CN106610391A - Energetic material flash point test method and equipment thereof - Google Patents
Energetic material flash point test method and equipment thereof Download PDFInfo
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Abstract
The invention relates to an energetic material flash point test method and equipment thereof. The method comprises the steps of placing an energetic material to be tested into an inner sample tank, and placing the inner sample tank into an outer sample tank; placing the outer sample tank on a heater; forming a test system through the heater, the sample tanks, a temperature sensor, a flash fire detection ring and a test module jointly, wherein the test module is connected with a control module through a data flat cable. The test system is separated from the control module, and the test system and the control module are separately arranged in different rooms and are separated through an explosion-proof wall. By means of separation operation and reducing the test sample amount, the energetic material flash point test is achieved; the essential security of a test process is improved through separated operation and by reducing the test sample amount, the casualty in a dangerous process is effectively avoided, and the damage to the equipment in the test process is also effectively reduced.
Description
Technical field
The present invention relates to a kind of method of testing, more particularly to energetic material flash-point method of testing.
Background technology
Flash-point is one of safe practice index of flammable liquid material, shows that it occurs burning or the possibility size exploded, and to transport, is stored and significant using the security protection of process.The partially liq raw material of liquid propellant, solid propellant（Such as nitric acid ester adhesive）Boiling point is relatively low, volatility is larger, and its flash-point is relatively low, in atmosphere occur burning or explode it is dangerous larger, hydrocarbon fuel, excipient propellant etc. are also required for carrying out flash-point test.In view of energetic material fires danger, yet there are no energetic material flash-point method of testing, measuring technology and instrument and equipment pertinent literature report, energetic material flash-point method of testing is manual operation face-to-face, because without special equipment, still tested using big dose, very big danger is brought to personnel and equipment.
The content of the invention
It is an object of the invention to overcome the drawbacks described above of prior art, a kind of energetic material flash-point method of testing is set up, by isolated operation and reduction two technological approaches of dose, solve the manual operation face-to-face and big dose dangerous problem next to personnel and equipment belt.
The present invention also provides the special equipment of above-mentioned energetic material flash-point method of testing.
Above-mentioned purpose of the present invention is achieved by following technical solution：Test system is separated with control module, different rooms are individually positioned in, centre is isolated by blast wall, there is explosion-proof observation window on blast wall, and by observation window specimen reaction situation is observed, to take necessary fire protection to reduce the infringement to test module.
Comprise the following steps that：
（1）Energetic material to be measured is placed in interior sample cell, the surface concave of energetic material to be measured is concordant with graduation mark；
（2）Interior sample cell is placed in outer sample cell；
（3）Outer sample cell is positioned on heater，Heater is heated by heating wire，Heater is connected by winding displacement with control module，Foundation estimates flash-point value design temperature，Heating mode is 14 DEG C/min ~ 17 DEG C/min for heating rate when beginning to warm up，Reach heating rate when flash-point estimates 56 DEG C before temperature and be reduced to 5 DEG C/min ~ 6 DEG C/min，Until estimating 20 DEG C of temperature higher than flash-point，Design temperature and heating mode are realized by control module，Flash temperature is recorded by temperature sensor，Temperature sensor is inserted perpendicularly in energetic material to be measured during test，Temperature sensor is suspended in metallic rod，Metallic rod is placed in parallel with heater，Temperature sensor is connected by data wire with test module，Test module passes through winding displacement link control module，The steam scintillation phenomenon under flame interaction that evaporates detects ring test by scintillation，Detection ring is annular，Built-in thermoelectric hinders，When steam generation scintillation，Thermal resistance resistance under flame temperature effect can change，Change in resistance is converted to the change of voltage and feeds back to control module by test module，After receiving voltage change signal，Control module sends stopping heating instructions to test module，And temperature value of recording voltage when changing，Complete scintillation detection process，Scintillation detection ring is suspended in the metallic rod for placing temperature sensor，By data wire connecting test module，Test module is connected to control module by winding displacement，Heater parameter is arranged and temperature test result is achieved by the read out instrument of control module，Also result can be printed out by the printer being connected with control module.Heater, sample cell, temperature sensor, scintillation detection ring and test module collectively constitute test system, test module is connected by data flat cable with control module, isolated by blast wall, test system is placed in blast wall one side during test, control module is placed in the other one side of blast wall.When flash-point is tested, it is a certain temperature first to preset flash-point value, air intake valve is opened, flame height 3mm～5mm is adjusted, starts flash-point test, flash-point arranges value is reduced when preset temperature is higher than flash-point value, and treat measuring cup to cool down next time to be tested, preset temperature can directly reset flash-point value when being less than flash-point value, continue to heat, until measuring flash-point value, that is, observe flash-point.After observation flash-point detection, normal atmosphere pressure, the as flash-point of the energetic material are adapted to by following formula；
Tc=T0+0.25（101.3-p）
In formula：
Tc- flash-point, DEG C；
T0- observation flash-point, DEG C；
P- ambient atmosphere pressures, kPa.
The special equipment of energetic material flash-point method of testing of the present invention, including scintillation detection ring, temperature sensor, for the interior sample cell for filling energetic material to be measured and the outer sample cell that is positioned on heater, interior sample cell is placed in outer sample cell, temperature sensor, scintillation detection ring be suspended on respectively equipped with energetic material to be measured interior sample cell top, also including a collecting temperature sensor signal and by the signal transmission to control module, collection scintillation detection ring signal and by the signal transmission to control module test module；Also include a setting heter temperature and heating mode, receive the signal displays temperature test result of test module, show scintillation testing result and heater heating is sent to test module or stop the control module of heater heating instructions；The scintillation detection ring is annular, built-in thermoelectric hinders, when steam generation scintillation, thermal resistance resistance under flame temperature effect can change, change in resistance is converted to the change of voltage and feeds back to control module by test module, and after receiving voltage change signal, control module sends stopping heating instructions to test module, and temperature value of recording voltage when changing, complete scintillation detection process.
Present invention additionally comprises a printer being connected with control module.
The present invention carries out isolated operation by the way that control module is separated with test module, is controlled and data transfer by data line connection between two parts, and signal and data transfer also can be realized by bluetooth.Control signal is transmitted respectively with test data by the way that Bluetooth transmission signal is appropriate to the occasion.
Interior sample cell external diameter of the present invention is less than outer sample cell internal diameter, interior sample cell and outer sample cell tight fit.
By processing sample cell in little volume, the reduction of test process amount of samples is realized, in processing during sample cell on the premise of temperature sensor and detection ring diameter is considered, its diameter should be as little as possible.
Interior sample cell of the present invention（Little volume measuring cup）It can be a series of 3～5, each interior sample cell external diameter is identical, and internal diameter is sequentially reduced.It is easy to investigate impact of the sample size to flash-point, it is adaptable to the test of the energetic material flash-point with different degrees of danger, the less interior sample cell of dangerous larger appropriate to the occasion selection volume.
The applicable energetic material of the method for testing include the raw material such as liquid propellant, liquid fire/explosive, propellant, fire/explosive energetic binder and other have volatile solid energetic material.
The present invention is using isolated operation and reduces test specimen consumption, improves test process safety, it is ensured that tester's life security, effectively reduces infringement of the test process to equipment.
The present invention has the advantage that compared to existing technology：
（1）The present invention realizes first the flash-point test of the energetic material class sample for firing danger；
（2）The present invention reduces the danger of manual operation face-to-face by isolated operation, effectively reduces the injury of burning, blast and toxicity to operating personnel；
（3）Present invention scope on probation is wide; it is applicable not only to liquid propellant, liquid fire/explosive; the raw material such as propellant, fire/explosive energetic binder and other have volatile solid energetic material flash-point to test, it may also be used for the flash-point test of the harmful influence with certain toxicity.
（4）The method of testing of the present invention can provide flash-point data for energetic material, be easy to be better understood by energetic material self-characteristic, can provide guidance for its application.
Description of the drawings
Fig. 1 is the special equipment structural representation of the present invention.
Fig. 2 is the equipment schematic block diagram of the present invention.
In figure, sample cell in 1-, the outer sample cells of 2-, 3- temperature sensors, 4- scintillations detection ring, 5- test modules, 6- heaters, 7- control modules, 8- printers.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is further detailed explanation with specific embodiment, but the present invention is not limited only to the example.
In Fig. 1, Fig. 2, the present invention includes scintillation detection ring 4, temperature sensor 3, for the interior sample cell 1 for filling energetic material to be measured and the outer sample cell 2 that is positioned on heater 6, interior sample cell 1 is placed in outer sample cell 2, temperature sensor 3, scintillation detection ring 4 is suspended on respectively the top of the interior sample cell 1 equipped with energetic material to be measured, also including a collecting temperature sensor signal and by the signal transmission to control module, collection scintillation detection ring signal and by the signal transmission to control module test module 5；Also include a temperature of setting heater 6 and heating mode, receive the signal displays temperature test result of test module, show scintillation testing result and heater heating is sent to test module or stop the control module 7 of heater heating instructions；The scintillation detection ring 4 is annular, built-in thermoelectric hinders, when steam generation scintillation, thermal resistance resistance under flame temperature effect can change, change in resistance is converted to the change of voltage and feeds back to control module 7 by test module 5, and after receiving voltage change signal, control module 7 sends stopping heating instructions to test module 5, and temperature value of recording voltage when changing, complete scintillation detection process.
Energetic material to be measured is put into interior sample cell 1, interior sample cell 1 is put into into outer sample cell 2, outer sample cell 2 is positioned on heater 6, it is a certain temperature first to preset flash-point value, air intake valve is opened, flame height 3mm～5mm is adjusted, starts flash-point test, flash-point arranges value is reduced when preset temperature is higher than flash-point value, and treat measuring cup to cool down next time to be tested, preset temperature can directly reset flash-point value when being less than flash-point value, continue to heat, until measuring flash-point value, that is, observe flash-point.After observation flash-point detection, normal atmosphere pressure, the as flash-point of the energetic material are adapted to by following formula.
Tc=T0+0.25（101.3-p）
In formula：
Tc- flash-point, DEG C；
T0- observation flash-point, DEG C；
P- ambient atmosphere pressures, kPa.
Little volume measuring cup in the embodiment of the present invention is one group, can be divided into 1～No. 3, and its external diameter is identical, and external diameter is less than outer sample cell internal diameter, interior sample cell and outer sample cell tight fit.Little volume measuring cup size is followed successively by little volume measuring cup 1#For external diameter 30.9mm, internal diameter 15mm, little volume measuring cup 2#For external diameter 30.9mm, internal diameter 10mm, little volume measuring cup 3#For external diameter 30.9mm, internal diameter 6mm, big volume measuring cup is No. 0, and big volume measuring cup 0 is external diameter 34mm, internal diameter 31mm.
Below by the test process for enumerating several specific embodiments detailed descriptions simulating test device of the present invention：
Embodiment 1
Precise energetic material nitromethane 10ml to be measured, is positioned over interior sample cell（Little volume measuring cup 1#）In；Interior sample cell is put into into outer sample cell（Big volume measuring cup 0）In, remaining step is as described above, test result is as follows：
Embodiment 2
Precise energetic material nitroethane 5ml to be measured, is positioned over interior sample cell（Little volume measuring cup 2#）In, interior sample cell is put into into outer sample cell（Big volume measuring cup 0）In, remaining step is as described above, test result is as follows：
Embodiment 3
Precise energetic material isooctyl ester nitrate 2ml to be measured, is positioned over interior sample cell（Little volume measuring cup 3#）In, interior sample cell is put into into outer sample cell（Big volume measuring cup 0）In, remaining step is as described above, test result is as follows：
The above; the only conventional specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, any those familiar with the art the invention discloses technical scope in; the change or replacement that can be readily occurred in, all should be included within the scope of the present invention.
The content not being described in detail in description of the invention belongs to the known technology of professional and technical personnel in the field.
Claims (5)
1. a kind of energetic material flash-point method of testing, it is characterised in that：
（1）Energetic material to be measured is placed in interior sample cell;
（2）Interior sample cell is placed in outer sample cell；
（3）Outer sample cell is positioned on heater，Foundation estimates flash-point value design temperature，Heating mode is 14 DEG C/min ~ 17 DEG C/min for heating rate when beginning to warm up，Reach heating rate when flash-point estimates 56 DEG C before temperature and be reduced to 5 DEG C/min ~ 6 DEG C/min，Until estimating 20 DEG C of temperature higher than flash-point，Design temperature and heating mode are realized by control module，Flash temperature is recorded by temperature sensor，Temperature sensor is inserted perpendicularly in energetic material to be measured during test，Temperature sensor is connected by data wire with test module，Test module passes through winding displacement link control module，The steam scintillation phenomenon under flame interaction that evaporates detects ring test by scintillation，Detection ring is annular，Built-in thermoelectric hinders，When steam generation scintillation，Thermal resistance resistance under flame temperature effect can change，Change in resistance is converted to the change of voltage and feeds back to control module by test module，After receiving voltage change signal，Control module sends stopping heating instructions to test module，And temperature value of recording voltage when changing，Complete scintillation detection process，Scintillation detection ring is suspended in the metallic rod for placing temperature sensor，By data wire connecting test module，Test module is connected to control module by winding displacement，Temperature test result is achieved by the read out instrument of control module，Also result can be printed out by the printer being connected with control module；Heater, sample cell, temperature sensor, scintillation detection ring and test module collectively constitute test system, test module is connected by data flat cable with control module, isolated by blast wall, test system is placed in blast wall one side during test, control module is placed in the other one side of blast wall；
When flash-point is tested, it is a certain temperature first to preset flash-point value, air intake valve is opened, flame height 3mm～5mm is adjusted, starts flash-point test, flash-point arranges value is reduced when preset temperature is higher than flash-point value, and treat measuring cup to cool down next time to be tested, preset temperature can directly reset flash-point value when being less than flash-point value, continue to heat, until measuring flash-point value, that is, observe flash-point；
After observation flash-point detection, normal atmosphere pressure, the as flash-point of the energetic material are adapted to by following formula；
Tc=T0+0.25（101.3-p）
In formula：
Tc- flash-point, DEG C；
T0- observation flash-point, DEG C；
P- ambient atmosphere pressures, kPa.
2. the special equipment of the energetic material flash-point method of testing described in a kind of claim 1, it is characterised in that：Ring is detected including scintillation, temperature sensor, for filling the interior sample cell of energetic material to be measured, with the outer sample cell being positioned on heater, interior sample cell is placed in outer sample cell, temperature sensor, scintillation detection ring is suspended on respectively the top of the interior sample cell equipped with energetic material to be measured, also include a collecting temperature sensor signal and by the signal transmission to control module, collection scintillation detection ring signal and by the signal transmission to control module test module, also include a setting heter temperature and heating mode, receive the signal of test module, displays temperature test result, show scintillation testing result and heater heating is sent to test module or stops the control module of heater heating instructions；The scintillation detection ring is annular, built-in thermoelectric hinders, when steam generation scintillation, thermal resistance resistance under flame temperature effect can change, change in resistance is converted to the change of voltage and feeds back to control module by test module, and after receiving voltage change signal, control module sends stopping heating instructions to test module, and temperature value of recording voltage when changing, complete scintillation detection process.
3. the special equipment of energetic material flash-point method of testing according to claim 2, it is characterised in that：Also include a printer being connected with control module.
4. the special equipment of energetic material flash-point method of testing according to claim 2, it is characterised in that：The interior sample cell external diameter is less than outer sample cell internal diameter, interior sample cell and outer sample cell tight fit.
5. the special equipment of energetic material flash-point method of testing according to claim 2, it is characterised in that：The interior sample cell is 3～5, and each interior sample cell external diameter is identical, and internal diameter is sequentially reduced.
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| CN201510682656.0A CN106610391A (en) | 2015-10-21 | 2015-10-21 | Energetic material flash point test method and equipment thereof |
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| CN201510682656.0A CN106610391A (en) | 2015-10-21 | 2015-10-21 | Energetic material flash point test method and equipment thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109406575A (en) * | 2018-11-01 | 2019-03-01 | 北京华科仪科技股份有限公司 | A kind of open flash point measurement device and method lighted a fire using flammable liquid |
| CN111766269A (en) * | 2020-08-11 | 2020-10-13 | 合肥国轩高科动力能源有限公司 | Automatic testing system and method for closed flash point of lithium ion battery electrolyte |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109406575A (en) * | 2018-11-01 | 2019-03-01 | 北京华科仪科技股份有限公司 | A kind of open flash point measurement device and method lighted a fire using flammable liquid |
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Application publication date: 20170503 |