废旧黑索今资源化再利用研究
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摘要
黑索今具有威力大、猛度高、化学稳定性好等特点,已经被广泛应用于武器装备和民用爆破器材。它作为一种战略物资,必须有一定的储备量,目前的国储黑索今多为上世纪60-70年代产品,主要有单质黑索今和钝化黑索今两类。由于受当时生产条件、工艺技术的限制,国储黑索今的一些性能指标已经不能满足使用要求,成为一种长期积压的废旧物资。国储单质黑索今的主要问题表现为晶体形态、晶体粒度不能满足使用要求,以及包装物被腐蚀破坏成为机械杂质进入黑索今中；国储钝化黑索今主要问题表现为黑索今表面钝感剂脱落、流散性差、结块成团、进入机械杂质等。因此对该类废旧黑索今的资源化再利用研究具有重大意义。
本论文通过对国储废旧黑索今现状的分析,进行了国储废旧黑索今资源化再利用研究。本论文创新点及研究成果主要有以下几点：
(1)首次提出“特质黑索今”概念,文中将具有感度低、晶体密度高、晶体粒度分布窄等特点的一类黑索今称为“特质黑索今”。“特质黑索今”是为满足一些新型号武器装备应运而生,是黑索今研究领域的特殊方向。
(2)由于受黑索今生产技术水平的限制,“特质黑索今”无法在工业生产中直接得到,必须依靠深加工制备。‘'250μm～425μm球形RDX"是具有代表性的“特质黑索今’不仅要求黑索今粒度分布窄,而且要求晶体呈球形。本文进行了以废旧单质黑索今为溶质、浓硝酸为溶剂制备‘'250μm～425μm球形RDX"的工艺研究,确定了溶液浓度、稀释剂用量、稀释速度、结晶温度、搅拌速度、保温时间等工艺条件。所得产晶体中"250μm～425μm球形RDX"含量达到77.6%,堆积密度达到1.26g/cm3,比同粒度级别的普通RDX提高31.3%；机械感度比同粒度级别的普通RDX有一定程度降低,其中撞击感度降低22%,摩擦感度降低20%
(3)进行了利用废旧黑索今制备导爆管专用黑索今研究。通过溶液浓度、结晶温度、结晶时间、搅拌速度等工艺研究,成功研制了普通导爆管和高爆速导爆管专用黑索今。经11个厂家22亿米导爆管的使用表明,研制的导爆管专用黑索今性能稳定、效果良好。
(4)进行了以废旧黑索今为原材料生产聚能石油射孔弹用高聚物粘结炸药研究。通过黑索今粒度级配研究,获得最佳级配为废旧RDX/D_(50)≤25μm=9:1,确定优化造粒工艺：RDX：水=1：2；造粒温度；55℃-60℃；搅拌速度：120r/min;蒸馏温度：65℃～75℃；蒸馏真空度0.04MPa～0.05MPa。制备的粘结炸药堆积密度达到0.90g/cm3,高于R852炸药12.5%,高于SH-931炸药5.9%；射孔深度比R852炸药和SH-931炸药提高7%。每年可以转化废旧黑索今120余吨,累计转化废旧黑索今300余吨。
(5)研究成功了激发穿透力强的宽高频子波震源炸药,并首次将金属粉末作为添加剂应用到震源炸药,新研制的炸药地震反射记录中浅层扫描频率比高爆速震源炸药提高10Hz以上；
(6)国内首先完成了废旧钝化黑索今工业化回收研究,利用表面活性剂的增溶作用对废旧钝化黑索今进行回收,得到的RDX-H纯度达到99.65%以上,满足民用爆破器材使用要求。平均每年可以转化废旧钝化黑索今400余吨,累计转化废旧钝化黑索今800余吨。
(7)研制成功了以RDX-H为主体的雷管许用炸药。优化工艺条件为：水：RDX-H:水=2：1；造粒搅拌速度：150r/min,破乳温度：50℃；造粒温度：55℃～60℃；蒸馏搅拌速度调：130r/min；蒸馏温度：65℃-75℃;真空度：0.04MPa～0.05Mpa。该工艺已经进行规模花生产,每年可以转化RDX-H 200余吨,累计转化钝化黑索今500余吨。
RDX, with the characteristic of high strength and brisance, has been widely used in ammunition and civil explosive materials. Since it is a kind of strategic material, a necessary amount of reserve is required. The current national reserved RDX are mostly the products of the period from 1960s to 1970s, including compound RDX and passivated RDX. Due to the restriction of the producing condition and technology, some performance properties of the national reserved RDX have fallen out of application requirements, becoming a kind of waste material. The major problem of the national reserved compound RDX are the shape and granularity of crystal as well as the mechanical impurities resulted from the corrosion of the package; the major problem of the national reserved passivated RDX are the falling off the superficial passivator, the poor free-flowing property, agglomerating, the mechanical impurities and so on. Therefore, it is of great importance to study the recycling and reapplication of the waste RDX reserved.
Through the analysis of the present situation, this study focused on the recycling and reapplication of the waste RDX reserved. The innovations and achievements of the study are as follows:
(1) It is the first time to propose the concept of "special quality RDX". RDX with low sensitivity, high crystal density and narrow distribution of crystal granularity is called "special quality RDX". It aims at satisfying the specific requirements of new weapons and has become a special field of this area.
(2) Constricted by the technology level, it is impossible to get "special quality RDX" directly and it can only be produced by deep process. As a representative of "special quality RDX", "250μm～425μm spherical RDX" calls for not only the narrow distribution of crystal granularity but also the spheroid of the crystal shape. In this study, technology research was conducted using waste compound RDX as solute, concentrated nitric acid as solvent to prepare "250μm～425μm spherical RDX", and some preparing parameters such as the concentration of the solution, the amount of dilution agent, the dilution speed, the temperature of crystallization, the stirring speed, the insulation time and so on have been determined. The obtained products have 77.6% the "250μm～425μm spherical RDX", and the bulk density reached 1.26g/cm~3, increased by 31.3 percent compared to the normal RDX with the same granularity level; The mechanical sensitivity reduced 20 percent compared to the normal RDX with the same granularity level.
(3) The preparation of special RDX for nonel (explosive lead) using waste RDX to prepare was researched. The solution concentration, crystallization temperature, crystallization time, stirring speed, were thoroughly investigated. The special RDX for normal nonel and the lead with high detonation velocity have been successfully developed. The application of 2.2 billion meters lead in 11 factories indicates the stable performance and effectiveness of the special RDX for lead.
(4) The research of using waste RDX as raw material to produce high polymer bonded explosive shaped charge for petroleum was conducted. Through the study of the RDX granularity, the best ratio was got when the waste RDX/D_(50)≤25μm=9:1, the granulation technology was optimized:RDX:water=1:2; granulation temperature 55～60℃; the stirring speed:120r/min; distillation temperature:65℃～75℃; distillation vacuum: 0.04MPa～0.05MPa. The bulk density of the polymer bonded explosive reached 0.90g/cm~3, which was 12.5 percent higher compared to R85 explosive,5.9 percent higher compared to SH-931 explosive; the perforation depth of the bonded explosive increased 7 percent compared to R85 explosive and SH-931 explosive. Above 120t waste RDX are transformed annually (above 300t cumulatively).
(5) Wide and high frequency wavelet seismic charge with strong penetration was successfully developed and metal powder was used in seismic charge as additive for the first time. Seismic reflection records of the newly developed explosive showed that shallow scanning frequency was increased by more than 10Hz compared to seismic source with high detonation velocity.
(6) The research of industrial recycling of passivated RDX was conducted for the first time in the country. With the solubilization of surfactant, the waste passivated RDX can be recycled. As a result, the purity of the RDX-H reached more than 99.65 percent, which was satisfied the requirements of civil explosive materials. More than 400t waste passivated RDX are transformed annually on average (800t cumulatively).
(7) Using RDX-H as the major components, available explosive for detonator was developed successfully. Optimized technological condition are as follows:water:RDX-H=2:1; stirring speed for granulation:150r/min; demulsification temperature:50℃; granulation temperature:55℃～60℃; stirring speed for distillation:130r/min; distillation temperature: 65℃～75℃; vacuum:0.04MPa-0.05MPa. This technology has been used in large-scale production to transform RDX-H for more than 200t per year, and more than 500t cumulatively.
本论文通过对国储废旧黑索今现状的分析,进行了国储废旧黑索今资源化再利用研究。本论文创新点及研究成果主要有以下几点：
(1)首次提出“特质黑索今”概念,文中将具有感度低、晶体密度高、晶体粒度分布窄等特点的一类黑索今称为“特质黑索今”。“特质黑索今”是为满足一些新型号武器装备应运而生,是黑索今研究领域的特殊方向。
(2)由于受黑索今生产技术水平的限制,“特质黑索今”无法在工业生产中直接得到,必须依靠深加工制备。‘'250μm～425μm球形RDX"是具有代表性的“特质黑索今’不仅要求黑索今粒度分布窄,而且要求晶体呈球形。本文进行了以废旧单质黑索今为溶质、浓硝酸为溶剂制备‘'250μm～425μm球形RDX"的工艺研究,确定了溶液浓度、稀释剂用量、稀释速度、结晶温度、搅拌速度、保温时间等工艺条件。所得产晶体中"250μm～425μm球形RDX"含量达到77.6%,堆积密度达到1.26g/cm3,比同粒度级别的普通RDX提高31.3%；机械感度比同粒度级别的普通RDX有一定程度降低,其中撞击感度降低22%,摩擦感度降低20%
(3)进行了利用废旧黑索今制备导爆管专用黑索今研究。通过溶液浓度、结晶温度、结晶时间、搅拌速度等工艺研究,成功研制了普通导爆管和高爆速导爆管专用黑索今。经11个厂家22亿米导爆管的使用表明,研制的导爆管专用黑索今性能稳定、效果良好。
(4)进行了以废旧黑索今为原材料生产聚能石油射孔弹用高聚物粘结炸药研究。通过黑索今粒度级配研究,获得最佳级配为废旧RDX/D_(50)≤25μm=9:1,确定优化造粒工艺：RDX：水=1：2；造粒温度；55℃-60℃；搅拌速度：120r/min;蒸馏温度：65℃～75℃；蒸馏真空度0.04MPa～0.05MPa。制备的粘结炸药堆积密度达到0.90g/cm3,高于R852炸药12.5%,高于SH-931炸药5.9%；射孔深度比R852炸药和SH-931炸药提高7%。每年可以转化废旧黑索今120余吨,累计转化废旧黑索今300余吨。
(5)研究成功了激发穿透力强的宽高频子波震源炸药,并首次将金属粉末作为添加剂应用到震源炸药,新研制的炸药地震反射记录中浅层扫描频率比高爆速震源炸药提高10Hz以上；
(6)国内首先完成了废旧钝化黑索今工业化回收研究,利用表面活性剂的增溶作用对废旧钝化黑索今进行回收,得到的RDX-H纯度达到99.65%以上,满足民用爆破器材使用要求。平均每年可以转化废旧钝化黑索今400余吨,累计转化废旧钝化黑索今800余吨。
(7)研制成功了以RDX-H为主体的雷管许用炸药。优化工艺条件为：水：RDX-H:水=2：1；造粒搅拌速度：150r/min,破乳温度：50℃；造粒温度：55℃～60℃；蒸馏搅拌速度调：130r/min；蒸馏温度：65℃-75℃;真空度：0.04MPa～0.05Mpa。该工艺已经进行规模花生产,每年可以转化RDX-H 200余吨,累计转化钝化黑索今500余吨。
RDX, with the characteristic of high strength and brisance, has been widely used in ammunition and civil explosive materials. Since it is a kind of strategic material, a necessary amount of reserve is required. The current national reserved RDX are mostly the products of the period from 1960s to 1970s, including compound RDX and passivated RDX. Due to the restriction of the producing condition and technology, some performance properties of the national reserved RDX have fallen out of application requirements, becoming a kind of waste material. The major problem of the national reserved compound RDX are the shape and granularity of crystal as well as the mechanical impurities resulted from the corrosion of the package; the major problem of the national reserved passivated RDX are the falling off the superficial passivator, the poor free-flowing property, agglomerating, the mechanical impurities and so on. Therefore, it is of great importance to study the recycling and reapplication of the waste RDX reserved.
Through the analysis of the present situation, this study focused on the recycling and reapplication of the waste RDX reserved. The innovations and achievements of the study are as follows:
(1) It is the first time to propose the concept of "special quality RDX". RDX with low sensitivity, high crystal density and narrow distribution of crystal granularity is called "special quality RDX". It aims at satisfying the specific requirements of new weapons and has become a special field of this area.
(2) Constricted by the technology level, it is impossible to get "special quality RDX" directly and it can only be produced by deep process. As a representative of "special quality RDX", "250μm～425μm spherical RDX" calls for not only the narrow distribution of crystal granularity but also the spheroid of the crystal shape. In this study, technology research was conducted using waste compound RDX as solute, concentrated nitric acid as solvent to prepare "250μm～425μm spherical RDX", and some preparing parameters such as the concentration of the solution, the amount of dilution agent, the dilution speed, the temperature of crystallization, the stirring speed, the insulation time and so on have been determined. The obtained products have 77.6% the "250μm～425μm spherical RDX", and the bulk density reached 1.26g/cm~3, increased by 31.3 percent compared to the normal RDX with the same granularity level; The mechanical sensitivity reduced 20 percent compared to the normal RDX with the same granularity level.
(3) The preparation of special RDX for nonel (explosive lead) using waste RDX to prepare was researched. The solution concentration, crystallization temperature, crystallization time, stirring speed, were thoroughly investigated. The special RDX for normal nonel and the lead with high detonation velocity have been successfully developed. The application of 2.2 billion meters lead in 11 factories indicates the stable performance and effectiveness of the special RDX for lead.
(4) The research of using waste RDX as raw material to produce high polymer bonded explosive shaped charge for petroleum was conducted. Through the study of the RDX granularity, the best ratio was got when the waste RDX/D_(50)≤25μm=9:1, the granulation technology was optimized:RDX:water=1:2; granulation temperature 55～60℃; the stirring speed:120r/min; distillation temperature:65℃～75℃; distillation vacuum: 0.04MPa～0.05MPa. The bulk density of the polymer bonded explosive reached 0.90g/cm~3, which was 12.5 percent higher compared to R85 explosive,5.9 percent higher compared to SH-931 explosive; the perforation depth of the bonded explosive increased 7 percent compared to R85 explosive and SH-931 explosive. Above 120t waste RDX are transformed annually (above 300t cumulatively).
(5) Wide and high frequency wavelet seismic charge with strong penetration was successfully developed and metal powder was used in seismic charge as additive for the first time. Seismic reflection records of the newly developed explosive showed that shallow scanning frequency was increased by more than 10Hz compared to seismic source with high detonation velocity.
(6) The research of industrial recycling of passivated RDX was conducted for the first time in the country. With the solubilization of surfactant, the waste passivated RDX can be recycled. As a result, the purity of the RDX-H reached more than 99.65 percent, which was satisfied the requirements of civil explosive materials. More than 400t waste passivated RDX are transformed annually on average (800t cumulatively).
(7) Using RDX-H as the major components, available explosive for detonator was developed successfully. Optimized technological condition are as follows:water:RDX-H=2:1; stirring speed for granulation:150r/min; demulsification temperature:50℃; granulation temperature:55℃～60℃; stirring speed for distillation:130r/min; distillation temperature: 65℃～75℃; vacuum:0.04MPa-0.05MPa. This technology has been used in large-scale production to transform RDX-H for more than 200t per year, and more than 500t cumulatively.
引文
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