg of the composite achieve5.8kJ/m2and104.6℃, respectively, which are much higher than that of neat PVC materials.
7. The interface interaction between PVC matrix and CaCO3particles before and after modification is studied by using Pukanszky equation. The degradation mechanism and behavior of PVC/LCC and PVC/CLCC composites are investigated by using Friedman equation and Kissinger equation. The results show that the interface adhension between CaCO3particles and PVC matrix significantly enhances after the addition of LMM-1and LMM-2. The degradation mechanism of PVC, PVC/LCC and PVC/CLCC composites are consistent at the first stage of degradation. The addition of LCC and CLCC particles only changes the decomposition speed of PVC materials, but does not alter its degradation mechanism.
引文
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