磷硅杂化与含磷壳聚糖阻燃剂的制备及其阻燃聚合物的性能和机理研究
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摘要
多糖类天然高分子材料具有来源广、价格低廉、可生物降解、可再生而且可替代化石资源、减少环境污染等优点,多年来得到了广泛的研究和应用。本文基于其含碳多羟基分子结构,开展了两个方面的研究。首先研究了广泛使用的传统多糖类天然高分子制品-棉纤维素织物的新型无卤阻燃方法,设计制备了含磷、硅的有机无机杂化阻燃剂,探讨其对于棉纤维织物的热稳定性、燃烧性能和阻燃性能的影响,以及无机协效剂对于棉纤维织物性能的影响。其次系统研究了一种多糖类天然高分子材料-壳聚糖的阻燃改性,将其作为反应起始物,引入磷或氮等阻燃元素或官能团,设计制备出多源一体的单组份天然高分子基阻燃剂,并将其应用于阻燃高聚物材料,研究了其热性能和燃烧性能,探讨了其阻燃机理。研究表明,杂化阻燃剂和含磷壳聚糖阻燃剂提高了材料高温区热稳定性,降低了其燃烧性能。具体研究工作内容如下：
1.采用含磷化合物9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和二氯代磷酸苯酯与硅烷偶联剂γ-氨丙基三乙氧基硅烷反应,合成出两种含磷硅氧烷单体DIA和PEA,使用溶胶凝胶法制备出两种含磷硅有机无机杂化阻燃剂。利用其分别对棉纤维织物进行阻燃整理,在其表面形成了杂化阻燃涂层。热重分析表明,杂化阻燃涂层可以提高织物在高温区的热稳定性,并使其成炭性能大幅度上升。热重红外联用分析结果表明,阻燃涂层的存在使得可燃的挥发性降解产物含量下降。燃烧性能结果表明,阻燃涂层可以使织物的热释放速率峰值下降,燃烧性能显著降低,而且织物的极限氧指数上升。以上研究表明含磷硅有机无机杂化阻燃剂可以提高棉纤维的阻燃性能
2.在上述研究的基础上将焦磷酸铁(FePP)作为阻燃协效剂引入阻燃体系,研究其对于阻燃棉纤维织物热性能和燃烧性能的影响。研究结果表明：FePP促进成炭,提高了样品在高温阶段(>300℃)的热稳定性。同时,FePP延缓了样品的热降解,推迟了热解产生的挥发性物质释放的时间。FePP的存在可以进一步降低样品的热释放速率峰值、总热释放量和热释放容量。
3.采用多糖类天然高分子壳聚糖为反应起始物,与五氧化二磷和三聚氰胺反应,合成了集酸源、炭源和气源于一体的天然高分子基膨胀型阻燃剂(MPCS),并将其应用于阻燃聚乙烯醇材料。热重分析数据表明MPCS可以提高聚乙烯醇的成炭量,提高了材料的热稳定性。材料热降解过程的研究结果表明MPCS执解脱氨,生成了不燃的挥发性产物-氨气,降低了环境气氛中的氧浓度,延缓了PVA的热氧化进程。同时,MPCS在升温降解的过程中生成了大量致密的含磷炭化层覆盖在材料表面。该炭化层可以作为物理阻隔层,不仅可以起到隔热隔氧的作用,同时还限制可燃的热解产物向材料表面迁移,从而延缓了材料的进一步热解与燃烧。燃烧性能研究表明MPCS降低了材料的热释放速率。
4.以壳聚糖与五氧化二磷及硝酸镍为原料制备出集阻燃和协效单元于一体的高效天然高分子基阻燃剂壳聚糖磷酸镍(NiPCS)。热重分析表明NiPCS在700℃的成炭量可以达到60.4wt%。燃烧性能研究表明,添加20wt%NiPCS后材料的总热释放速率降低40%。材料的热性能研究结果表明,NiPCS的加入提高了聚乙烯醇在高温阶段的热稳定性,增加了残炭量。NiPCS促进了材料在低温区的脱水作用,促进了含磷炭层的形成,同时降低了材料热解过程中产生的可燃性挥发性产物含量减少。对比含镍和不含镍阻燃剂处理聚乙烯醇后的数据可知,镍元素的存在延缓了材料的热降解,并使得材料中可燃性挥发产物的浓度进一步降低。
5.以甲基丙烯酸缩水甘油酯、壳聚糖和五氧化二磷为原料,合成了具有丙烯酸双键官能团的天然高分子基阻燃剂(GPCS)。并将其与环氧丙烯酸酯(EA)混合,通过紫外光固化,制备出紫外光固化阻燃材料(GPCS/EA)。燃烧性能研究表明,当添加20wt%的GPCS后,材料的最大热释放速率下降56%。热降解过程研究结果表明,材料中的磷氧官能团先降解生成了聚磷酸结构,催化环氧丙烯酸酯的降解、交联成炭。动态热机械性能分析表明低添加量下阻燃剂的增强作用显著,弥补了交联密度下降所带的负面影响；然而,伴随着GPCS含量的进一步增加,交联密度下降所带来的影响占据主导地位,导致储能模量下降。体系交联密度的下降和阻燃剂磷酸酯基团具有的良好柔韧性使得GPCS/EA材料的玻璃化温度下降。
How to reduce the human impact on the environment has been a focus around the world. Today, special attention has been paid on the natural polysaccharide materials, which is owning to their various merits, such as abundant yield and low cost. In this dissertation, we combined the natural polysaccharide materials with flame retardant technology. On one hand, the novel halogen free flame retardant, organic/inorganic hybrid flame retardant has been prepared to investigate its impact on thermal properties and flame retardancy of cotton fabrics. On the other hand, chitosan has been used to synthesize the novel natural resources based flame retardants and study their effect on thermal and combustible properites. The research work of this dissertation is composed of the following parts:
1. Two kinds of phosphorus modified siloxane (DIA and PEA) have been synthesized. Then the organic/inorganic hybrid flame retardant coatings were prepared with sol-gel method. They were applied on cellulose fabrics to investigate their effects on thermal properties and flame retardancy. Thermogravimetric analysis (TGA) showed that coatings can improve the thermal stability of cellulose fabrics in high temperature and enhance the residual char. Thermogravimetric analysis/infrared spectrometry (TGA-FTIR) data exhibited that organic/inorganic hybrid flame retardant coatings can reduce the flammable volatile degradation product. The combustion performance was examined by the microscale combustion calorimeter (MCC). Its resultes showed that the heat release rate decreased with the increase of the content of coatings. The result of LOI indicated that coatings improved the flame retardancy of cellulose fabircs.
2. Ferric pyrophosphate (FePP) was used as additive to study its synergistic effect of thermal degradation on cotton fabrics. MCC, TGA, TGA-IR, Real Time Fourier transform infrared spectroscopy (RT-FTIR) and Raman spectroscopy were utilized to evaluate the synergistic effects of FePP on DIA/cotton. TGA results showed that presence of FePP improved the thermal stability of materials after300℃. The MCC results revealed that FePP/DIA/cotton generated less combustion heat during heating than that of DIA/cotton. TGA-FTIR results showed that FePP can delay the thermal degradation process. RT-FTIR data revealed the mechanism of the influence of FePP, which can catalyze the break of the flame retardant as well as promote the char forming.
3. A novel nature material based flame retardant melamine chitosan phosphate (MPCS) has been prepared with chitosan, phosphorus pentoxide and melamine. Its impact on thermal properties and flammability performance of polyvinyl alcohol (PVA) was analyzed. Thermogravimetric analysis data exhibited that MPCS enhanced the thermal stability of materials at high temperature as well as the residual char at700℃. RT-FTIR revealed that MPCS promoted the thermal degradation of materials at a lower temperature and accelerated the char forming at high temperature. MCC was used to evaluate the combustion properties. The results showed that peak heat release rate (PHRR), total heat release (THR) and heat release capacity (HRC) all reduced.
4. Nickel chitosan phosphate (NiPCS) has been prepared, which was the combination of flame retardant and synergist. Its effect on thermal properties and flammability of PVA has been investigated. MCC test proved that NiPCS can decrease the PHRR and THR greatly. TGA results indicated that NiPCS possessed a high formation of char. With the increase of the flame retardant, the thermal stability of materials enhanced at high temperature. RT-FTIR data confirmed that the flame retardant can promoted the dehydration effect as well as accelerated the char forming. The volatilized products and the synergistic effect of nickel on thermal properties were both investigated with TGA-FTIR and laser Raman spectroscopy (LRS). The results revealed that nickel restained the thermal degradation of materials as well as improved the structural organization level of char.
5. Chitosan phosphate acrylate (GPCS) containing phosphorus and acrylate structure has been prepared. Its effect on flammability and thermal properties of epoxy acrylate (EA) has been investigated. MCC data showed that addition of20wt%GPCS reduced56%PHRR. Investigation of RT-FTIR and TGA-IR revealed that GPCS promoted the formation of char and reduced the release of combustible gas. Thermomechanical properties results showed that the storage modulus of samples increased then decreased with increasing GPCS content while the glass transition temperature showed the inverse trend.
1.采用含磷化合物9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和二氯代磷酸苯酯与硅烷偶联剂γ-氨丙基三乙氧基硅烷反应,合成出两种含磷硅氧烷单体DIA和PEA,使用溶胶凝胶法制备出两种含磷硅有机无机杂化阻燃剂。利用其分别对棉纤维织物进行阻燃整理,在其表面形成了杂化阻燃涂层。热重分析表明,杂化阻燃涂层可以提高织物在高温区的热稳定性,并使其成炭性能大幅度上升。热重红外联用分析结果表明,阻燃涂层的存在使得可燃的挥发性降解产物含量下降。燃烧性能结果表明,阻燃涂层可以使织物的热释放速率峰值下降,燃烧性能显著降低,而且织物的极限氧指数上升。以上研究表明含磷硅有机无机杂化阻燃剂可以提高棉纤维的阻燃性能
2.在上述研究的基础上将焦磷酸铁(FePP)作为阻燃协效剂引入阻燃体系,研究其对于阻燃棉纤维织物热性能和燃烧性能的影响。研究结果表明：FePP促进成炭,提高了样品在高温阶段(>300℃)的热稳定性。同时,FePP延缓了样品的热降解,推迟了热解产生的挥发性物质释放的时间。FePP的存在可以进一步降低样品的热释放速率峰值、总热释放量和热释放容量。
3.采用多糖类天然高分子壳聚糖为反应起始物,与五氧化二磷和三聚氰胺反应,合成了集酸源、炭源和气源于一体的天然高分子基膨胀型阻燃剂(MPCS),并将其应用于阻燃聚乙烯醇材料。热重分析数据表明MPCS可以提高聚乙烯醇的成炭量,提高了材料的热稳定性。材料热降解过程的研究结果表明MPCS执解脱氨,生成了不燃的挥发性产物-氨气,降低了环境气氛中的氧浓度,延缓了PVA的热氧化进程。同时,MPCS在升温降解的过程中生成了大量致密的含磷炭化层覆盖在材料表面。该炭化层可以作为物理阻隔层,不仅可以起到隔热隔氧的作用,同时还限制可燃的热解产物向材料表面迁移,从而延缓了材料的进一步热解与燃烧。燃烧性能研究表明MPCS降低了材料的热释放速率。
4.以壳聚糖与五氧化二磷及硝酸镍为原料制备出集阻燃和协效单元于一体的高效天然高分子基阻燃剂壳聚糖磷酸镍(NiPCS)。热重分析表明NiPCS在700℃的成炭量可以达到60.4wt%。燃烧性能研究表明,添加20wt%NiPCS后材料的总热释放速率降低40%。材料的热性能研究结果表明,NiPCS的加入提高了聚乙烯醇在高温阶段的热稳定性,增加了残炭量。NiPCS促进了材料在低温区的脱水作用,促进了含磷炭层的形成,同时降低了材料热解过程中产生的可燃性挥发性产物含量减少。对比含镍和不含镍阻燃剂处理聚乙烯醇后的数据可知,镍元素的存在延缓了材料的热降解,并使得材料中可燃性挥发产物的浓度进一步降低。
5.以甲基丙烯酸缩水甘油酯、壳聚糖和五氧化二磷为原料,合成了具有丙烯酸双键官能团的天然高分子基阻燃剂(GPCS)。并将其与环氧丙烯酸酯(EA)混合,通过紫外光固化,制备出紫外光固化阻燃材料(GPCS/EA)。燃烧性能研究表明,当添加20wt%的GPCS后,材料的最大热释放速率下降56%。热降解过程研究结果表明,材料中的磷氧官能团先降解生成了聚磷酸结构,催化环氧丙烯酸酯的降解、交联成炭。动态热机械性能分析表明低添加量下阻燃剂的增强作用显著,弥补了交联密度下降所带的负面影响；然而,伴随着GPCS含量的进一步增加,交联密度下降所带来的影响占据主导地位,导致储能模量下降。体系交联密度的下降和阻燃剂磷酸酯基团具有的良好柔韧性使得GPCS/EA材料的玻璃化温度下降。
How to reduce the human impact on the environment has been a focus around the world. Today, special attention has been paid on the natural polysaccharide materials, which is owning to their various merits, such as abundant yield and low cost. In this dissertation, we combined the natural polysaccharide materials with flame retardant technology. On one hand, the novel halogen free flame retardant, organic/inorganic hybrid flame retardant has been prepared to investigate its impact on thermal properties and flame retardancy of cotton fabrics. On the other hand, chitosan has been used to synthesize the novel natural resources based flame retardants and study their effect on thermal and combustible properites. The research work of this dissertation is composed of the following parts:
1. Two kinds of phosphorus modified siloxane (DIA and PEA) have been synthesized. Then the organic/inorganic hybrid flame retardant coatings were prepared with sol-gel method. They were applied on cellulose fabrics to investigate their effects on thermal properties and flame retardancy. Thermogravimetric analysis (TGA) showed that coatings can improve the thermal stability of cellulose fabrics in high temperature and enhance the residual char. Thermogravimetric analysis/infrared spectrometry (TGA-FTIR) data exhibited that organic/inorganic hybrid flame retardant coatings can reduce the flammable volatile degradation product. The combustion performance was examined by the microscale combustion calorimeter (MCC). Its resultes showed that the heat release rate decreased with the increase of the content of coatings. The result of LOI indicated that coatings improved the flame retardancy of cellulose fabircs.
2. Ferric pyrophosphate (FePP) was used as additive to study its synergistic effect of thermal degradation on cotton fabrics. MCC, TGA, TGA-IR, Real Time Fourier transform infrared spectroscopy (RT-FTIR) and Raman spectroscopy were utilized to evaluate the synergistic effects of FePP on DIA/cotton. TGA results showed that presence of FePP improved the thermal stability of materials after300℃. The MCC results revealed that FePP/DIA/cotton generated less combustion heat during heating than that of DIA/cotton. TGA-FTIR results showed that FePP can delay the thermal degradation process. RT-FTIR data revealed the mechanism of the influence of FePP, which can catalyze the break of the flame retardant as well as promote the char forming.
3. A novel nature material based flame retardant melamine chitosan phosphate (MPCS) has been prepared with chitosan, phosphorus pentoxide and melamine. Its impact on thermal properties and flammability performance of polyvinyl alcohol (PVA) was analyzed. Thermogravimetric analysis data exhibited that MPCS enhanced the thermal stability of materials at high temperature as well as the residual char at700℃. RT-FTIR revealed that MPCS promoted the thermal degradation of materials at a lower temperature and accelerated the char forming at high temperature. MCC was used to evaluate the combustion properties. The results showed that peak heat release rate (PHRR), total heat release (THR) and heat release capacity (HRC) all reduced.
4. Nickel chitosan phosphate (NiPCS) has been prepared, which was the combination of flame retardant and synergist. Its effect on thermal properties and flammability of PVA has been investigated. MCC test proved that NiPCS can decrease the PHRR and THR greatly. TGA results indicated that NiPCS possessed a high formation of char. With the increase of the flame retardant, the thermal stability of materials enhanced at high temperature. RT-FTIR data confirmed that the flame retardant can promoted the dehydration effect as well as accelerated the char forming. The volatilized products and the synergistic effect of nickel on thermal properties were both investigated with TGA-FTIR and laser Raman spectroscopy (LRS). The results revealed that nickel restained the thermal degradation of materials as well as improved the structural organization level of char.
5. Chitosan phosphate acrylate (GPCS) containing phosphorus and acrylate structure has been prepared. Its effect on flammability and thermal properties of epoxy acrylate (EA) has been investigated. MCC data showed that addition of20wt%GPCS reduced56%PHRR. Investigation of RT-FTIR and TGA-IR revealed that GPCS promoted the formation of char and reduced the release of combustible gas. Thermomechanical properties results showed that the storage modulus of samples increased then decreased with increasing GPCS content while the glass transition temperature showed the inverse trend.
引文
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