CN1900706A - Detector for boron containing lean oxygen propellant heat value - Google Patents
Detector for boron containing lean oxygen propellant heat value Download PDFInfo
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- CN1900706A CN1900706A CN 200610042932 CN200610042932A CN1900706A CN 1900706 A CN1900706 A CN 1900706A CN 200610042932 CN200610042932 CN 200610042932 CN 200610042932 A CN200610042932 A CN 200610042932A CN 1900706 A CN1900706 A CN 1900706A
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 49
- 239000001301 oxygen Substances 0.000 title claims abstract description 49
- 239000003380 propellant Substances 0.000 title claims abstract description 45
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 35
- 238000002485 combustion reaction Methods 0.000 claims abstract description 49
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Abstract
含硼贫氧推进剂热值测试装置，为了克服现有技术中含硼贫氧推进剂不能充分燃烧和氧弹部件被烧蚀的缺陷，本发明采用一个厚壁容器弹体1，弹头2上有放气阀门3，电极4，充气阀6，电极4和弹头2绝缘，充气阀6和电极4之间连接点火丝10，点火丝10采用已知热值的金属丝，样品11通过点火丝10缠绕悬挂在氧弹中，样品离开坩埚一定距离，坩埚12放在坩埚架13上，坩埚架13放在氧弹的底部，支撑坩埚12。坩埚12上放置规定质量的已知热值的助燃剂。本发明通过坩埚上的助燃剂保障了贫氧推进剂的完全燃烧，同时由于高热值的贫氧推进剂没有完全在坩锅中燃烧，减小了对坩埚的烧蚀程度。
Boron-containing oxygen-poor propellant calorific value testing device, in order to overcome the defects in the prior art that boron-containing oxygen-poor propellant cannot be fully burned and oxygen bomb parts are ablated, the present invention adopts a thick-walled container projectile body 1, and the warhead 2 There are deflation valve 3, electrode 4, inflation valve 6, electrode 4 is insulated from warhead 2, ignition wire 10 is connected between inflation valve 6 and electrode 4, ignition wire 10 is a metal wire with known calorific value, and sample 11 passes through the ignition wire 10 is wound and suspended in the oxygen bomb, the sample is a certain distance away from the crucible, the crucible 12 is placed on the crucible frame 13, and the crucible frame 13 is placed at the bottom of the oxygen bomb to support the crucible 12. A combustion accelerant of known calorific value with a specified mass is placed on the crucible 12 . The invention ensures the complete combustion of the oxygen-poor propellant through the combustion aid on the crucible, and at the same time reduces the ablation degree of the crucible because the oxygen-poor propellant with high calorific value does not completely burn in the crucible.
Description
(一)所属技术领域(1) Technical field
本发明涉及一种热值测量装置，尤其是应用于推进剂、煤炭、石油化工和电力行业中推进剂、煤、油或其它发热物质之发热量的测定仪器。The invention relates to a calorific value measuring device, in particular to an instrument for measuring the calorific value of propellant, coal, oil or other exothermic substances in propellant, coal, petrochemical and electric power industries.
(二)背景技术(2) Background technology
现有技术领域里，测定物质发热量的仪器中经常采用氧弹式热量计，其中样品燃烧室也就是通常所说的氧弹，氧弹包括弹体1，弹头2，放气阀门3，电极4，坩埚架5，进气阀6，充气管7，燃烧挡板8，坩埚9。氧气通过进气阀6和充气管7进入氧弹，燃烧后的气体由放气阀门3排出，电极4和弹头2之间绝缘，另一电极由进气阀门6和充气管7兼作。样品放在坩埚9中，试验时，通电点火，使样品在富氧环境中充分燃烧。对于含硼贫氧推进剂，其中单质硼的熔点和沸点很高(分别为2430K和2823K)，硼的燃烧是一种固相和气相介质间的燃烧，相对于气相介质间的燃烧要慢的多，硼粒子表面包覆有由于硼氧化形成的B2O3，其沸点较高(约2133K)，如果燃烧温度不够高，熔化而变得粘稠的B2O3阻碍了氧气向硼与液态氧化层界面的扩散，导致硼粒子点火燃烧滞后(困难)。含硼贫氧推进剂在坩埚中燃烧时，在周围氧气气氛中，首先是可气化的黏合剂体系和低燃点的金属添加剂迅速燃烧放出大量的热，推进剂局部达到很高的温度，同时硼等高燃点的金属添加剂也开始燃烧，随着含硼贫氧推进剂中易燃组份的迅速燃烧，氧弹式量热计作为一个导热性能很好的热交换系统，其中的热量迅速散失，温度降至2133K以下，导致硼氧化生成的B2O3不能汽化而是包覆在硼表面，阻碍了氧气向硼与液态氧化层界面的扩散，使部分硼在现有量热计的氧弹中不能完全燃烧，燃烧放出的热量不是该含硼推进剂的燃烧热。同时，含硼贫氧推进剂的热值很高，为30MJ/Kg以上，且金属含量高，燃温高，使氧弹的部件严重烧蚀，尤其是坩埚9和坩埚架5。In the prior art, oxygen bomb calorimeters are often used in instruments for measuring the calorific value of substances, wherein the sample combustion chamber is also commonly referred to as an oxygen bomb. 4. Crucible frame 5, intake valve 6, gas charging tube 7, combustion baffle 8, crucible 9. Oxygen enters the oxygen bomb through the intake valve 6 and the inflation tube 7, the gas after combustion is discharged by the deflation valve 3, the electrode 4 is insulated from the
(三)发明内容(3) Contents of the invention
为了克服现有技术中含硼贫氧推进剂不能充分燃烧的缺陷，本发明采用了一种新的热值测试装置，能够有效的保障贫氧推进剂的完全燃烧。In order to overcome the defect that the boron-containing oxygen-poor propellant cannot be fully burned in the prior art, the present invention adopts a new calorific value testing device, which can effectively ensure the complete combustion of the oxygen-poor propellant.
本发明包括弹体1，弹体是一个厚壁容器；弹头2上有放气阀门3，电极4，充气阀6，电极4和弹头2绝缘，其特征在于：充气阀6和电极4之间连接点火丝10，点火丝10采用已知热值的金属丝，样品11通过点火丝10缠绕悬挂在氧弹中，样品离开坩埚一定距离，坩埚12放在坩埚架13上，坩埚架13放在氧弹的底部，支撑坩埚12。坩埚12上放置规定质量的已知热值的助燃剂。The present invention comprises projectile body 1, and projectile body is a thick-walled container;
本发明工作时，两电极间施加12～24V直流电压，点火丝通电加热使贫氧推进剂点火燃烧，样品用量为0.5g～1.5g的含硼贫氧推进剂的点火燃烧是在悬空状态，集中放热，燃速较慢的金属粒子在悬空状态不能完全燃烧；燃烧若干时间后，点火丝自行烧断，贫氧推进剂随后掉到坩埚上，引燃助燃剂，在助燃剂集中放热的作用下，使金属粒子又处于高温环境，得以完全燃烧。在这个过程中，高热值高燃温的贫氧推进剂没有直接在坩埚中燃烧，而是助燃剂在坩埚中燃烧，助燃剂的燃温为2000～3000K，远远低于贫氧推进剂的燃温，使坩埚烧蚀程度大大减小。坩埚支架不直接与火焰接触，并通过坩埚得到一定的保护，克服了氧弹部件烧蚀严重的问题。When the present invention works, a 12-24V DC voltage is applied between the two electrodes, and the ignition wire is energized and heated to ignite and burn the oxygen-poor propellant. The ignition and combustion of the boron-containing oxygen-poor propellant with a sample dosage of 0.5g to 1.5g is in a suspended state. Concentrated heat release, metal particles with a slow burning rate cannot be completely burned in the suspended state; after burning for a certain period of time, the ignition wire will burn out by itself, and the oxygen-poor propellant will then fall onto the crucible, igniting the combustion accelerant, and concentrated heat release in the combustion accelerant Under the action of the metal particles in a high temperature environment, they can be completely burned. In this process, the oxygen-depleted propellant with high calorific value and high combustion temperature is not directly burned in the crucible, but the combustion accelerant is burned in the crucible. The combustion temperature greatly reduces the degree of crucible ablation. The crucible support is not directly in contact with the flame, and is protected by the crucible, which overcomes the problem of severe ablation of oxygen bomb components.
作为本发明的一项优选方案，所述的氧弹也可以不采用坩埚12及坩埚支架13，助燃剂直接放置在氧弹的底部，适当加大助燃剂的用量。施加点火信号之后，点火丝引燃待测样品，点火丝自行烧断，贫氧推进剂随后掉到燃烧室底部，助燃剂燃烧。贫氧推进剂的点火燃烧是在悬空状态，集中放热，燃速较慢的金属粒子在悬空状态不能完全燃烧，在重力的作用下，掉入其下方的助燃剂中，引燃助燃剂，在助燃剂集中放热的作用下，使金属粒子又处于高温环境，得以完全燃烧。由于没有使用坩埚10及坩埚支架11，因此不存在坩埚及其支架的烧蚀问题。As a preferred solution of the present invention, the oxygen bomb may not use the
作为本发明的另一个优选方案，所述的样品离开坩埚的距离不小于10mm。As another preferred solution of the present invention, the distance between the sample and the crucible is not less than 10 mm.
作为本发明的第三个优选方案，所述的助燃剂可以选用双铅-2推进剂，其热值为11.2MJ/kg；也可选用改性双基推进剂171-25，热值为10.9MJ/kg。助燃剂应具有一定的形状，比如外径为10mm，高度为5mm的推进剂药柱，而不应是粉末状，这样可以保障助燃剂在一定的时间内燃烧，而不是瞬间全部烧完。As the third preferred solution of the present invention, the described combustion aid can be selected from double lead-2 propellant, and its calorific value is 11.2MJ/kg; it can also be selected from modified double-base propellant 171-25, with a calorific value of 10.9 MJ/kg. The combustion aid should have a certain shape, such as a propellant grain with an outer diameter of 10 mm and a height of 5 mm, rather than a powder, so that the combustion aid can be burned within a certain period of time instead of being completely burned out in an instant.
作为本发明的第四个优选方案，所述的坩埚12为绝热耐烧蚀的碳/碳复合材料，也可选择模压烧结的钨坩埚。As a fourth preferred solution of the present invention, the
作为本发明的第五个优选方案，所述的坩埚架13为耐热防腐蚀镍铬钼合金钢上下环坩埚支架。As a fifth preferred solution of the present invention, the
本发明通过坩埚上的助燃剂保障了贫氧推进剂的完全燃烧，同时由于高热值的贫氧推进剂没有完全在坩锅中燃烧，减小了对坩埚的烧蚀程度。本发明结构简单，性能稳定可靠，具有广泛的应用前景。The invention ensures the complete combustion of the oxygen-poor propellant through the combustion aid on the crucible, and at the same time reduces the ablation degree of the crucible because the oxygen-poor propellant with high calorific value does not completely burn in the crucible. The invention has simple structure, stable and reliable performance and wide application prospect.
(四)附图说明(4) Description of drawings
图1为现有技术的氧弹式量热计的氧弹结构图Fig. 1 is the oxygen bomb structural diagram of the oxygen bomb type calorimeter of prior art
图2为本发明的样品引燃装置结构图Fig. 2 is the structural diagram of sample ignition device of the present invention
图3为本发明的氧弹式量热计的氧弹结构图Fig. 3 is the oxygen bomb structural diagram of the oxygen bomb type calorimeter of the present invention
(五)具体实施方式(5) Specific implementation methods
图2和图3展示了本发明的应用实例。Figure 2 and Figure 3 show application examples of the present invention.
实例1：本发明采用了一种新的热值测试装置，包括弹体1，弹体是容积为300毫升的厚壁圆筒；弹头2上有放气阀门3，电极4，充气阀6，电极4和弹头2绝缘，充气阀6和电极4之间连接点火丝10，点火丝为直径0.1mm的镍铬合金丝，热值为3.2J/cm。样品11为1.0g的含硼贫氧推进剂，通过点火丝10缠绕悬挂在氧弹中，样品离开坩埚的距离为15mm，坩埚12放在坩埚架13上，坩埚12为绝热耐烧蚀的碳/碳复合材料，坩埚架13为耐热防腐蚀镍铬钼合金钢上下环坩埚支架，放在氧弹的底部，支撑坩埚。坩锅12上放置规定质量的已知热值的助燃剂，助燃剂为外径为10mm，高度为5.0mm的双铅-2推进剂，其热值为11.2MJ/kg。用图3所示的氧弹测试样品的热值，坩埚和坩埚架无烧蚀现象，测得样品热值为29.85MJ/Kg，燃烧凝聚相产物为白色粉末和少量褐色烧结物。Example 1: the present invention has adopted a kind of new calorific value testing device, comprises projectile body 1, and projectile body is the thick-walled cylinder that volume is 300 milliliters; There is deflation valve 3, electrode 4, inflation valve 6 on
实例2：本发明包括弹体1，弹体是容积为300毫升的厚壁圆筒；弹头2上有放气阀门3，电极4，充气阀6，电极4和弹头2绝缘，充气阀6和电极4之间连接点火丝10，点火丝为直径0.1mm的镍铬合金丝，热值为3.2J/cm。样品11为0.5g的含硼贫氧推进剂，通过点火丝10缠绕悬挂在氧弹中，离开氧弹底部的距离为60mm，放在氧弹的底部助燃剂为双铅-2推进剂，其直径为50mm，高度为1.5mm。用不带坩埚和坩埚支架的氧弹测试样品的热值，测得样品热值为29.89MJ/Kg，燃烧产物为白色粉末和少量褐色烧结物。Example 2: the present invention comprises projectile body 1, and projectile body is the thick-walled cylinder that volume is 300 milliliters; There is deflation valve 3, electrode 4, inflation valve 6 on
本发明的具体实施步骤：Concrete implementation steps of the present invention:
1、经过计算，含硼贫氧推进剂的理论热值为30MJ/kg左右，若采用长沙奔特仪器有限公司生产的GR3500型氧弹式热量计，则根据标定，其水当量为15000J/K，因此，取一定量含硼贫氧推进剂(即附图3中样品11)，将其切成条块状(一般以切成小立方块状)，将其放入分析天平上精确称量。1. After calculation, the theoretical calorific value of the boron-containing oxygen-poor propellant is about 30MJ/kg. If the GR3500 oxygen bomb calorimeter produced by Changsha Bent Instrument Co., Ltd. is used, according to the calibration, its water equivalent is 15000J/K Therefore, take a certain amount of boron-containing oxygen-poor propellant (
2、量取25厘米已知热值的点火丝10，在块状待测推进剂表面环向刻划3-4道小缝，将点火丝环向缠绕嵌入小缝内，以便于悬挂可靠，也便于提高点火可靠性。再将点火丝两端接在氧弹头内的点火电极上。2. Measure the
3、称量助燃剂的质量，放入坩埚12内，再将坩埚安放在坩埚支架13上，并将二者放入氧弹。3. Weigh the mass of the combustion aid, put it into the
4、组装氧弹后，充入约1.2MPa的氧气。4. After assembling the oxygen bomb, fill it with about 1.2MPa of oxygen.
5、在已经对实验仪器系统进行调节的基础上，装上贝克曼温度计。在安装贝克曼温度计之前，需对其测量范围进行调节。通过第一步可以近似估计1g左右的推进剂能使系统温度升高约2度，因此，贝克曼温度计的测量范围应该能够满足测量的需求。观察贝克曼温度计的初始读数，以读数在1度---2度之间为宜，若高于2.5度或低于0.5摄氏度就需要调节。5. On the basis of the adjustment of the experimental instrument system, install the Beckman thermometer. Before installing a Beckmann thermometer, its measuring range needs to be adjusted. Through the first step, it can be roughly estimated that about 1g of propellant can raise the temperature of the system by about 2 degrees. Therefore, the measurement range of the Beckmann thermometer should be able to meet the measurement requirements. Observe the initial reading of the Beckman thermometer. It is advisable for the reading to be between 1 degree and 2 degrees. If it is higher than 2.5 degrees or lower than 0.5 degrees Celsius, it needs to be adjusted.
5、将氧弹放入内桶，安装点火信号线，打开控制箱电源，搅拌器和振动器开始工作。5. Put the oxygen bomb into the inner barrel, install the ignition signal line, turn on the power of the control box, and the agitator and vibrator start to work.
6、开始记录初期温度变化，待系统达到平衡后，施加点火信号，点火丝迅速点燃样品，点火丝自行烧断，样品在失去悬挂力之后，在燃烧的同时掉入其下方的坩埚中，引燃助燃剂，助燃剂燃烧释放的热量保障了氧弹中的温度处于样品的燃温之上，也即保证了样品的完全燃烧。同时记录主期温度变化，记录至系统温度不再上升并开始下降前的为止。继而开始记录末期温度变化，一般记录10---15个数据。实验结束，关闭控制箱电源。6. Start to record the initial temperature change. After the system reaches equilibrium, apply an ignition signal. The ignition wire quickly ignites the sample, and the ignition wire burns itself. The heat released by the combustion of the combustion enhancer ensures that the temperature in the oxygen bomb is above the combustion temperature of the sample, which also ensures the complete combustion of the sample. At the same time, record the temperature change in the main period until the system temperature stops rising and starts to drop. Then start to record the temperature change at the end, generally record 10---15 data. At the end of the experiment, turn off the power of the control box.
7、取出氧弹，打开排气阀放出废气。打开氧弹，观察氧弹内部，发现氧弹的内壁上附着有大量白色粉末，坩锅(实例1)或者氧弹底部(实例2)上除白色粉末外还有极少量的褐色烧结物，氧弹内部坩埚、坩埚支架完好无损，无烧蚀现象。取下剩余点火丝，测量并记录剩余点火丝长度。对凝聚相燃烧产物进行分析表明：白色粉末为B2O3和MgO的混合物，褐色烧结物为硼酸和铁的氧化物，没有找到单质硼的存在。说明含硼贫氧推进剂中的难燃金属完全燃烧了，解决了含硼贫氧推进剂燃烧热测试中的问题。7. Take out the oxygen bomb, open the exhaust valve to release the exhaust gas. Open the oxygen bomb, observe the inside of the oxygen bomb, and find that a large amount of white powder is attached to the inner wall of the oxygen bomb, and there is a small amount of brown sintered matter except the white powder on the crucible (example 1) or the bottom of the oxygen bomb (example 2). The internal crucible and crucible support of the bomb are intact and there is no ablation phenomenon. Remove the remaining ignition wire, measure and record the length of the remaining ignition wire. Analysis of the condensed phase combustion products showed that the white powder was a mixture of B 2 O 3 and MgO, the brown sintered product was boric acid and iron oxide, and no elemental boron was found. It shows that the flame retardant metal in the boron-containing oxygen-poor propellant is completely burned, which solves the problem in the combustion heat test of the boron-containing oxygen-poor propellant.
8、清洗氧弹，并进行滴定。8. Clean the oxygen bomb and perform titration.
9、实验数据的处理，采用通用方法进行数据处理。得到含硼贫氧推进剂的热值。9. The processing of experimental data adopts general methods for data processing. Obtain the calorific value of the boron-containing oxygen-poor propellant.
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