碱木质素改性以及原竹纤维增强酚醛泡沫材料制备与性能研究
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摘要
随着地球上化石资源的枯竭，人们越来越重视可再生的生物质资源开发利用研究，利用可再生生物质资源完全或部分替代不可再生的矿物资源及其衍生产品制备新型轻质建材，促进了生物质资源高效利用，为生物质资源制备新型生物质基泡沫复合材料提供了一条新的途径，对高分子发泡材料可持续发展具有重大意义。本文利用碱木质素替代石化原料制备环保型酚醛树脂保温发泡材料，减少造纸废液对环境的污染；利用阻燃改性的原竹纤维增强酚醛泡沫，提高泡沫的力学性能，促进生物质资源高效利用；制备低毒性高性能酚醛泡沫复合材料；同时应用制备的泡沫复合材料开发新型轻质阻燃复合板材，为节能保温、轻质隔音建材等方面提供高性能、高安全性的新型材料。论文的主要研究内容和结论如下：
1.利用碱木质素酚羟基的特性替代部分苯酚，制备碱木质素替代10~40%苯酚量的可发性碱木质素-酚醛树脂，研究了碱木质素引入对树脂制备、结构和性能的影响。结果表明，碱木质素替代苯酚量≤30%的树脂黏度能够达到可发泡性树脂的要求，游离甲醛和苯酚残余量较低，树脂流体符合牛顿流体行为。TGA-DTG-DSC分析表明，随碱木质素替代苯酚量的增加，树脂的热稳定性和放热峰值呈下降趋势，而反应焓变也呈明显降低趋势。~(13)C-NMR核磁共振分析表明，酚醛树脂（PF）的酚核间连接方式基本以对-对位连接方式为主，而碱木质素替代苯酚量30%的树脂（KLPF-30）存在邻-对位和对-对位2种连接方式。通过KLPF-30树脂非等温DSC固化过程分析，建立了固化动力学模型，其中固化体系表观活化能为93.51kJ/mol，反应级数为0.9506。
2.分析了碱木质素改性对酚醛泡沫力学性能、热稳定性、阻燃性能及其微观结构的影响。结果表明，碱木质素替代苯酚量的增加导致泡沫的压缩强度、弯曲强度、表面粉化度等力学性能的下降，泡孔孔径增大、分布不均匀，但对酚醛泡沫的阻燃性和热稳定性影响较小。根据Gibson-Ashby经典模型建模和密度与力学性能数据的拟合2种方法,建立了碱木质素-酚醛泡沫表观密度-力学性能模型，其结果在密度0.030~0.300g/cm~3范围内基本相符，指数值在1.3941~1.7758范围内，基本接近于Gibson-Ashby公式中的指数。
3.采用硅烷偶联剂对原竹纤维进行表面改性，改善了其与酚醛泡沫和碱木质素-酚醛泡沫基体的界面相容性；采用改性原竹纤维增强酚醛泡沫和碱木质素-酚醛泡沫，研究了改性原竹纤维对泡沫材料结构、力学、阻燃性能的影响。在力学性能方面，改性原竹纤维的加入能够提高泡孔壁的韧性，对酚醛泡沫和碱木质素-酚醛泡沫的压缩强度、弯曲强度和表面粉化度都具有较明显的促进作用，改性原竹纤维增强酚醛泡沫和碱木质素-酚醛泡沫时加入量分别为3.0%和4%时增强效果最佳。阻燃性能的分析表明，随着原竹纤维加入量的增大，酚醛泡沫和碱木质素-酚醛泡沫的热释放速率、总放热量、质量损失速率、生烟速率（或烟释放速率）和总发烟量（或总烟释放量）等总体都呈上升趋势，说明原竹纤维的加入量降低2种泡沫的阻燃性能；且改性原竹纤维增强酚醛泡沫材料加入量≥5.0、改性原竹纤维增强碱木质素-酚醛泡沫的用量≥4.0%时，泡沫材料的阻燃性能有较大幅度的降低，需对改性原竹纤维进行阻燃改性。
4.原竹纤维和酚醛泡沫阻燃剂的筛选、评价及其机理研究的结果表明，原竹纤维的阻燃剂木材用磷-氮复合阻燃剂和磷酸二氢铵是磷系阻燃剂，最佳加入量均为15%。三聚氰胺吸热快速分解生成氨和大量氮气等不可燃气体是其对酚醛泡沫起到阻燃作用的关键，2%三聚氰胺阻燃改性酚醛泡沫的氧指数为67.8，比纯酚醛泡沫提高35.06%。通过正交试验确定阻燃工艺为磷酸二氢铵加入量15%、三聚氰胺加入量3%，制备的阻燃型原竹纤维增强碱木质素-酚醛泡沫的氧指数55.6，压缩强度、弯曲强度、掉渣率性能分别为92.99kPa、134.96kPa、7.99%。
5.采用锥形量热仪对碱木质素-酚醛泡沫（KLPF）、5%原竹纤维增强的碱木质素-酚醛泡沫（5B-KLPF）和阻燃改性的5%原竹纤维增强的碱木质素-酚醛泡沫（ZR-5B-KLPF）在热辐射通量为25、50和75kW/m2条件下的动态燃烧行为进行了对比分析，磷酸二氢铵和三聚氰胺对5B-KLPF泡沫的阻燃改性效果明显，显示出较高的成炭率，较低的热释放和烟释放。同时，基于CONE试验的聚合物材料燃烧的火势增长指数（FGI）、放热指数（THRI_(6min)）、发烟指数（TSPI_(6min)）、毒性气体生成速率指数（ToxPI_(6min)）4个特性指数，建立了聚合物材料火灾危险综合评价体系。KLPF、5B-KLPF和ZR-5B-KLPF3种泡沫的火灾危险综合指数IFHI对比表明ZR-5B-KLPF的火灾危险性最小。
6.利用原竹纤维、薄竹单板等短生长周期的可再生生物质资源制备了薄竹面改性原竹纤维增强酚醛泡沫夹芯复合板材。确定粘合剂为环氧AB胶、增强材料为天然麻纤维网格布，制备的薄竹面酚醛泡沫夹芯复合板材性能基本达到JC/T1051-2007“铝箔面硬质酚醛泡沫夹芯板”行业标准。确定薄竹单板的阻燃剂为木材用磷-氮复合阻燃剂，最佳载药率为3.80%，并采用锥形量热仪对制备的薄竹面原竹纤维增强酚醛泡沫夹芯复合板材的阻燃效果进行了对比分析。结果表明，阻燃剂对复合板材的阻燃效果非常明显，制备的泡沫夹芯复合板材具有高成炭率、低热释放和低烟释放的特点。同时论文还试制了多种泡沫夹芯复合板材。
With the growing shortage of crude oil resources, considerable research effort has beendevoted to developing new products using renewable biomass resources as raw materials.Using renewable resources and their derivative products to prepare new lightweight buildingmaterial instead of non-renewable mineral resources completely or partially, which couldpromote the efficient use of biomass resources, and provide a new way for the preparation ofnew biomass-based foam sandwich panels. It is of great significance to the sustainabledevelopment of foam material. Due to these reasons, the development of environmentallyfriendly foam sandwich materials has become a popular area of study in China and othercountries.
In this thesis, environmentally friendly PF foaming materials were prepared using alkalilignin to replace crude oil resources, which reduce the pollution of papermaking waste onenvironment. Reinforced phenolic foams by natural bamboo fiber were also prepared. Theaddition of bamboo fiber could improve the mechanical properties of foam and promote theefficient use of biomass resources. In addition, the reinforced PF foams were modified byflame-retardant modification of natural bamboo fiber and phenolic foam, which could bestowfoam materials with low toxicity and high performance. Meanwhile a new lightweightfire-retardant panel for energy-saving insulation and sound insulation were also prepared usingmodified PF foam compositing material as core materials to develop, lightweight buildingmaterials, damping materials, decoration and other aspects with high performance and highsafety. The main research contents and conclusions are as follows:
1. First, modified PF resins were prepared by utilizing alkali lignin as phenol’ssubstitution to prepare PF resin instead of phenol partially. Prepared alkali lignin-phenolicresin has a phenol substitution level in the range of10~40%. The effects of alkali lignin on thestructure, preparation and properties of the resin were studied in detail. When the formaldehydeto phenol (F/P) molar ratio is1.8and the substitution level of phenol less than30%, the viscosity of prepared resin could meet the demand of expandable resin, in this case the residualfree formaldehyde and phenol is very low. The analysis of rheological properties showed thatthe prepared resin possessed Newton fluid behavior when alkali lignin's substitution lever wasin the range of10%to30%. TGA-DTG-DSC analysis illustrated that thermal stability and theexothermic peak of the resin decreased with the increase of the substitution level of alkalilignin to phenol, and the reaction enthalpy also showed an obvious downtrend.13C-NMRanalysis suggested that connected mode between pure PF phenol internuclear connections waspara-position based, while in the resin with30%of alkali lignin substitution level (KLPF-30)there existed ortho-and and on-para two different linkages. DSC analysis showed that Theanalysis of non-isothermal DSC showed cured process of KLPF-30resin. The cure kineticmode was also established, the apparent activation energy of the curing system was93.51kJ/mol and the reaction order was0.9506.
2. By studying the influence of curing agent on mechanical properties, oxygen index andthermal stability of the phenolic foam, we took hydrochloric acid-phosphoric acid-organicacid-water mixed curing agent as the curing agent of PF foam and alkali lignin-phenolic foam.The effects of alkali lignin's substitution level on mechanical properties, thermal stability,flame retardant properties and microstructure of PF foam were analyzed. The analysis resultsshowed that compressive strength, flexural strength, foam powder surface salinity and othermechanical properties decreased with the increase of alkali lignin's substitution level, and thepore of foam material showed enlargement size and uneven distribution. While the flameretardant and thermal stability of phenolic foam showed changing tendency with the variationof alkali lignin content. The mathematical models of the density-mechanical properties of thealkali lignin-PF foam were established according to the classical Gibson-Ashby model and fitmodel of density and mechanical properties data, and the established model was basicallyconsistent with real testing data in the density range of0.030~0.300g/cm3, and the obtainedindex was close to the simplified Gibson-Ashby formula's index value in the range of1.3941~1.7758.
3. The compatibility between natural bamboo fiber and PF foams or alkalinelignin-phenolic foams was improved using silane coupling agent KH550as bamboo fiber'ssurface modification agent, and then the effect of modified bamboo fiber on the flame retardant,mechanical and the structure of modified compositing foams were studied. For theirmechanical properties, modified bamboo fiber improved the toughness of cell walls andincreased compression strength, flexural strength and surface powder degree of foams. Theoptimal addition of modified bamboo fiber for reinforced PF foam and alkali lignin-phenolicfoam was3%and4%, respectively. Smoke release characteristics and heat release rate of PFfoam and alkali lignin-phenolic foam modification with different addition amount of bamboofiber were measured by cone calorimeter. The analysis results displayed that the heat releaserate, total heat release, mass loss rate, smoke production rate (or smoke release rate) and thetotal amount of smoke (or total smoke release amount) of PF foam and alkali lignin-phenolicfoam showed uptrend with the increase in bamboo fiber content, which indicated that theaddition of bamboo fiber could reduce the flame retardant properties of PF foam and alkalilignin-phenolic foam. Especially when bamboo fiber content in PF foam is≥5%and in alkalinelignin-phenolic foam is≥4%, the flame retardant properties of foam materials had a greatreduction, so it is necessary to carry flame retardant modification for bamboo fiber.
4. The best fit flame retardant of nature bamboo fiber and PF foam was explored. Theanalysis results showed that N-P composed of flame retardant and ammonium dihydrogenphosphate (ADP) flame retardant was fitted for nature bamboo fiber. Two kinds of flameretardants are phosphorus flame retardant and their retardant mechanism were consistent, andthe optimum addition amount was15%. The mechanism of flame retardant of melamine wasthat rapid decomposition of ammonia and nitrogen that are not combustible gas and theseplayed the key role for PF foam's flame retardant property. Oxygen index of2%melamineflame retardant modified PF foam was67.8, which was over35.06%than that of PF foam.Orthogonal testing analysis showed the optimal flame retardant for nature bamboo fiber is ADPand optimal content was15%, the optimal flame retardant for alkali lignin-phenolic foam agentwas melamine and optimal content was3%. Oxygen index of lignin-phenolic foam reinforced by flame retardant nature bamboo fiber could reach55.6. The compressive strength, bendingstrength and dregs rate of lignin-phenolic foam were92.99kPa,134.96kPa and7.99%,respectively.
5. The combustion characteristics of alkali lignin-phenolic foam (KLPF),5%naturebamboo fiber reinforced alkali lignin-phenolic foam (5B-KLPF) and5%flame retardantmodified bamboo fiber reinforced alkali lignin-phenolic foam (ZR-5B-KLPF), were analyzedby using the cone calorimeter under the condition of thermal radiation flux at25,50and75kW/m2. Flame retardant ADP and melamine had obvious effect on modifying5B-KLPFfoam, and5B-KLPF foam had a high char yield, low heat release and smoke release.Meanwhile, the fire risk comprehensive evaluation system of polymer material was establishedby analyzing the data of fire growth index (FGI), heat index (THRI_(6min)), smoking index(TSPI_(6min)), toxic gas generation rate index (ToxPI_(6min)) via CONE test, the fire dangerindex-IFHI of these3kinds of foams showed that ZR-5B-KLPF had the minimum fire hazard.The mechanical and flame retardant properties of alkali lignin-phenolic foam had promoted toobtain a certain degree of promotion via flame retardant modification and nature bamboo fiberreinforced.
6. The reinforced PF foam sandwich panels were manufactured using renewable bamboofiber, sliced bamboo veneer and bamboo lamina as raw materials. The nature bamboo fiberreinforced PF foam sandwich panel was prepared with epoxy adhesive and natural hemp's fibermesh fabrics. The properties of the sandwich panels reinforced by natural hemp's fibers meshfabrics could closely meet the demands of industry standard (JC/T1051–2007)"Aluminum foilfaced rigid phenolic foam sandwich panels". In order to improve the mechanical properties andprocessability of sandwich panels, alkali lignin-phenolic sandwich panels was prepared byusing bamboo lamina existed in market as raw material. N-P compositing flame retardant andADP flame retardant were much fitted for sliced bamboo veneer and bamboo lamina, and theoptimal retention rate was3.80%and3.58%, respectively. A comparative analysis of flameretardant properties of natural bamboo fiber reinforced sliced bamboo veneer PF foamsandwich panels and natural bamboo fiber reinforced bamboo lamina alkaline lignin-phenolic foam sandwich panels were studied by using the cone calorimeter. The results showed thatthese2kinds of flame retardants had obvious effect on each composite plate. The preparedfoam sandwich panels had high char yield, low heat release and smoke release. Meanwhile, avariety of foam sandwich panels were also trial-manufactured.
1.利用碱木质素酚羟基的特性替代部分苯酚，制备碱木质素替代10~40%苯酚量的可发性碱木质素-酚醛树脂，研究了碱木质素引入对树脂制备、结构和性能的影响。结果表明，碱木质素替代苯酚量≤30%的树脂黏度能够达到可发泡性树脂的要求，游离甲醛和苯酚残余量较低，树脂流体符合牛顿流体行为。TGA-DTG-DSC分析表明，随碱木质素替代苯酚量的增加，树脂的热稳定性和放热峰值呈下降趋势，而反应焓变也呈明显降低趋势。~(13)C-NMR核磁共振分析表明，酚醛树脂（PF）的酚核间连接方式基本以对-对位连接方式为主，而碱木质素替代苯酚量30%的树脂（KLPF-30）存在邻-对位和对-对位2种连接方式。通过KLPF-30树脂非等温DSC固化过程分析，建立了固化动力学模型，其中固化体系表观活化能为93.51kJ/mol，反应级数为0.9506。
2.分析了碱木质素改性对酚醛泡沫力学性能、热稳定性、阻燃性能及其微观结构的影响。结果表明，碱木质素替代苯酚量的增加导致泡沫的压缩强度、弯曲强度、表面粉化度等力学性能的下降，泡孔孔径增大、分布不均匀，但对酚醛泡沫的阻燃性和热稳定性影响较小。根据Gibson-Ashby经典模型建模和密度与力学性能数据的拟合2种方法,建立了碱木质素-酚醛泡沫表观密度-力学性能模型，其结果在密度0.030~0.300g/cm~3范围内基本相符，指数值在1.3941~1.7758范围内，基本接近于Gibson-Ashby公式中的指数。
3.采用硅烷偶联剂对原竹纤维进行表面改性，改善了其与酚醛泡沫和碱木质素-酚醛泡沫基体的界面相容性；采用改性原竹纤维增强酚醛泡沫和碱木质素-酚醛泡沫，研究了改性原竹纤维对泡沫材料结构、力学、阻燃性能的影响。在力学性能方面，改性原竹纤维的加入能够提高泡孔壁的韧性，对酚醛泡沫和碱木质素-酚醛泡沫的压缩强度、弯曲强度和表面粉化度都具有较明显的促进作用，改性原竹纤维增强酚醛泡沫和碱木质素-酚醛泡沫时加入量分别为3.0%和4%时增强效果最佳。阻燃性能的分析表明，随着原竹纤维加入量的增大，酚醛泡沫和碱木质素-酚醛泡沫的热释放速率、总放热量、质量损失速率、生烟速率（或烟释放速率）和总发烟量（或总烟释放量）等总体都呈上升趋势，说明原竹纤维的加入量降低2种泡沫的阻燃性能；且改性原竹纤维增强酚醛泡沫材料加入量≥5.0、改性原竹纤维增强碱木质素-酚醛泡沫的用量≥4.0%时，泡沫材料的阻燃性能有较大幅度的降低，需对改性原竹纤维进行阻燃改性。
4.原竹纤维和酚醛泡沫阻燃剂的筛选、评价及其机理研究的结果表明，原竹纤维的阻燃剂木材用磷-氮复合阻燃剂和磷酸二氢铵是磷系阻燃剂，最佳加入量均为15%。三聚氰胺吸热快速分解生成氨和大量氮气等不可燃气体是其对酚醛泡沫起到阻燃作用的关键，2%三聚氰胺阻燃改性酚醛泡沫的氧指数为67.8，比纯酚醛泡沫提高35.06%。通过正交试验确定阻燃工艺为磷酸二氢铵加入量15%、三聚氰胺加入量3%，制备的阻燃型原竹纤维增强碱木质素-酚醛泡沫的氧指数55.6，压缩强度、弯曲强度、掉渣率性能分别为92.99kPa、134.96kPa、7.99%。
5.采用锥形量热仪对碱木质素-酚醛泡沫（KLPF）、5%原竹纤维增强的碱木质素-酚醛泡沫（5B-KLPF）和阻燃改性的5%原竹纤维增强的碱木质素-酚醛泡沫（ZR-5B-KLPF）在热辐射通量为25、50和75kW/m2条件下的动态燃烧行为进行了对比分析，磷酸二氢铵和三聚氰胺对5B-KLPF泡沫的阻燃改性效果明显，显示出较高的成炭率，较低的热释放和烟释放。同时，基于CONE试验的聚合物材料燃烧的火势增长指数（FGI）、放热指数（THRI_(6min)）、发烟指数（TSPI_(6min)）、毒性气体生成速率指数（ToxPI_(6min)）4个特性指数，建立了聚合物材料火灾危险综合评价体系。KLPF、5B-KLPF和ZR-5B-KLPF3种泡沫的火灾危险综合指数IFHI对比表明ZR-5B-KLPF的火灾危险性最小。
6.利用原竹纤维、薄竹单板等短生长周期的可再生生物质资源制备了薄竹面改性原竹纤维增强酚醛泡沫夹芯复合板材。确定粘合剂为环氧AB胶、增强材料为天然麻纤维网格布，制备的薄竹面酚醛泡沫夹芯复合板材性能基本达到JC/T1051-2007“铝箔面硬质酚醛泡沫夹芯板”行业标准。确定薄竹单板的阻燃剂为木材用磷-氮复合阻燃剂，最佳载药率为3.80%，并采用锥形量热仪对制备的薄竹面原竹纤维增强酚醛泡沫夹芯复合板材的阻燃效果进行了对比分析。结果表明，阻燃剂对复合板材的阻燃效果非常明显，制备的泡沫夹芯复合板材具有高成炭率、低热释放和低烟释放的特点。同时论文还试制了多种泡沫夹芯复合板材。
With the growing shortage of crude oil resources, considerable research effort has beendevoted to developing new products using renewable biomass resources as raw materials.Using renewable resources and their derivative products to prepare new lightweight buildingmaterial instead of non-renewable mineral resources completely or partially, which couldpromote the efficient use of biomass resources, and provide a new way for the preparation ofnew biomass-based foam sandwich panels. It is of great significance to the sustainabledevelopment of foam material. Due to these reasons, the development of environmentallyfriendly foam sandwich materials has become a popular area of study in China and othercountries.
In this thesis, environmentally friendly PF foaming materials were prepared using alkalilignin to replace crude oil resources, which reduce the pollution of papermaking waste onenvironment. Reinforced phenolic foams by natural bamboo fiber were also prepared. Theaddition of bamboo fiber could improve the mechanical properties of foam and promote theefficient use of biomass resources. In addition, the reinforced PF foams were modified byflame-retardant modification of natural bamboo fiber and phenolic foam, which could bestowfoam materials with low toxicity and high performance. Meanwhile a new lightweightfire-retardant panel for energy-saving insulation and sound insulation were also prepared usingmodified PF foam compositing material as core materials to develop, lightweight buildingmaterials, damping materials, decoration and other aspects with high performance and highsafety. The main research contents and conclusions are as follows:
1. First, modified PF resins were prepared by utilizing alkali lignin as phenol’ssubstitution to prepare PF resin instead of phenol partially. Prepared alkali lignin-phenolicresin has a phenol substitution level in the range of10~40%. The effects of alkali lignin on thestructure, preparation and properties of the resin were studied in detail. When the formaldehydeto phenol (F/P) molar ratio is1.8and the substitution level of phenol less than30%, the viscosity of prepared resin could meet the demand of expandable resin, in this case the residualfree formaldehyde and phenol is very low. The analysis of rheological properties showed thatthe prepared resin possessed Newton fluid behavior when alkali lignin's substitution lever wasin the range of10%to30%. TGA-DTG-DSC analysis illustrated that thermal stability and theexothermic peak of the resin decreased with the increase of the substitution level of alkalilignin to phenol, and the reaction enthalpy also showed an obvious downtrend.13C-NMRanalysis suggested that connected mode between pure PF phenol internuclear connections waspara-position based, while in the resin with30%of alkali lignin substitution level (KLPF-30)there existed ortho-and and on-para two different linkages. DSC analysis showed that Theanalysis of non-isothermal DSC showed cured process of KLPF-30resin. The cure kineticmode was also established, the apparent activation energy of the curing system was93.51kJ/mol and the reaction order was0.9506.
2. By studying the influence of curing agent on mechanical properties, oxygen index andthermal stability of the phenolic foam, we took hydrochloric acid-phosphoric acid-organicacid-water mixed curing agent as the curing agent of PF foam and alkali lignin-phenolic foam.The effects of alkali lignin's substitution level on mechanical properties, thermal stability,flame retardant properties and microstructure of PF foam were analyzed. The analysis resultsshowed that compressive strength, flexural strength, foam powder surface salinity and othermechanical properties decreased with the increase of alkali lignin's substitution level, and thepore of foam material showed enlargement size and uneven distribution. While the flameretardant and thermal stability of phenolic foam showed changing tendency with the variationof alkali lignin content. The mathematical models of the density-mechanical properties of thealkali lignin-PF foam were established according to the classical Gibson-Ashby model and fitmodel of density and mechanical properties data, and the established model was basicallyconsistent with real testing data in the density range of0.030~0.300g/cm3, and the obtainedindex was close to the simplified Gibson-Ashby formula's index value in the range of1.3941~1.7758.
3. The compatibility between natural bamboo fiber and PF foams or alkalinelignin-phenolic foams was improved using silane coupling agent KH550as bamboo fiber'ssurface modification agent, and then the effect of modified bamboo fiber on the flame retardant,mechanical and the structure of modified compositing foams were studied. For theirmechanical properties, modified bamboo fiber improved the toughness of cell walls andincreased compression strength, flexural strength and surface powder degree of foams. Theoptimal addition of modified bamboo fiber for reinforced PF foam and alkali lignin-phenolicfoam was3%and4%, respectively. Smoke release characteristics and heat release rate of PFfoam and alkali lignin-phenolic foam modification with different addition amount of bamboofiber were measured by cone calorimeter. The analysis results displayed that the heat releaserate, total heat release, mass loss rate, smoke production rate (or smoke release rate) and thetotal amount of smoke (or total smoke release amount) of PF foam and alkali lignin-phenolicfoam showed uptrend with the increase in bamboo fiber content, which indicated that theaddition of bamboo fiber could reduce the flame retardant properties of PF foam and alkalilignin-phenolic foam. Especially when bamboo fiber content in PF foam is≥5%and in alkalinelignin-phenolic foam is≥4%, the flame retardant properties of foam materials had a greatreduction, so it is necessary to carry flame retardant modification for bamboo fiber.
4. The best fit flame retardant of nature bamboo fiber and PF foam was explored. Theanalysis results showed that N-P composed of flame retardant and ammonium dihydrogenphosphate (ADP) flame retardant was fitted for nature bamboo fiber. Two kinds of flameretardants are phosphorus flame retardant and their retardant mechanism were consistent, andthe optimum addition amount was15%. The mechanism of flame retardant of melamine wasthat rapid decomposition of ammonia and nitrogen that are not combustible gas and theseplayed the key role for PF foam's flame retardant property. Oxygen index of2%melamineflame retardant modified PF foam was67.8, which was over35.06%than that of PF foam.Orthogonal testing analysis showed the optimal flame retardant for nature bamboo fiber is ADPand optimal content was15%, the optimal flame retardant for alkali lignin-phenolic foam agentwas melamine and optimal content was3%. Oxygen index of lignin-phenolic foam reinforced by flame retardant nature bamboo fiber could reach55.6. The compressive strength, bendingstrength and dregs rate of lignin-phenolic foam were92.99kPa,134.96kPa and7.99%,respectively.
5. The combustion characteristics of alkali lignin-phenolic foam (KLPF),5%naturebamboo fiber reinforced alkali lignin-phenolic foam (5B-KLPF) and5%flame retardantmodified bamboo fiber reinforced alkali lignin-phenolic foam (ZR-5B-KLPF), were analyzedby using the cone calorimeter under the condition of thermal radiation flux at25,50and75kW/m2. Flame retardant ADP and melamine had obvious effect on modifying5B-KLPFfoam, and5B-KLPF foam had a high char yield, low heat release and smoke release.Meanwhile, the fire risk comprehensive evaluation system of polymer material was establishedby analyzing the data of fire growth index (FGI), heat index (THRI_(6min)), smoking index(TSPI_(6min)), toxic gas generation rate index (ToxPI_(6min)) via CONE test, the fire dangerindex-IFHI of these3kinds of foams showed that ZR-5B-KLPF had the minimum fire hazard.The mechanical and flame retardant properties of alkali lignin-phenolic foam had promoted toobtain a certain degree of promotion via flame retardant modification and nature bamboo fiberreinforced.
6. The reinforced PF foam sandwich panels were manufactured using renewable bamboofiber, sliced bamboo veneer and bamboo lamina as raw materials. The nature bamboo fiberreinforced PF foam sandwich panel was prepared with epoxy adhesive and natural hemp's fibermesh fabrics. The properties of the sandwich panels reinforced by natural hemp's fibers meshfabrics could closely meet the demands of industry standard (JC/T1051–2007)"Aluminum foilfaced rigid phenolic foam sandwich panels". In order to improve the mechanical properties andprocessability of sandwich panels, alkali lignin-phenolic sandwich panels was prepared byusing bamboo lamina existed in market as raw material. N-P compositing flame retardant andADP flame retardant were much fitted for sliced bamboo veneer and bamboo lamina, and theoptimal retention rate was3.80%and3.58%, respectively. A comparative analysis of flameretardant properties of natural bamboo fiber reinforced sliced bamboo veneer PF foamsandwich panels and natural bamboo fiber reinforced bamboo lamina alkaline lignin-phenolic foam sandwich panels were studied by using the cone calorimeter. The results showed thatthese2kinds of flame retardants had obvious effect on each composite plate. The preparedfoam sandwich panels had high char yield, low heat release and smoke release. Meanwhile, avariety of foam sandwich panels were also trial-manufactured.
引文
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