CN102519833A - Complete immersion type online vacuum stability tester - Google Patents
Complete immersion type online vacuum stability tester Download PDFInfo
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- CN102519833A CN102519833A CN201110417864XA CN201110417864A CN102519833A CN 102519833 A CN102519833 A CN 102519833A CN 201110417864X A CN201110417864X A CN 201110417864XA CN 201110417864 A CN201110417864 A CN 201110417864A CN 102519833 A CN102519833 A CN 102519833A
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Abstract
The invention relates to a complete immersion type online vacuum stability tester, which comprises a furnace body, a reactor, a vacuum unit and a temperature control unit. The reactor is completely immersed into the furnace body and communicated with the vacuum unit and a decomposed product detection unit through a sampling joint. The reactor is provided with a pressure sensor. The invention avoids the phenomenon that sublimating solid materials or volatile liquid materials are condensed on a wall of a pipeline machine at test temperatures, so as to obtain an accurate release amount of gas and scientifically evaluate the compatibility and stability of sublimating or volatile materials. The invention performs online real time measurement and continuously traces the amount of decomposed gas of a heated sample. The experimental data obtained can be used to research the compatibility and stability deeply in the mechanism aspect of thermodynamics and kinetics and master the mechanism of interaction of components so as to provide theoretical guidance for improving the stability of the energy-containing materials and improving the compatibility among the components.
Description
Technical field
The present invention relates to a kind of fiery explosive vacuum stability proving installation, belong to fiery explosive performance test ing technical field.
Background technology
Explosive stability is meant that its physics under the fiery explosive storage requirement, chemical property change the ability that is no more than allowed band; The compatibility of fire explosive is meant that its physics, chemical property change the ability that is no more than allowed band when being in contact with one another between the component relevant with the body composition.Good stability and compatibility are to estimate the burning that fiery explosive do not meet accident in production process or ammunition storage process often or the key foundation of explosion accident.The evaluation method of stability, compatibility has calorimetry, eudiometry, test paper method, mass and size rate of change method, product component analytic approach etc.Vacuum stability test is a kind of of eudiometry, with quantitative sample decomposes under constant volume, constant temperature and certain vacuum condition, estimates stability and compatibility through measuring the volume that decomposes release gas.With data by MoM and MEI, this method scope of application is wide, and sample size is moderate, and is not only representative but also guarantee safety basically, and obtain quantitative data, is a kind of method the most commonly used.Existing vacuum stability proving installation has following deficiency: 1, reactor is for partly soaking formula; The sample cell that is reactor immerses heating furnace body; The pipeline and the piston portion that connect sample cell and piston expose in air; Its wall temperature is lower than immersion part wall temperature during heating, for the solid of distillation or the fluent material of volatilization take place under the test temperature, condensation takes place on the pipeline wall; Gas burst size accurately can't be obtained, thereby the compatibility and the stability of distillation or volatile material can not be accurately estimated.2, can not monitor and changed by the gas flow of thermal process, can only obtain final total discharge quantity, can't distinguish physisorption gas and chemical reaction decomposition gas, also can't carry out deep Analysis on Mechanism.
Summary of the invention
The purpose of this invention is to provide a kind of full immersed type at line vacuum stability proving installation; It is dipped in heating furnace body entirely through the corrosion-and high-temp-resistant reactor; But and the device of online in real time measurement gas burst size and analytical gas composition; Be used for energetic material stability, compatibility evaluation and Analysis on Mechanism, to overcome the main deficiency of prior art.
Implementation procedure of the present invention:
A kind of full immersed type is at line vacuum stability proving installation; Comprise body of heater, reactor, vacuum unit and temperature control unit; It is characterized in that: reactor all immerses body of heater inside; Reactor is communicated with vacuum unit and decomposition product detecting unit through the sampling interface, and pressure transducer is installed on the reactor.
Vacuum unit is connected to form by vacuum line, stop valve, surge flask and vacuum pump successively, and the decomposition product detecting unit is connected to form by air guide pipeline, interface and gas chromatography successively, the sampling interface of reactor and vacuum line and air guide pipeline connection.Be provided with 3～8 reactors in the body of heater.The thermal conductance layer outside of body of heater is zone of heating, heat-insulation layer and housing successively, and reactor places in the thermal conductance layer bottoming hole.
Reactor includes sample cell and sampling interface, and sample cell is connected through the revolving fragment that has gas port that is arranged in the seal sleeve with the sampling interface, realizes the conducting and the released state of sample cell and sampling interface through rotating revolving fragment.The seal sleeve dividing plate is divided into lower chamber and upper cavity with sleeve, and upper cavity is connected with the sampling interface with revolving fragment successively, and lower chamber is connected with sample cell, has gas port and pressure tap on the seal sleeve dividing plate.
Said body of heater is made up of heat-conducting layer, zone of heating, thermofin, shell, solid-state relay, temperature controller etc.Heat-conducting layer is provided with 3～8 bottoming holes, and temperature receives temperature control unit and computer control in the hole.
The seal sleeve dividing plate at seal sleeve middle part is divided into upper cavity and lower chamber with sleeve, and the seal sleeve two ends are internal thread, sample cell is connected with the interface of sampling and seals through elements such as rotation nut and pad and sealing gaskets.The seal sleeve dividing plate is provided with force samples hole, chromatogram thieff hatch, pressure transducer mounting hole (lateral aperture) in vertical direction, and the sleeve lateral wall of seal sleeve dividing plate top is provided with the rectangle horizontal through hole of two symmetries, be used for through and rotate turning handle.
Revolving fragment is a right cylinder, and sidewall has two symmetrical lateral apertures, is used to install turning handle, runs through revolving fragment from the horizontal by the gas port at 60 ° of angles.
Sampling interface lower port is provided with the abduction edge, conveniently is connected with seal sleeve, and port is the pagoda interface.Reacting sample cell port abduction adds gasket seal and is connected with seal sleeve dividing plate lower surface along the upper surface, the port abduction adds gasket seal and is anchored on the seal sleeve lower chamber with nut along the lower end.
Revolving fragment places seal sleeve dividing plate upper surface, and chromatogram sampling interface abduction adds gasket seal along bottom face and links to each other with revolving fragment, and chromatogram sampling interface abduction adds gasket seal and is anchored on the seal sleeve lower chamber with nut along the upper surface.
Said vacuum unit contains vacuum line, stop valve, surge flask and vacuum pump.Reactor links to each other with vacuum pump with surge flask through vacuum line, is provided with stop valve between reactor and the surge flask; Said gaseous tension detecting unit contains high-precision micro pressure transducer and atmospheric pressure transmitter, and the high-precision micro pressure transducer is installed on the pressure transducer mounting hole of seal sleeve, and the atmospheric pressure transmitter places intensification heating unit outside.
Said reactor unit is connected with special purpose interface through the air guide pipeline, and special purpose interface is connected with gas chromatography, and the data from gas chromatography analysis is by computer control.Computing machine is equipped with data collecting card, graphic presentation control and data processing unit, and data processing unit comprises data acquisition module, data memory module, graphical module, data analysis module and system management module.Pressure-time array that data acquisition module obtains temperature thermocouple output in real time through data collecting card temperature-time array and pressure transducer are exported also is deposited in the data memory module; Graphical module is called data and the graphic presentation control in the data memory module, and temperature-time array and pressure-time array are changed into the time dependent relation curve of gas flow under the test temperature; The test parameters that system management module is imported according to manual work is controlled the heating rate of said calandria, accomplishes user management and printout simultaneously.
Advantage of the present invention and beneficial effect:
1, the full immersed type of reactor unit design; Solid or the volatile fluent material generation condensation of having avoided being prone under the test temperature distillation are on the pipeline wall; Thereby obtain gas burst size accurately, the compatibility and the stability of scientific evaluation distillation or volatile material;
2, online in real time is measured; Realized the Continuous Tracking of the decomposition gas amount of heating sample; The experimental data that obtains can be from the mechanism aspect further investigation compatibility and the stability of thermodynamics and kinetics; Grasp component interaction mechanism is for improving the energetic material stability, improving group partition inter-capacitive theoretical direction is provided;
3, the pressure of decomposition gas generation is 0.02～0.03MPa, decomposition product detecting unit equipment gas chromatography, but measurement gas is formed the Continuous Tracking of the decomposition gas composition of online in real time measurement heating sample;
4, mostly the energetic material decomposition product is NO
x , ClO
4 -, CO
x , NH
4 +Etc. structure, meet H
2Acidity or alkaline product that O forms, at high temperature very corrosive is damaged sensor.High-precision sensor adopts craft of gilding, has realized corrosion-resistantly, has guaranteed the test accuracy of sensor, and has improved sensor serviceable life.
5, reacting sample cell is corrosion-resistant material (glass or a stainless steel), the corrosion of ability acid resistance or alkaline decomposition product, and sealing gasket adopts polytetrafluoroethylmaterial material, the impermeability under the warranty test temperature, the design of realization response device full immersed type.
Description of drawings
Fig. 1 is that full immersed type of the present invention is at line vacuum stability proving installation structural representation;
Fig. 2 is the structure of reactor synoptic diagram;
Reference numeral is expressed as among the figure:
1-gas chromatography, 2-interface, 3-air guide pipeline, 4-vacuum line
5-stop valve, 6-surge flask, 7-vacuum pump, 8-computing machine
9-thermal conductance layer, 10-reactor, 12-temperature sensor, 13-zone of heating
14-solid-state relay, 15-temperature controller, 16-housing
17-heat-insulation layer 19-last heat insulating mattress 20-upper cover plate
21-reacting sample cell, 22-underspin turn nut, 23-seal sleeve
24-go up sealing gaskets 25-on rotate nut 26-sampling interface
27-revolving fragment, 28-Upper gasket, 29-rotary handle
30-pressure transducer, 31-lower seal pad, 32-lower gasket.
Embodiment
Below in conjunction with accompanying drawing the present invention is made further detailed description.
Shown in Fig. 1 to 2, full immersed type provided by the invention comprises body of heater, reactor, vacuum unit, gaseous tension detecting unit, decomposition product detecting unit and computing machine at line vacuum stability proving installation.
Body of heater comprises upper cover plate 20, goes up heat insulating mattress 19, thermal conductance layer 9, zone of heating 13, heat-insulation layer 17, housing 16, temperature sensor 12, solid-state relay 14, temperature controller 15.Thermal conductance layer 9 is the right cylinders that process with the good aluminium alloy of thermal conductivity, is evenly distributed with 6 bottoming holes on its end face on the same circumference.Zone of heating 13 is the column type heating jacket, adopts the winding mode, and heater strip is the nickel-cadmium material, and after the uniform winding, the corrosion resistant plate thick with 2mm encapsulates.Add magnesium oxide at two ends and carry out insulation processing, zone of heating 13 lock rings are on the cylinder of thermal conductance layer 9.The heat-insulation layer made from the aluminosilicate fiberboard felt 17 is housed in the space between zone of heating 13 and the housing 16.Housing 16 adopts stainless steel.The disc heat shield that last heat insulating mattress 19 is processed for aluminosilicate fiberboard; Last heat insulating mattress 19 is installed in the upper surface of thermal conductance layer 9 and heat-insulation layer 17; Wherein go up heat insulating mattress 19 be evenly distributed with on the same circumference with thermal conductance layer 9 on the bottoming hole concentric hole, be used for through reactor.Upper cover plate 20 adopts stainless steel to process.And fixing through screw and housing 16,6 temperature sensors 12 lay respectively at the bottom of 6 bottoming holes and pass housing 16, are connected with temperature controller 15 with the signal shielding line.Zone of heating 13 adopts high temperature resistant wire to be connected with solid-state relay 14, and solid-state relay 14 is connected with temperature controller 15, and temperature controller 15 is connected with computing machine 8.Temperature sensor 12 adopts RTD, and model is Pt100, four-wire system.
Reactor contains reacting sample cell 21, underspin turn nut 22, seal sleeve 23, last sealing gasket 24, on rotate nut 25, chromatogram sampling interface 26, revolving fragment 27, Upper gasket 28, rotary handle 29, pressure transducer 30, lower seal pad 31, lower gasket 32.
The seal sleeve dividing plate at seal sleeve 23 middle parts is divided into lower chamber and upper cavity with sleeve; Lower chamber and upper cavity two ends are respectively equipped with internal thread; The abduction of sample cell 21 is along top installation lower seal pad 31; Abduction is along following installation lower gasket 32, and is connected with seal sleeve 23 through underspin turn nut 22.The high temperature resistant silica gel of pressure transducer 30 usefulness is encapsulated in the lateral aperture of seal sleeve 23.Install pad 28 above the abduction edge of chromatogram sampling interface 26, abduction is installed sealing gasket 24 below the edge, and is connected with seal sleeve 23 through last rotation nut 25.
Revolving fragment 27 materials are teflon, diameter Ф 32mm, and thick 6mm, two symmetrical lateral aperture diameter Ф 4mm of sidewall, dark 6mm, the rotary handle 29 that is used to pack into, the gas port diameter Ф 3mm on the revolving fragment 27 becomes 60 ° of angles with level; Last sealing gasket 24 materials are teflon, internal diameter Ф 13mm, external diameter Ф 30mm, thick 3mm; Upper gasket 28 is the rubber material, internal diameter Ф 16mm, external diameter Ф 30mm, thick 3mm; Last rotation nut 25 is M32 * 20mm.
Vacuum unit comprises vacuum line 4, stop valve 5, surge flask 6 and vacuum pump 7 (2XZ-1 type sliding vane rotary vacuum pump); Chromatogram sampling interface 26 links to each other with vacuum pump 7 with surge flask 6 through vacuum line 4, is provided with stop valve 5 between reactor chromatogram interface 26 and the surge flask 6.
The gaseous tension detecting unit contains high-precision micro pressure transducer and atmospheric pressure transmitter (JQYB-A type), and the high-precision micro pressure transducer is built in the standard reaction device, and the atmospheric pressure transmitter places intensification heating unit outside.
The decomposition product detecting unit contains air guide pipeline 3, interface 2 and gas chromatography 1, and chromatogram sampling interface 26 is connected with interface 2 through air guide pipeline 3, and interface 2 is connected with gas chromatography 1, and the data from gas chromatography analysis is by computing machine 8 controls.
Computing machine 8 is equipped with data acquisition equipment (XSLE series) gathers the temperature-time data of various environmental parameters, temperature thermocouple output and the pressure-time data of pressure transducer output etc. in real time.Temperature controller (WEST 4100) is controlled the temperature and the heating process of heating furnace.Computer software partly comprises: the real time data acquisition module, be responsible for gathering in real time each association; Data memory module is responsible for the storage and the management of real-time image data; The environmental change curve that graphical data display module, real-time exhibition collect, temperature-time changing curve, pressure-time changing curve etc.; Data analysis and processing module; Be responsible for temperature-time data and pressure-time data are changed into the time dependent relation curve of gas flow under the test temperature; And each item work of treatment of experimentizing, each item character of laboratory sample is provided analysis result, report output work; Temperature control modules according to requirement of experiment, is controlled the temperature of heating furnace, guarantees constant temperature, the intensification requirement of experiment to temperature; System management module is accomplished the setting and the management work of user management and system's parameters.
When 6 reactors are equipped with different tested gunpowder; The pressure signal acquisition component can be gathered the output of 6 pressure transducers simultaneously; Set up the pressure-time array of 6 correspondences, computing machine is handled data, and shows corresponding pressure-time-temperature curve in real time; Through data processing and analysis, the character and the characteristics of 6 kinds of tested gunpowder are made evaluation at last.
Following enumeration method of application of the present invention:
(1) relevant parameters such as furnace temp, pressure transducer acquired signal time is set.
(2) sample that national military standard GJB 772A-97 method 501.2 was handled has been pressed in weighing, packs in the reacting sample cell with funnel, and sample is added a little absorbent cotton by suck-back at the reacting sample cell mouth when preventing to vacuumize, or a little test paper.
(3) reactor the first half is installed.In seal sleeve, put into successively revolving fragment, on sealing gasket, chromatogram sampling interface, Upper gasket, install rotary handle from the side, use the rotation nut screwing clamping, handle is rotated to the position that gas port is opened.
(4) assembling reactor.Seal sleeve is vertically placed, put into lower seal pad, reacting sample cell, lower gasket successively from below, slowly tighten with the underspin turn nut.
(5) vacuum tube connects chromatogram sampling interface, opens vacuum pump and vacuumizes, and the gaseous tension signal changes in the software observes reactor.
(6) select experiment type.1. during the continuous coverage of decomposition gas amount; Gaseous tension is decreased to steady state value when (at least 10 minutes pumpdown times) in the question response device; Slowly the rotary handle on the rotational response device is closed gas port, then closes vacuum pump, breaks off being connected of vacuum tube and chromatogram sampling interface; 2. decomposition gas form continuous coverage the time, gaseous tension is decreased to steady state value when (at least 10 minutes pumpdown times) in the question response device, the stop valve on blinding off a line is then closed vacuum pump, opens the professional interface that connects gas chromatograph.
(7) unload rotary handle on the reactor, stove to be heated is constant to design temperature, and reactor is put into heating furnace and covered bell.
(8) gas flow that sample discharges in the observing response device is according to the stability or the compatibility of standard rating sample.
Claims (8)
1. a full immersed type is at line vacuum stability proving installation; Comprise body of heater, reactor, vacuum unit and temperature control unit; It is characterized in that: reactor all immerses body of heater inside; Reactor is communicated with vacuum unit and decomposition product detecting unit through the sampling interface, and pressure transducer is installed on the reactor.
2. full immersed type according to claim 1 is at line vacuum stability proving installation; It is characterized in that: vacuum unit is connected to form by vacuum line, stop valve, surge flask and vacuum pump successively; The decomposition product detecting unit is connected to form by air guide pipeline, interface and gas chromatography successively, the sampling interface of reactor and vacuum line and air guide pipeline connection.
3. full immersed type according to claim 2 is characterized in that at line vacuum stability proving installation: be provided with 3～8 reactors in the body of heater.
4. full immersed type according to claim 3 is characterized in that at line vacuum stability proving installation: the thermal conductance layer outside of body of heater is zone of heating, heat-insulation layer and housing successively, and reactor places in the thermal conductance layer bottoming hole.
5. full immersed type according to claim 1 is at line vacuum stability proving installation; It is characterized in that: the sample cell of reactor is connected through the revolving fragment that has gas port that is arranged in the seal sleeve with the sampling interface, realizes the conducting and the released state of sample cell and sampling interface through rotating revolving fragment.
6. full immersed type according to claim 5 is at line vacuum stability proving installation; It is characterized in that: the dividing plate of seal sleeve is divided into lower chamber and upper cavity with sleeve; Upper cavity is connected with the sampling interface with revolving fragment successively; Lower chamber is connected with sample cell, has gas port and pressure tap on the seal sleeve dividing plate.
7. full immersed type according to claim 6 is characterized in that at line vacuum stability proving installation: chromatogram sampling interface lower port is provided with the abduction edge, and port is the pagoda interface.
8. full immersed type according to claim 5 is characterized in that at line vacuum stability proving installation: revolving fragment is a right cylinder, and sidewall has two symmetrical lateral apertures, is used to install turning handle, runs through revolving fragment from the horizontal by the gas port at 60 ° of angles.
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|---|---|---|---|
| CN201110417864XA CN102519833A (en) | 2011-12-15 | 2011-12-15 | Complete immersion type online vacuum stability tester |
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|---|---|---|---|
| CN201110417864XA CN102519833A (en) | 2011-12-15 | 2011-12-15 | Complete immersion type online vacuum stability tester |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103076354A (en) * | 2012-12-28 | 2013-05-01 | 中国工程物理研究院化工材料研究所 | Automatic test system and method for vacuum stability |
| CN104406968A (en) * | 2014-11-25 | 2015-03-11 | 山西北方兴安化学工业有限公司 | Chemical stability detection method for nitroglycerin-containing product |
| CN104931384A (en) * | 2015-06-26 | 2015-09-23 | 四川省科源工程技术测试中心 | Vacuum metering device |
| CN105588854A (en) * | 2016-02-26 | 2016-05-18 | 中国计量学院 | Quick temperature scanning screening calorimeter |
| CN106769643A (en) * | 2016-12-05 | 2017-05-31 | 西南科技大学 | A kind of new equipment for determining energetic material Isothermal Hot decomposition gas quantity |
| CN106872662A (en) * | 2017-02-09 | 2017-06-20 | 西安近代化学研究所 | The device that a kind of thermostability of explosive wastewater powder column is continuously measured |
| CN108896495A (en) * | 2018-09-14 | 2018-11-27 | 贵州电网有限责任公司 | A kind of environmental protection insulating gas and metal phase capacitive experiment simulator and test method |
| CN109085271A (en) * | 2018-09-07 | 2018-12-25 | 中国工程物理研究院化工材料研究所 | A kind of small pit goaf thermal explosion gas collector and analysis method for gases |
| CN110646459A (en) * | 2019-10-14 | 2020-01-03 | 中国工程物理研究院化工材料研究所 | Compatibility evaluation method of tetrazole-based energetic material based on gas product |
| CN112067649A (en) * | 2020-08-24 | 2020-12-11 | 西安近代化学研究所 | Explosive vacuum stability test device |
| CN113295060A (en) * | 2021-05-20 | 2021-08-24 | 中国工程物理研究院化工材料研究所 | Unattended vacuum stability test equipment, system and method |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103076354A (en) * | 2012-12-28 | 2013-05-01 | 中国工程物理研究院化工材料研究所 | Automatic test system and method for vacuum stability |
| CN104406968A (en) * | 2014-11-25 | 2015-03-11 | 山西北方兴安化学工业有限公司 | Chemical stability detection method for nitroglycerin-containing product |
| CN104931384A (en) * | 2015-06-26 | 2015-09-23 | 四川省科源工程技术测试中心 | Vacuum metering device |
| CN105588854A (en) * | 2016-02-26 | 2016-05-18 | 中国计量学院 | Quick temperature scanning screening calorimeter |
| CN105588854B (en) * | 2016-02-26 | 2018-12-07 | 中国计量学院 | Fast temperature scanning screening calorimeter |
| CN106769643A (en) * | 2016-12-05 | 2017-05-31 | 西南科技大学 | A kind of new equipment for determining energetic material Isothermal Hot decomposition gas quantity |
| CN106872662A (en) * | 2017-02-09 | 2017-06-20 | 西安近代化学研究所 | The device that a kind of thermostability of explosive wastewater powder column is continuously measured |
| CN106872662B (en) * | 2017-02-09 | 2019-02-12 | 西安近代化学研究所 | A kind of device that the thermostability of explosive wastewater powder column continuously measures |
| CN109085271A (en) * | 2018-09-07 | 2018-12-25 | 中国工程物理研究院化工材料研究所 | A kind of small pit goaf thermal explosion gas collector and analysis method for gases |
| CN109085271B (en) * | 2018-09-07 | 2021-06-22 | 中国工程物理研究院化工材料研究所 | Small-dose thermal explosion gas collecting device and gas analysis method |
| CN108896495A (en) * | 2018-09-14 | 2018-11-27 | 贵州电网有限责任公司 | A kind of environmental protection insulating gas and metal phase capacitive experiment simulator and test method |
| CN108896495B (en) * | 2018-09-14 | 2024-04-12 | 贵州电网有限责任公司 | Environment-friendly insulating gas and metal compatibility test simulation device and test method |
| CN110646459A (en) * | 2019-10-14 | 2020-01-03 | 中国工程物理研究院化工材料研究所 | Compatibility evaluation method of tetrazole-based energetic material based on gas product |
| CN110646459B (en) * | 2019-10-14 | 2021-12-17 | 中国工程物理研究院化工材料研究所 | Compatibility evaluation method of tetrazole-based energetic material based on gas product |
| CN112067649A (en) * | 2020-08-24 | 2020-12-11 | 西安近代化学研究所 | Explosive vacuum stability test device |
| CN112067649B (en) * | 2020-08-24 | 2023-08-11 | 西安近代化学研究所 | Device for testing vacuum stability of explosives and powders |
| CN113295060A (en) * | 2021-05-20 | 2021-08-24 | 中国工程物理研究院化工材料研究所 | Unattended vacuum stability test equipment, system and method |
| CN113295060B (en) * | 2021-05-20 | 2022-11-15 | 中国工程物理研究院化工材料研究所 | Unattended vacuum stability test equipment, system and method |
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Application publication date: 20120627 |