超细含能材料结晶品质的超临界控制技术研究
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摘要
当今战场环境变化的日新月异，对含能材料性能提出了越来越高的要求，提高含能材料的结晶品质变得至关重要。目前提高含能材料结晶品质的控制与研究有很多不足之处，而新兴的超临界流体技术发展方兴未艾，展现出了优异的特性和广阔的空间。因此，将超临界流体技术应用于控制含能材料结晶品质具有重要意义。本论文通过挖掘超临界条件下控制晶体成核和生长以及晶体形态的机理，以及研究多种溶剂在超临界CO2（SC-CO2）中的溶解特性和变化规律，利用超临界流体技术对含能材料的结晶品质进行了控制，并对影响含能材料结晶品质的各因素进行了更为深入的探讨，以实现得到理想晶型为基本目标，对理想晶型的样品做了较为系统的表征和性能测试，为其进一步工程化研究打好基础。主要工作如下：
1.测定常用有机溶剂在SC-CO2中的溶解度。过饱和度是晶体成核和生长的推动力，通过调节过饱和度可以控制晶体粒度和粒度分布，需要对有机溶剂在SC-CO2中的溶解特性进行研究。在温度308.15K、318.15K、328.15K，压力8-15MPa的范围内，测定了丙酮、乙酸乙酯、N,N-二甲基甲酰胺（DMF）、二甲基亚砜（DMSO）、环己酮和N-甲基吡咯烷酮（NMP）共7种有机溶剂在SC-CO2中的溶解度，表现出如下规律：温度相同时，溶解度随压力的升高先增大后减小；在相同压力下，高于转变压力时，温度越高，溶解度越大；低于转变压力时，温度越低，溶解度越大。这为进一步地确定和研究溶剂及不同工艺过程中的温度和压力对含能材料结晶品质的控制作用提供了良好的数据及理论支持。
2. SEDS法（超临界流体增强溶液扩散技术）对RDX超细结晶品质的控制和扩试研究。溶剂是影响晶体形貌重要的因素，溶剂的性质不同得到了RDX的形貌不同。通过选用多种不同的有机溶剂一一进行试验对比，最终确定DMF是制备出粒状RDX的理想溶剂。在此基础上，研究了影响SEDS法制备超细RDX结晶品质的主要因素，如压力、CO2流速、溶液流速和温度等，结果表明：RDX颗粒状所占的比例随着压力升高而降低，粒度也相应减小和粒度分布变窄；温度的升高不利于得到粒度小且分布窄的RDX结晶。为制得超细结晶品质良好的RDX，做了扩试实验，扩试工艺条件为：RDX/DMF浓度26.7%、温度35℃、压力9.0MPa、溶液流速2ml/min和CO2流速6kg/h，萃取时间为15min。在最佳工艺条件下所得RDX晶体边缘光滑、形貌规则趋于球形，且粒度减小到1μm左右、粒度分布均匀，流散性良好，1h内可处理32g。SEDS法制备出的超细RDX与原料RDX相比，表现出较低的表观热分解活化能，机械感度有显著地降低。其中，特性落高值、摩擦爆炸概率和冲击波感度分别下降了67.3%、56.7%和45.6%，静电安全性合格。
3. SEDS法和GAS法（超临界反溶剂法）对HMX结晶品质的控制。HMX是多晶型化合物，其中以β-HMX的综合性能最好、为理想晶型，因此，成功制备出对β-HMX是控制HMX结晶品质的关键。综合考虑到溶剂和工艺对HNIW晶型的作用，研究了SEDS法和GAS法工艺中多种溶剂对HMX晶型的影响，结果表明：SEDS法不能成功制得β-HMX，大都为γ-HMX结晶；当以丙酮或DMSO为有机溶剂时，在合适的工艺条件下GAS可得到β-HMX；环己酮或乙腈为溶剂时GAS工艺制得的HMX为γ-型，NMP作溶剂时为δ-型。同时，研究了溶剂和工艺对HMX形貌、粒度及粒度分布的影响，结果表明：SEDS法制得的HMX粒度小且粒度分布窄，部分可达到亚微米级，但其形貌复杂，压力升高、温度降低和浓度增大均有助于得到粒度小而形貌趋于粒状的HMX粒子；GAS法制得的HMX结晶几乎全为粒状，但粒度分布宽，有的粒度达到了30μm及以上，压力是影响HMX粒度的最主要因素。对GAS法丙酮制得的β-HMX做了性能测试，其热分析、机械感度和冲击波感度与原料相差不大。
4. SEDS法、GAS法及“优化”SAS法对HNIW结晶品质的控制。结晶条件决定着含能材料的结晶品质，研究了不同工艺和有机溶剂对HNIW结晶品质的控制作用，结果表明：SEDS法和“优化”SAS法制备出的HNIW样品颗粒表面光滑、粒度小且分布均匀、形状规整、球形度高、纯度高；但是不能成功制得理想的ε-HNIW；分别以丙酮、乙酸乙酯为溶剂，采用GAS法可制得ε-HNIW。性能测试结果表明，GAS法以乙酸乙酯和丙酮制备出的HNIW的分解峰温较原料HNIW提前了4.29和2.93℃，放热量分别提高了647.7和357.7J/g；机械感度和冲击波感度降低，其以乙酸乙酯为有机溶剂的特性落高、爆炸概率和隔板厚度分别约降低了50.0%、30.0%和47.7%；以丙酮为有机溶剂的分别降低了约47.6%、21.7%和41.6%，静电安全性符合要求。
Battlefield environment never-ending changes and improvements, all kinds of applicationsin reality require higher and higher performance on energetic materials. So it is critical toimprove crystallization quality of the energetic materials. There are many deficiencies in thecontrol and study on enhancing crystallization quality of the energetic materials. But thenewly born supercritical fluids technology which has developed rapidly in recent years in theworld, exhibit fantastic properties and lead to an even more diverse range of applications.Therefore, it has very important significance in applying supercritical fluids technique intoenhancing crystallization quality of the energetic materials.
In this dissertation, the dissolution characteristic and the changing trend of a variety oforganic solvents (for example, acetone, ethyl acetate, N, N-dimethyl formamide, dimethylsulfoxide, cyclohexanone, and N-methyl pyrrolidone) in supercritical CO2(SC-CO2) wasinvestigated. And the influences of experiment parameters in different manufacturingprocesses were studied. Based on the mentioned above researches, ultra-fine energeticmaterials with good crystallization quality were prepared by a series of experiments andseveral major factors influencing their quality were investigated. In the end, samples withideal crystal form were characterized and performance testing systematically so as to make agood theoretical basis for further engineering research. The main study is as follows:
1. The solubility of common organic solvents in SC-CO2was determined. At thetemperature of308.15K,318.15K,328.15K, the range of the pressure within8-15MPa, thesolubility in common organic solvents in SC-CO2show the following rules:(1) at the sametemperature, the solubility increases with pressure increases first and then decreases;(2) underthe same pressure which is higher than the transition pressure, with the increase of thetemperature, the solubility increases either; below the transition pressure, the lower thetemperature, the greater the solubility. That provides a good data and theoretical basis for thedifferent supercritical fluids crystallization processed to study the influences of temperatureand pressure and control crystallization quality of energetic materials.
2. The control of RDX crystallization quality and engineering research were investigatedduring the process of solution enhanced dispersion by supercritical fluids (SEDS process). Inthe SEDS process, the solvent is the most important factor to influence the morphology ofRDX crystals. For the complex morphology of crystals obtained by SEDS process, we had chosen a variety of different organic solvents and contrasted the results one by one. Theresults show that DMF is the ideal solvent to prepare granular RDX crystals. In order tocontrol effectively particle size and particle size of RDX, we explore the effects of the mainfactors (such as pressure, CO2flow rate, solution flow rate and temperature, etc) oncrystallization quality in SEDS process. When the pressure increases, the proportion of RDXgranular decreases, the particle size reduced and particle size distribution becomes narrow. Inaddition, improving temperature is not conducive to obtain RDX with small particle size andnarrow distribution. The experiment conditions on the sea are concentration26.7%,temperature35℃, pressure9.0MPa, solvent flow rate2ml/min, CO2flow rate6kg/h andextraction time15min. The edge of fine RDX particles is smooth, and shape nearly spherical;particle size reduced to1μm; fine RDX particles have good fluidity, low mechanicalsensitivity and can be prepared32g per hour. Compared with raw material RDX, ultrafineRDX prepared by SEDS process showed the activation energy is much lower, and mechanicalsensitivity reduced remarkably. Among them, characteristic height value, friction explosionprobability and shock sensitivity decreased by67.3%,56.7%and45.6%, and the electrostaticsafety is qualified.
3. The control of HMX crystallization quality was investigated during SEDS process andGAS process (Gas Supercritical Anti-solvent). Change rule of crystal morphology and particlesize and size distribution were studied using variety of organic solvent by SEDS process andGAS process, respectively. The morphology of HMX particle prepared by SEDS process iscomplex, but the particle size is small and size distribution is narrow. In other words, theybelong to ultra-fine particle and some reaches submicron-size. Pressure increases, temperaturedecreases or concentration augments is helpful to get granular and small size HMX particles.HMX particles obtained by GAS process are almost all the granular, but have a wide particlesize distribution. Pressure is the most important factor influencing the particle size of HMX.When the other conditions are the same, the morphology and particle size varies with organicsolvent changes. Under the suitable process conditions, using GAS process can obtainβ-HMX when acetone or DMSO as organic solvent. Performance test were performed on theβ-HMX particles crystallized from acetone by GAS process. The results show that the thermalanalysis, the mechanical sensitivity and shock sensitivity tend to raw HMX.
4. The control of HNIW crystallization quality was investigated during SEDS process, GAS process and "optimization" SAS process. Compared with "optimization" SAS processand GAS process, the HNIW particles obtained by SEDS process has smooth surface, smallsize, uniform distribution, regular shape, high sphericity, and high purity. But ε-HNIW cannotbe prepared successfully which is mainly attributed to the SEDS process. While using GASprocess, ε-HNIW can be obtained when acetone as solvent. The performance test results showthat compared with raw HNIW, the peak temperature ahead of4.29and2.93℃; heat outputincreased647.7and357.7J/g when ethyl acetate and acetone as solvent respectively.Mechanical sensitivity and shock sensitivity reduced, the drop height, the explosionprobability and the plate thickness were reduced by50%,30%and47.7%when ethyl acetateas solvent; when acetone as solvent they reduced approximately by47.6%,21.7%and41.6%;the electrostatic safety is qualified.
1.测定常用有机溶剂在SC-CO2中的溶解度。过饱和度是晶体成核和生长的推动力，通过调节过饱和度可以控制晶体粒度和粒度分布，需要对有机溶剂在SC-CO2中的溶解特性进行研究。在温度308.15K、318.15K、328.15K，压力8-15MPa的范围内，测定了丙酮、乙酸乙酯、N,N-二甲基甲酰胺（DMF）、二甲基亚砜（DMSO）、环己酮和N-甲基吡咯烷酮（NMP）共7种有机溶剂在SC-CO2中的溶解度，表现出如下规律：温度相同时，溶解度随压力的升高先增大后减小；在相同压力下，高于转变压力时，温度越高，溶解度越大；低于转变压力时，温度越低，溶解度越大。这为进一步地确定和研究溶剂及不同工艺过程中的温度和压力对含能材料结晶品质的控制作用提供了良好的数据及理论支持。
2. SEDS法（超临界流体增强溶液扩散技术）对RDX超细结晶品质的控制和扩试研究。溶剂是影响晶体形貌重要的因素，溶剂的性质不同得到了RDX的形貌不同。通过选用多种不同的有机溶剂一一进行试验对比，最终确定DMF是制备出粒状RDX的理想溶剂。在此基础上，研究了影响SEDS法制备超细RDX结晶品质的主要因素，如压力、CO2流速、溶液流速和温度等，结果表明：RDX颗粒状所占的比例随着压力升高而降低，粒度也相应减小和粒度分布变窄；温度的升高不利于得到粒度小且分布窄的RDX结晶。为制得超细结晶品质良好的RDX，做了扩试实验，扩试工艺条件为：RDX/DMF浓度26.7%、温度35℃、压力9.0MPa、溶液流速2ml/min和CO2流速6kg/h，萃取时间为15min。在最佳工艺条件下所得RDX晶体边缘光滑、形貌规则趋于球形，且粒度减小到1μm左右、粒度分布均匀，流散性良好，1h内可处理32g。SEDS法制备出的超细RDX与原料RDX相比，表现出较低的表观热分解活化能，机械感度有显著地降低。其中，特性落高值、摩擦爆炸概率和冲击波感度分别下降了67.3%、56.7%和45.6%，静电安全性合格。
3. SEDS法和GAS法（超临界反溶剂法）对HMX结晶品质的控制。HMX是多晶型化合物，其中以β-HMX的综合性能最好、为理想晶型，因此，成功制备出对β-HMX是控制HMX结晶品质的关键。综合考虑到溶剂和工艺对HNIW晶型的作用，研究了SEDS法和GAS法工艺中多种溶剂对HMX晶型的影响，结果表明：SEDS法不能成功制得β-HMX，大都为γ-HMX结晶；当以丙酮或DMSO为有机溶剂时，在合适的工艺条件下GAS可得到β-HMX；环己酮或乙腈为溶剂时GAS工艺制得的HMX为γ-型，NMP作溶剂时为δ-型。同时，研究了溶剂和工艺对HMX形貌、粒度及粒度分布的影响，结果表明：SEDS法制得的HMX粒度小且粒度分布窄，部分可达到亚微米级，但其形貌复杂，压力升高、温度降低和浓度增大均有助于得到粒度小而形貌趋于粒状的HMX粒子；GAS法制得的HMX结晶几乎全为粒状，但粒度分布宽，有的粒度达到了30μm及以上，压力是影响HMX粒度的最主要因素。对GAS法丙酮制得的β-HMX做了性能测试，其热分析、机械感度和冲击波感度与原料相差不大。
4. SEDS法、GAS法及“优化”SAS法对HNIW结晶品质的控制。结晶条件决定着含能材料的结晶品质，研究了不同工艺和有机溶剂对HNIW结晶品质的控制作用，结果表明：SEDS法和“优化”SAS法制备出的HNIW样品颗粒表面光滑、粒度小且分布均匀、形状规整、球形度高、纯度高；但是不能成功制得理想的ε-HNIW；分别以丙酮、乙酸乙酯为溶剂，采用GAS法可制得ε-HNIW。性能测试结果表明，GAS法以乙酸乙酯和丙酮制备出的HNIW的分解峰温较原料HNIW提前了4.29和2.93℃，放热量分别提高了647.7和357.7J/g；机械感度和冲击波感度降低，其以乙酸乙酯为有机溶剂的特性落高、爆炸概率和隔板厚度分别约降低了50.0%、30.0%和47.7%；以丙酮为有机溶剂的分别降低了约47.6%、21.7%和41.6%，静电安全性符合要求。
Battlefield environment never-ending changes and improvements, all kinds of applicationsin reality require higher and higher performance on energetic materials. So it is critical toimprove crystallization quality of the energetic materials. There are many deficiencies in thecontrol and study on enhancing crystallization quality of the energetic materials. But thenewly born supercritical fluids technology which has developed rapidly in recent years in theworld, exhibit fantastic properties and lead to an even more diverse range of applications.Therefore, it has very important significance in applying supercritical fluids technique intoenhancing crystallization quality of the energetic materials.
In this dissertation, the dissolution characteristic and the changing trend of a variety oforganic solvents (for example, acetone, ethyl acetate, N, N-dimethyl formamide, dimethylsulfoxide, cyclohexanone, and N-methyl pyrrolidone) in supercritical CO2(SC-CO2) wasinvestigated. And the influences of experiment parameters in different manufacturingprocesses were studied. Based on the mentioned above researches, ultra-fine energeticmaterials with good crystallization quality were prepared by a series of experiments andseveral major factors influencing their quality were investigated. In the end, samples withideal crystal form were characterized and performance testing systematically so as to make agood theoretical basis for further engineering research. The main study is as follows:
1. The solubility of common organic solvents in SC-CO2was determined. At thetemperature of308.15K,318.15K,328.15K, the range of the pressure within8-15MPa, thesolubility in common organic solvents in SC-CO2show the following rules:(1) at the sametemperature, the solubility increases with pressure increases first and then decreases;(2) underthe same pressure which is higher than the transition pressure, with the increase of thetemperature, the solubility increases either; below the transition pressure, the lower thetemperature, the greater the solubility. That provides a good data and theoretical basis for thedifferent supercritical fluids crystallization processed to study the influences of temperatureand pressure and control crystallization quality of energetic materials.
2. The control of RDX crystallization quality and engineering research were investigatedduring the process of solution enhanced dispersion by supercritical fluids (SEDS process). Inthe SEDS process, the solvent is the most important factor to influence the morphology ofRDX crystals. For the complex morphology of crystals obtained by SEDS process, we had chosen a variety of different organic solvents and contrasted the results one by one. Theresults show that DMF is the ideal solvent to prepare granular RDX crystals. In order tocontrol effectively particle size and particle size of RDX, we explore the effects of the mainfactors (such as pressure, CO2flow rate, solution flow rate and temperature, etc) oncrystallization quality in SEDS process. When the pressure increases, the proportion of RDXgranular decreases, the particle size reduced and particle size distribution becomes narrow. Inaddition, improving temperature is not conducive to obtain RDX with small particle size andnarrow distribution. The experiment conditions on the sea are concentration26.7%,temperature35℃, pressure9.0MPa, solvent flow rate2ml/min, CO2flow rate6kg/h andextraction time15min. The edge of fine RDX particles is smooth, and shape nearly spherical;particle size reduced to1μm; fine RDX particles have good fluidity, low mechanicalsensitivity and can be prepared32g per hour. Compared with raw material RDX, ultrafineRDX prepared by SEDS process showed the activation energy is much lower, and mechanicalsensitivity reduced remarkably. Among them, characteristic height value, friction explosionprobability and shock sensitivity decreased by67.3%,56.7%and45.6%, and the electrostaticsafety is qualified.
3. The control of HMX crystallization quality was investigated during SEDS process andGAS process (Gas Supercritical Anti-solvent). Change rule of crystal morphology and particlesize and size distribution were studied using variety of organic solvent by SEDS process andGAS process, respectively. The morphology of HMX particle prepared by SEDS process iscomplex, but the particle size is small and size distribution is narrow. In other words, theybelong to ultra-fine particle and some reaches submicron-size. Pressure increases, temperaturedecreases or concentration augments is helpful to get granular and small size HMX particles.HMX particles obtained by GAS process are almost all the granular, but have a wide particlesize distribution. Pressure is the most important factor influencing the particle size of HMX.When the other conditions are the same, the morphology and particle size varies with organicsolvent changes. Under the suitable process conditions, using GAS process can obtainβ-HMX when acetone or DMSO as organic solvent. Performance test were performed on theβ-HMX particles crystallized from acetone by GAS process. The results show that the thermalanalysis, the mechanical sensitivity and shock sensitivity tend to raw HMX.
4. The control of HNIW crystallization quality was investigated during SEDS process, GAS process and "optimization" SAS process. Compared with "optimization" SAS processand GAS process, the HNIW particles obtained by SEDS process has smooth surface, smallsize, uniform distribution, regular shape, high sphericity, and high purity. But ε-HNIW cannotbe prepared successfully which is mainly attributed to the SEDS process. While using GASprocess, ε-HNIW can be obtained when acetone as solvent. The performance test results showthat compared with raw HNIW, the peak temperature ahead of4.29and2.93℃; heat outputincreased647.7and357.7J/g when ethyl acetate and acetone as solvent respectively.Mechanical sensitivity and shock sensitivity reduced, the drop height, the explosionprobability and the plate thickness were reduced by50%,30%and47.7%when ethyl acetateas solvent; when acetone as solvent they reduced approximately by47.6%,21.7%and41.6%;the electrostatic safety is qualified.
引文
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