GAP基含能热塑性弹性体研究
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摘要
传统硝化纤维素粘结剂能量高但受热、机械、冲击波、射流等刺激易发生燃烧转爆轰,降低武器装备的生存能力。发射药用惰性热塑性弹性体粘结剂虽具有良好的力学性能但能量低,聚叠氮缩水甘油醚(GAP)是侧链带叠氮基的新型含能粘结剂,兼具高能量和低敏感性特点,是发展新一代发射药的关键组份之一。GAP预聚物虽具有较高的能量但其强极性的叠氮侧链,使主链柔软性恶化,力学性能变差。本文借鉴惰性热塑性聚氨酯弹性体的设计、合成方法,针对发射药用粘结剂高能量、高强度要求,结合共混技术,开展了发射药用含能热塑性弹性体的设计、合成工艺及力学性能研究,获得了未见文献报道的DEG扩链GAP-TPE和硝化棉(NC)/GAP-TPE共混物,为发展高能量、高强度发射药提供粘结剂方面的理论和应用基础,并研究了GAP-TPE与NC/GAP-TPE共混物的热分解动力学,为评估高分子材料的热稳定性和预测材料的使用寿命提供依据。主要开展以下几方面工作：
通过对含能热塑性弹性体(ETPE)结构分析和分子设计,选择相对分子质量为3000的GAP为软段,MDI和BDO为硬段,合成了一类GAP-TPE,对合成工艺进行了研究,当采用预聚体法,R值为0.98,预聚反应时间为2小时,得到的弹性体的力学性能较佳；降温扩链法合成的GAP-TPE力学性能较好,并改善了升温扩链法合成体系粘度大、出料困难和DMF难排除等问题；随硬段质量分数的增加,BDO扩链GAP-TPE的拉伸强度增大,而断裂伸长率减小。
为保证含能粘结剂有尽可能高的能量,同时也具有良好的力学性能,以35%的硬段质量分数为前提,研究了具有HO(CH2CH2)nOH结构的几种扩链剂,如EDO、BDO和HDO对GAP-TPE性能的影响。用FTIR、GPC、元素分析、真密度、DMA和SEM等分析手段对弹性体的结构和性能进行了表征,合成的样品具有聚氨酯结构和一定的微相分离,BDO扩链GAP-TPE具有较好的综合性能,其密度为1.35 g·cm-3,数均相对分子质量为76630,拉伸强度(σb)为13.4 MPa,断裂伸长率(εb)为362%,玻璃化温度(Tg)为-22.3℃,储能模量(E',T=50℃)为22.6 MPa,合成的GAP-TPE具有较均一的断面形貌。
选择结构规整且含有内旋转柔性醚键的DEG为扩链剂,合成了GAP-TPE,与结构为HO(CH2CH2)nOH的扩链剂合成的弹性体相比较,DEG扩链GAP-TPE(硬段质量分数35%)的氢键密度增大,微相分离程度增强,力学性能提高。数均相对分子质量为84530,密度为1.37 g·cm-3,σb为14.6MPa,εb为414%,Tg为-24.9℃,储能模量(E’,T=50℃)为69MPa。
由于GAP-TPE的高温模量低影响发射药的高温力学性能,用扩链共混熟化的方法制备了NC/GAP-TPE共混物。XRD、真密度分析显示随着NC含量的增加,共混物的密度增大,促进了GAP-TPE硬段微区结晶；DMA分析显示5/95、10/90(质量比,下同)的NC/GAP-TPE只有一个玻璃化转变温度,20/80、40/60、60/40和80/20的NC/GAP-TPE试样有两个玻璃化转变峰且向中间靠拢,表明共混物为部分相混体系；σb由NC/GAP-TPE(5/95)的10.4MPa提高到NC/GAP-TPE(20/80)的20.4MPa,εb由NC/GAP-TPE(5/95)的264%降为NC/GAP-TPE(20/80)的139%；随着NC含量的增加,高温储能模量(E’,T=50℃)也增加,当NC/GAP-TPE的质量比为5/95、10/90、20/80、40/60、60/40和80/20时,储能模量E'分别为14、16、42、236、1747和2650 MPa；通过共混的方法可以制备性能互补的NC/GAP-TPE复合含能粘结剂,发挥NC高能量、高强度和GAP-TPE良好韧性的优点,通过调节其配比满足能量性能和力学性能的不同要求。
采用TG/DTG法,研究了DEG扩链GAP-TPE和质量比为20/80的NC/GAP-TPE的热分解过程和机理,根据DTG曲线的特点分峰,Kissinger法和Ozawa法求得活化能基本一致,GAP-TPE三个阶段分解的活化能分别是223,235和57kJ·mol-1, NC/GAP-TPE三个明显阶段的热分解活化能分别是163,166和292 kJ·mol-1,叠氮基的分解活化能下降,硬段氨基甲酸酯的分解活化能有所提高；Coats-Redfern积分法求得GAP-TPE的三个阶段的机理函数的积分式分别为[-ln(1-α)]1/3、-ln(1-α)和-ln(1-α), NC/GAP-TPE热分解的三个阶段的机理函数积分式都是G(α)=α2。
High energy and low vulnerability is being the trend of gun propellant development. Traditional Nitrocellulose (NC) binder based gun propellants has high energy, however the survival ability of weapon system is strongly affected by the vulnerability of the gun propellants, which has the possibility of deflagration-to-detonation upon stimulation such as heat, mechanical force, blast wave and efflux jet. Gun propellants which are based non energetic binders (such as cellulose, crosslinking or thermoset binder, and thermoplastic elastomer) have satisfactory mechanical properties but give relatively low energy. Glycidyl azide polymer (GAP) is a novel energetic binder being considered as the key component of gun propellants due to its insensitivity and high energy. The pendant azide group of GAP main chain results in low mechanical properties of gun propellants. So it is necessary to improve the mechanical properties of GAP binder. In this paper, a series of energetic thermoplastic elastomers with GAP prepolymer were synthesized and characterized for improving the micro domain of crystallization and then the mechanical properties of the binders. A novel blend with NC and GAP-TPE is further prepared to modify the GAP-TPE's drawback of modulus decreasing as temperature increasing. At last, the thermal decomposition kinetics of GAP-TPE and NC/GAP-TPE blends was thoroughly studied. The main work is as follows:
Energetic thermoplastic polyurethane elastomer is synthesized using GAP with number averaged molecular weight of 3000 as soft segment,4,4'-diphenylmethane diisocyanate (MDI) and 1,4-butanediol (BDO) as hard segments. The results showed that GAP-TPE synthesized by melt-prepolymerization has better mechanical properties, having the -NCO/-OH mole ratio (R) of 0.98 and reacting for 2h. The mechanical properties of GAP-TPE are better when reducing the chain extension temperature. The bulk viscosity of the mixture decreased as the reaction temperature of the chain extension decreased. Using BDO as chain extender, the GAP-TPE showed higher tensile strength and elongation at break at higher content of the hard segment.
In order to improve the mechanical properties of GAP-TPE, GAP-TPEs were synthesized with different chain extenders while the hard segment content was fixed as 35%. The studied chain extenders included EDO, BDO and HDO, having the structure of HO(CH2CH2)n OH. FTIR, GPC, Elemental analysis, DMA and Density are applied to characterize the synthesized elastomers. The elastomers have the same structure characteristic of polyurethane. The GAP-TPE using BDO as chain extender has better mechanical properties, tensile stress (σb) of 13.4 MPa, elongation at break (εb) of 362%, storage modulus (E',T=50℃) of 22.6 MPa. Its density is 1.35 g·cm-3. the number averaged molecular weight is 76630, and the glass-transition temperature (Tg) is -22.3℃. SEM photographs showed the homogeneous microstructure of the GAP-TPE.
Further using DEG as chain extender, the synthesized GAP-TPE with hard segment of 35% has better properties than those of HO (CH2CH2)n OH extended GAP-TPE. DEG extended GAP-TPE has a density of 1.37 g·cm-3, number averaged molecular weight of 84530,σb, of 14.6 MPa,εb of 414%, storage modulus (E',T=50℃) of 69MPa, and Tg of -24.9℃. DEG extended GAP-TPE also has higher degree of hydrogen bonding and micro-phase separation.
To improve the storage modulus of GAP-TPE at high temperature, NC/GAP-TPE blends are prepared by the step of chain extension, blending and aging. XRD and density analysis show that the densities of NC/GAP-TPE blends increase with the increase of NC content. The DMA analysis shows that NC/GAP-TPE (9/95,10/90, mass ratio, the same as follows) owns only one glass transition temperature, while two glass transition temperatures of NC/GAP-TPE (20/80,40/60,60/40,80/20) are observed and they shift closer to each other with the increase of NC content, implying that the blend was partially miscible. Theσb andεb of NC/GAP-TPE (20/80) are 20.4MPa and 139% whereas theσb andεb of NC/PEG-TPE (5/95) are 10.4MPa and 264%, respectively. When the mass ratio are 5/95,10/90,20/80,40/60, 60/40 and 80/20 for NC/PEG-TPE, the storage modulus (E', T=50℃) are 14,16,42,236, 1747 and 2650 MPa, respectively. Thus, the composite energetic binder, NC/GAP-TPE, combined the high modulus of NC with the good toughness of GAP-TPE, having the potential to adjust the properties of NC/GAP-TPE by changing the mass ratio of NC and GAP-TPE.
Thermogravimetric analysis (TG) and derivative thermogravimetry (DTG) are employed to evaluate the thermal decomposition behaviors of GAP-TPE and NC/GAP-TPE. The peak separation is performed to separate the thermal decomposition peak of GAP-TPE into several stages according to the characteristic of the experimental differential mass loss curve. The activation energy calculated with Ozawa methods for each decomposition stage has good agreement with the result calculated with Kissinger method. The activation energy of GAP-TPE in the three stages are 223,235 and 57 kJ·mol-1, respectively. The activation energy of NC/GAP-TPE in the three stages are 163,166 and 292 kJ·mol-1. The thermal decomposition activation energy of pendant azide group decreased and the hard segment carbamate increased after blending. In addition, the three stage's mechanism functions of GAP-TPE calculated by the Coats-Redfen method are [-ln(1-α)]1/3、-ln(1-α) and -ln(1-α), respectively. The mechanism functions of NC/GAP-TPE in three stages calculated by the Coats-Redfen method are all a2.
通过对含能热塑性弹性体(ETPE)结构分析和分子设计,选择相对分子质量为3000的GAP为软段,MDI和BDO为硬段,合成了一类GAP-TPE,对合成工艺进行了研究,当采用预聚体法,R值为0.98,预聚反应时间为2小时,得到的弹性体的力学性能较佳；降温扩链法合成的GAP-TPE力学性能较好,并改善了升温扩链法合成体系粘度大、出料困难和DMF难排除等问题；随硬段质量分数的增加,BDO扩链GAP-TPE的拉伸强度增大,而断裂伸长率减小。
为保证含能粘结剂有尽可能高的能量,同时也具有良好的力学性能,以35%的硬段质量分数为前提,研究了具有HO(CH2CH2)nOH结构的几种扩链剂,如EDO、BDO和HDO对GAP-TPE性能的影响。用FTIR、GPC、元素分析、真密度、DMA和SEM等分析手段对弹性体的结构和性能进行了表征,合成的样品具有聚氨酯结构和一定的微相分离,BDO扩链GAP-TPE具有较好的综合性能,其密度为1.35 g·cm-3,数均相对分子质量为76630,拉伸强度(σb)为13.4 MPa,断裂伸长率(εb)为362%,玻璃化温度(Tg)为-22.3℃,储能模量(E',T=50℃)为22.6 MPa,合成的GAP-TPE具有较均一的断面形貌。
选择结构规整且含有内旋转柔性醚键的DEG为扩链剂,合成了GAP-TPE,与结构为HO(CH2CH2)nOH的扩链剂合成的弹性体相比较,DEG扩链GAP-TPE(硬段质量分数35%)的氢键密度增大,微相分离程度增强,力学性能提高。数均相对分子质量为84530,密度为1.37 g·cm-3,σb为14.6MPa,εb为414%,Tg为-24.9℃,储能模量(E’,T=50℃)为69MPa。
由于GAP-TPE的高温模量低影响发射药的高温力学性能,用扩链共混熟化的方法制备了NC/GAP-TPE共混物。XRD、真密度分析显示随着NC含量的增加,共混物的密度增大,促进了GAP-TPE硬段微区结晶；DMA分析显示5/95、10/90(质量比,下同)的NC/GAP-TPE只有一个玻璃化转变温度,20/80、40/60、60/40和80/20的NC/GAP-TPE试样有两个玻璃化转变峰且向中间靠拢,表明共混物为部分相混体系；σb由NC/GAP-TPE(5/95)的10.4MPa提高到NC/GAP-TPE(20/80)的20.4MPa,εb由NC/GAP-TPE(5/95)的264%降为NC/GAP-TPE(20/80)的139%；随着NC含量的增加,高温储能模量(E’,T=50℃)也增加,当NC/GAP-TPE的质量比为5/95、10/90、20/80、40/60、60/40和80/20时,储能模量E'分别为14、16、42、236、1747和2650 MPa；通过共混的方法可以制备性能互补的NC/GAP-TPE复合含能粘结剂,发挥NC高能量、高强度和GAP-TPE良好韧性的优点,通过调节其配比满足能量性能和力学性能的不同要求。
采用TG/DTG法,研究了DEG扩链GAP-TPE和质量比为20/80的NC/GAP-TPE的热分解过程和机理,根据DTG曲线的特点分峰,Kissinger法和Ozawa法求得活化能基本一致,GAP-TPE三个阶段分解的活化能分别是223,235和57kJ·mol-1, NC/GAP-TPE三个明显阶段的热分解活化能分别是163,166和292 kJ·mol-1,叠氮基的分解活化能下降,硬段氨基甲酸酯的分解活化能有所提高；Coats-Redfern积分法求得GAP-TPE的三个阶段的机理函数的积分式分别为[-ln(1-α)]1/3、-ln(1-α)和-ln(1-α), NC/GAP-TPE热分解的三个阶段的机理函数积分式都是G(α)=α2。
High energy and low vulnerability is being the trend of gun propellant development. Traditional Nitrocellulose (NC) binder based gun propellants has high energy, however the survival ability of weapon system is strongly affected by the vulnerability of the gun propellants, which has the possibility of deflagration-to-detonation upon stimulation such as heat, mechanical force, blast wave and efflux jet. Gun propellants which are based non energetic binders (such as cellulose, crosslinking or thermoset binder, and thermoplastic elastomer) have satisfactory mechanical properties but give relatively low energy. Glycidyl azide polymer (GAP) is a novel energetic binder being considered as the key component of gun propellants due to its insensitivity and high energy. The pendant azide group of GAP main chain results in low mechanical properties of gun propellants. So it is necessary to improve the mechanical properties of GAP binder. In this paper, a series of energetic thermoplastic elastomers with GAP prepolymer were synthesized and characterized for improving the micro domain of crystallization and then the mechanical properties of the binders. A novel blend with NC and GAP-TPE is further prepared to modify the GAP-TPE's drawback of modulus decreasing as temperature increasing. At last, the thermal decomposition kinetics of GAP-TPE and NC/GAP-TPE blends was thoroughly studied. The main work is as follows:
Energetic thermoplastic polyurethane elastomer is synthesized using GAP with number averaged molecular weight of 3000 as soft segment,4,4'-diphenylmethane diisocyanate (MDI) and 1,4-butanediol (BDO) as hard segments. The results showed that GAP-TPE synthesized by melt-prepolymerization has better mechanical properties, having the -NCO/-OH mole ratio (R) of 0.98 and reacting for 2h. The mechanical properties of GAP-TPE are better when reducing the chain extension temperature. The bulk viscosity of the mixture decreased as the reaction temperature of the chain extension decreased. Using BDO as chain extender, the GAP-TPE showed higher tensile strength and elongation at break at higher content of the hard segment.
In order to improve the mechanical properties of GAP-TPE, GAP-TPEs were synthesized with different chain extenders while the hard segment content was fixed as 35%. The studied chain extenders included EDO, BDO and HDO, having the structure of HO(CH2CH2)n OH. FTIR, GPC, Elemental analysis, DMA and Density are applied to characterize the synthesized elastomers. The elastomers have the same structure characteristic of polyurethane. The GAP-TPE using BDO as chain extender has better mechanical properties, tensile stress (σb) of 13.4 MPa, elongation at break (εb) of 362%, storage modulus (E',T=50℃) of 22.6 MPa. Its density is 1.35 g·cm-3. the number averaged molecular weight is 76630, and the glass-transition temperature (Tg) is -22.3℃. SEM photographs showed the homogeneous microstructure of the GAP-TPE.
Further using DEG as chain extender, the synthesized GAP-TPE with hard segment of 35% has better properties than those of HO (CH2CH2)n OH extended GAP-TPE. DEG extended GAP-TPE has a density of 1.37 g·cm-3, number averaged molecular weight of 84530,σb, of 14.6 MPa,εb of 414%, storage modulus (E',T=50℃) of 69MPa, and Tg of -24.9℃. DEG extended GAP-TPE also has higher degree of hydrogen bonding and micro-phase separation.
To improve the storage modulus of GAP-TPE at high temperature, NC/GAP-TPE blends are prepared by the step of chain extension, blending and aging. XRD and density analysis show that the densities of NC/GAP-TPE blends increase with the increase of NC content. The DMA analysis shows that NC/GAP-TPE (9/95,10/90, mass ratio, the same as follows) owns only one glass transition temperature, while two glass transition temperatures of NC/GAP-TPE (20/80,40/60,60/40,80/20) are observed and they shift closer to each other with the increase of NC content, implying that the blend was partially miscible. Theσb andεb of NC/GAP-TPE (20/80) are 20.4MPa and 139% whereas theσb andεb of NC/PEG-TPE (5/95) are 10.4MPa and 264%, respectively. When the mass ratio are 5/95,10/90,20/80,40/60, 60/40 and 80/20 for NC/PEG-TPE, the storage modulus (E', T=50℃) are 14,16,42,236, 1747 and 2650 MPa, respectively. Thus, the composite energetic binder, NC/GAP-TPE, combined the high modulus of NC with the good toughness of GAP-TPE, having the potential to adjust the properties of NC/GAP-TPE by changing the mass ratio of NC and GAP-TPE.
Thermogravimetric analysis (TG) and derivative thermogravimetry (DTG) are employed to evaluate the thermal decomposition behaviors of GAP-TPE and NC/GAP-TPE. The peak separation is performed to separate the thermal decomposition peak of GAP-TPE into several stages according to the characteristic of the experimental differential mass loss curve. The activation energy calculated with Ozawa methods for each decomposition stage has good agreement with the result calculated with Kissinger method. The activation energy of GAP-TPE in the three stages are 223,235 and 57 kJ·mol-1, respectively. The activation energy of NC/GAP-TPE in the three stages are 163,166 and 292 kJ·mol-1. The thermal decomposition activation energy of pendant azide group decreased and the hard segment carbamate increased after blending. In addition, the three stage's mechanism functions of GAP-TPE calculated by the Coats-Redfen method are [-ln(1-α)]1/3、-ln(1-α) and -ln(1-α), respectively. The mechanism functions of NC/GAP-TPE in three stages calculated by the Coats-Redfen method are all a2.
引文
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