CN107656031B - High-pressure gas impact loading safety performance testing method for energetic material - Google Patents
High-pressure gas impact loading safety performance testing method for energetic material Download PDFInfo
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- 238000012360 testing method Methods 0.000 title claims abstract description 87
- 238000011068 loading method Methods 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 50
- 238000004880 explosion Methods 0.000 claims abstract description 47
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 36
- 238000001514 detection method Methods 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000012545 processing Methods 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 3
- 238000002485 combustion reaction Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 230000007613 environmental effect Effects 0.000 claims description 5
- 150000001540 azides Chemical class 0.000 claims description 4
- 239000002826 coolant Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 2
- GDDNTTHUKVNJRA-UHFFFAOYSA-N 3-bromo-3,3-difluoroprop-1-ene Chemical compound FC(F)(Br)C=C GDDNTTHUKVNJRA-UHFFFAOYSA-N 0.000 claims 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims 2
- 239000000853 adhesive Substances 0.000 claims 2
- 230000001070 adhesive effect Effects 0.000 claims 2
- 229920001973 fluoroelastomer Polymers 0.000 claims 2
- NDEMNVPZDAFUKN-UHFFFAOYSA-N guanidine;nitric acid Chemical compound NC(N)=N.O[N+]([O-])=O.O[N+]([O-])=O NDEMNVPZDAFUKN-UHFFFAOYSA-N 0.000 claims 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims 1
- 229910000019 calcium carbonate Inorganic materials 0.000 claims 1
- -1 dihydroxyethyl Chemical group 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 1
- 239000003381 stabilizer Substances 0.000 claims 1
- 239000002360 explosive Substances 0.000 abstract description 4
- 238000011056 performance test Methods 0.000 abstract description 2
- 239000003380 propellant Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 238000007619 statistical method Methods 0.000 abstract 1
- 239000000446 fuel Substances 0.000 description 9
- 239000004721 Polyphenylene oxide Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 229920000570 polyether Polymers 0.000 description 6
- 239000004449 solid propellant Substances 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
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- 238000011156 evaluation Methods 0.000 description 2
- 239000003721 gunpowder Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 1
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Abstract
The invention relates to a high-pressure gas impact loading safety performance test method for energetic materials, which relates to the technical detection of explosives, pyrotechnic compositions and solid-liquid propellants, and comprises the following detection steps: sample preparation, condition selection, detection implementation and data processing. During sample preparation, the dosage of liquid and powder samples is 100 mg, and solid samples are prepared into tablets with the diameter of 10mm multiplied by 3 mm. The selected equipment is a high-pressure gas generating device, a high-pressure gas releasing device and a gas pressure detecting device, the high-pressure gas generating device adopts low-temperature gas generating agent to rapidly burn so as to provide high-pressure gas required by the test, and the maximum pressure deviation of the gas generated by the test device is +/-0.25 MPa. And when the detection is carried out, measuring the gas pressure value of the 50% explosion probability of the tested sample or the minimum explosion gas pressure value of the tested sample. And during data processing, calculating the critical burst gas pressure value according to a mathematical statistical method. The invention also has the advantages of simple method, reliable data and good test repeatability.
Description
Technical Field
The invention relates to a safety detection technology for energetic materials such as gunpowder, solid-liquid propellant and the like in the processes of production, use and the like, in particular to a high-pressure gas impact loading safety performance test method for the energetic materials.
Background
During the production and use of energetic materials, the danger of ignition and detonation by high-pressure gas impact loading often exists, for example, pipeline transportation and high-pressure injection of liquid fuel are carried out under the high-pressure gas impact loading environmental condition, but people have insufficient understanding, attention and evaluation methods of the danger, and related characterization technologies and test methods are not available for the safety performance of the energetic materials in the high-pressure gas impact loading process.
In the prior art, a high-pressure gas impact loading safety performance identification test is carried out, firstly, normal-temperature, clean and stable high-pressure gas must be provided, and an air compressor is usually adopted in industry, but a domestic air compressor cannot meet the requirement of the test on a high-pressure value of the gas, and a large-scale high-pressure air compressor unit imported from abroad is large in size, expensive and not suitable for being used in conventional tests. At present, the common high-pressure gas generating device is a device such as a light gas gun, and the like, and the device utilizes a gunpowder high-speed launching device to provide power and generate high-pressure gas, and has the following defects: large size, high cost, unstable pressure of produced gas and complex operation. At present, another technology is a solid engine cold supercharging system, and the method is as follows: an imported air compressor set is adopted to inflate a specially-made high-pressure air storage tank, then a control ball valve is adjusted, the gas in the high-pressure air storage tank is used for impact loading on a simulated solid engine, the ignition and pressure building process of the engine is simulated by quickly pressurizing the inner cavity of a explosive column, the main examination target is the structural integrity of the explosive column, and the safety performance of the explosive column in the pressurizing process cannot be evaluated.
Disclosure of Invention
The invention aims to provide a high-pressure gas impact loading safety performance testing method for an energetic material, which can effectively utilize the rapid combustion of a low-temperature gas generating agent to provide normal-temperature, clean and stable high-pressure gas required by a test, and reliably utilize a gas pressure value with 50% explosion probability or a minimum explosion gas pressure value to quantitatively represent the safety performance of the energetic material in the high-pressure gas impact loading process.
The design scheme of the invention is as follows:
the detection steps of the invention are as follows: sample preparation, condition selection, detection implementation and data processing.
In the sample preparation process, the dosage of liquid and powder samples is 100 mg, the samples are accurately weighed and added into a ceramic crucible and placed at the bottom of a sample pool in each test, solid samples are made into cylindrical tablets with the diameter of 10mm multiplied by 3mm, and one tablet is directly and horizontally placed at the bottom of the sample pool in each test.
In the condition selection process, the equipment conditions are as follows: a high-pressure gas generating device, a high-pressure gas releasing device and a gas pressure detecting device are adopted. The high pressure gas generating device adopts low temperature gas generating agent, which is non-azide gas generating agent capable of generating a large amount of gas during fast combustion, the chemical reaction is rapid, the effective gas production is large, the solid residue is less, and the gas generating agent is added with chemical coolant to facilitate the reduction of gas making temperature. The high-pressure gas release device is provided with a gas guide plug head, a cooling system, a stainless steel gas guide screw, a high-pressure gas pipe and a high-pressure ball valve, so that the high-pressure gas is optimal in purification and cooling effects and rapid in introduction and release; the gas pressure detection device is provided with a horizontally fixed closed sample cell and a piston type pressure sensor, and in each test, the peak value in a pressure curve signal detected by the pressure sensor represents the gas pressure value of the current test; the detection environmental conditions were: the maximum deviation of the pressure value of the gas generated by the test device is +/-0.25 MPa, and the pressure attenuation in 100ms is less than 10 percent; the detection equipment has good air tightness, effective high-pressure gas loading and obvious filtering and cooling effects.
In the detection implementation process, in order to determine the required gas generating agent loading amount during different pressure tests, at least 6 groups of calibration tests are required to be carried out on the adopted gas generating agent, single-group three-cycle repeated detection is respectively carried out, the average pressure peak value of the generated gas is measured when the low-temperature gas generating agent is different in loading amount, and a relation curve graph of the gas amount and the pressure value is drawn by adopting a least square method according to the calibration test result; in order to obtain a gas pressure value with 50% explosion probability of a detected sample, a group of constant step effective test times of not less than 25 detections are carried out on the detected sample according to a 'lifting method', or in order to obtain a minimum explosion gas pressure value of the detected sample, 5 repeated tests are carried out on the detected sample under different pressures until at least one explosion occurs in 5 tests of a certain pressure, and no explosion occurs in 5 tests with one step pressure, wherein the pressure value is the minimum explosion gas pressure value, and the method for judging whether the sample generates the 'explosion' comprises the following steps: and observing whether the sample has phenomena of explosion sound and trace, combustion, decomposition, color change and the like, judging that the sample is in explosion if one phenomenon appears, and judging that the sample is not in explosion if the other phenomenon appears.
In the data processing process, after a group of tests are completed on a tested sample, according to a test result recording table under different gas pressures, a gas pressure value with 50% explosion probability is calculated according to a mathematical statistics 'lifting method', or a minimum gas pressure value with at least one explosion is determined, and the safety performance of the tested sample under the high-pressure gas impact loading condition is represented according to the minimum gas pressure value.
The beneficial technical effects of the invention are as follows: because the high-pressure gas generating device adopts the low-temperature gas generating agent, and the gas making temperature is reduced by the cooling system, normal-temperature, clean and stable high-pressure gas can be provided for the detection process, so that the requirement of the detection process on the normal-temperature high-pressure gas is met. Meanwhile, because a relation curve graph of the dosage of the gas generating agent and the pressure value is drawn in the detection process, the high-pressure gas with the pressure value required by each test can be accurately and reliably provided by controlling the dosage of the gas generating agent, and the maximum deviation of the pressure value of the generated gas is +/-0.25 MPa. In addition, in the data processing process, the 'gas pressure value with 50% explosion probability' or the 'minimum explosion gas pressure value' is used as an evaluation index, so quantitative evaluation parameters are introduced in the field for the first time. The invention also has the advantages of wide application range, strong operability, reliable detection data and good test repeatability.
Drawings
FIG. 1 is a flowchart of a test procedure for the method of the present invention.
FIG. 2 is a schematic diagram of the structure of a test apparatus used in the method of the present invention.
In the figure, 1 is a closed sample cell, 2 is a tested sample, 3 is a piston type pressure sensor, 4 is a high-pressure air pipe, 5 is a high-pressure ball valve, 6 is a stainless steel air guide screw, 7 is a cooling system, 8 is an air guide plug, 9 is a closed combustion chamber, 10 is a low-temperature gas generating agent, and 11 is an ignition electrode.
Detailed Description
The invention will be further explained in two parts with reference to the embodiments provided in the drawings.
Example 1: minimum burst gas pressure value test for fish-2 liquid fuel.
Step one, sample preparation.
In each test, a fish-2 liquid fuel test sample ⑵ 100 is accurately weighed, the fish-2 liquid fuel test sample is put into a ceramic crucible and placed at the bottom of a closed sample cell ⑴, and a low-temperature gas generating agent adopted in the test is dried in a water bath oven for 4 hours at 40 ℃ before use.
And step two, selecting conditions.
In the condition selection process, the equipment conditions are that a high-pressure gas generating device, a high-pressure gas releasing device and a gas pressure detecting device are adopted, the high-pressure gas generating device adopts a low-temperature gas generating agent ⑽ which is a non-azide gas generating agent capable of generating a large amount of gas when being excited by an ignition electrode ⑾ to rapidly combust in a closed combustion chamber ⑼, the high-pressure gas releasing device has the advantages of rapid chemical reaction, large effective gas generation amount and less solid residues, and chemical cooling agents are added into the gas generating agent so as to be beneficial to reducing the gas production temperature, the high-pressure gas releasing device is provided with a high-pressure gas pipe ⑷, a high-pressure ball valve 45, a stainless steel gas guide screw ⑹, a cooling system ⑺ and a gas guide plug ⑻, the device has the best purification and temperature reduction effects and rapid release of high-pressure gas, the gas pressure detecting device is provided with a horizontally fixed closed sample 493 pool 2 and a piston type pressure sensor ⑶, the detection environmental conditions are that the maximum pressure deviation of the gas generated by the testing device is +/-0.25, the pressure attenuation of the gas generated by the testing device within 100ms time is reduced by less than 10%, the pressure of the gas tightness testing device, the high-pressure testing device loading and the high-pressure testing device is obviously debugged, the gas testing device is adjusted within 100ms, the time of the high-pressure testing device.
And step three, detection is implemented.
In the detection implementation process, firstly, a test target and a test process are determined, the test target is to obtain the minimum explosion gas pressure value of the fish-2 liquid fuel, in order to determine the required gas generating agent loading amount during different pressure tests, a calibration test needs to be carried out on the relationship between the gas generating agent dosage and the pressure value, the calibration test carries out 6 groups, single-group three-cycle repeated detection is respectively carried out, a gas pressure signal is detected through a pressure sensor, a data recorder records a time-pressure curve signal, reads a pressure peak value, calculates the average pressure peak value of the single-group three-cycle test, according to the average pressure peak value of gas generated during different loading amounts of the gas generating agent, a relation curve graph of the gas generating agent dosage and the pressure value is drawn by adopting a least square method, when tested sample ⑵ is tested, in order to obtain the minimum explosion gas pressure value of the fish-2 liquid fuel, a first group of tests is carried out from 30MPa, the pressure of the test is set to be 2.0MPa, 5 times of the test is repeatedly carried out under each pressure condition, whether explosion phenomenon occurs or not, and whether the explosion phenomenon occurs or not is judged to be one of the explosion phenomenon, if the explosion phenomenon occurs, the test is carried out, if the test is carried out, the test method is carried out, and the method is carried out, if the method is carried out, and the method is carried out, wherein the method is carried out, the method is carried out.
And step four, data processing.
During the data processing, the minimum gas pressure value of at least one 'explosion' is determined, and the safety performance of the fish-2 liquid fuel under the high-pressure gas impact loading condition is represented. The determination method comprises the following steps: at least one explosion occurs in 5 tests of a certain pressure, and no explosion occurs in 5 tests of reducing one step pressure, and the pressure value is the minimum explosion gas pressure value.
Table 1 is a record table of the test results of the fish-2 liquid fuel, the sample has a ' burst ' phenomenon under 36MPa, and the samples have no burst ' after 5 times of tests under 34MPa, so that the minimum burst gas pressure value of the fish-2 liquid fuel is 36 MPa.
TABLE 1
Note that "○" represents a test sample outbreak, and "X" represents a test sample not outbreak.
Example 2: HTPE-103 polyether composite solid propellant gas pressure value at 50% probability of burst was tested.
Step one, sample preparation.
The HTPE-103 polyether composite solid propellant is prepared into a phi 10mm multiplied by 3mm tablet test sample ⑵, a test sample ⑵ is horizontally placed at the bottom of a closed sample pool ⑴ during each test, and a low-temperature gas generating agent adopted in the test is dried in a water bath oven for 4 hours at 40 ℃ before being used.
And step two, selecting conditions.
In the condition selection process, the equipment conditions are that a high-pressure gas generating device, a high-pressure gas releasing device and a gas pressure detecting device are adopted, the high-pressure gas generating device adopts a low-temperature gas generating agent ⑽ which is a non-azide gas generating agent capable of generating a large amount of gas when being excited by an ignition electrode ⑾ to rapidly combust in a closed combustion chamber ⑼, the high-pressure gas releasing device has the advantages of rapid chemical reaction, large effective gas generation amount and less solid residues, and chemical cooling agents are added into the gas generating agent so as to be beneficial to reducing the gas production temperature, the high-pressure gas releasing device is provided with a high-pressure gas pipe ⑷, a high-pressure ball valve 45, a stainless steel gas guide screw ⑹, a cooling system ⑺ and a gas guide plug ⑻, the device has the best purification and temperature reduction effects and rapid release of high-pressure gas, the gas pressure detecting device is provided with a horizontally fixed closed sample 493 pool 2 and a piston type pressure sensor ⑶, the detection environmental conditions are that the maximum pressure deviation of the gas generated by the testing device is +/-0.25, the pressure attenuation of the gas generated by the testing device within 100ms time is reduced by less than 10%, the pressure of the gas tightness testing device, the high-pressure testing device loading and the high-pressure testing device is obviously debugged, the gas testing device is adjusted within 100ms, the time of the high-pressure testing device.
And step three, detection is implemented.
In the detection implementation process, firstly, a test target and a test process are determined, the test target is to obtain a gas pressure value with 50% explosion probability of the HTPE-103 polyether composite solid propellant, in order to determine the required gas generating agent loading amount during different pressure tests, a calibration test needs to be carried out on the relation between the gas generating agent loading amount and the pressure value, the calibration test is carried out for 6 groups, single-group three-cycle repeated detection is respectively carried out, a time-pressure curve signal is recorded through a pressure sensor gas pressure signal and a data recorder, the pressure peak value is read, the average pressure peak value of the single-group three-cycle test is calculated, a relation curve graph of the gas generating agent loading amount and the pressure value is drawn by adopting a least square method according to the average pressure peak value of gas generated when the gas generating agent loading amount is different, when a detected sample ⑵ is detected, in order to obtain the gas pressure value with 50% explosion probability of the HTPE-103 polyether composite solid propellant, 2.0MPa is taken as a constant pressure step length, the test is carried out according to a rising and falling method, if the explosion probability of the initial pressure value is increased until the explosion phenomenon is observed, and the explosion phenomenon is judged to be one of the explosion phenomenon, if the explosion phenomenon is not generated, the explosion phenomenon is observed, and the step length is judged to be one of the explosion phenomenon is judged to be one, wherein the method, the method is that the explosion phenomenon is found, and the explosion phenomenon is judged to be one.
And step four, data processing.
In the data processing process, the test results of the tested sample are subjected to data processing according to a lifting method, the gas pressure value with 50% explosion probability is calculated, the gas pressure with 50% explosion probability of the HTPE-103 polyether composite solid propellant tablet is 46.0MPa, and a table 2 is a test result recording table of the HTPE-103 polyether composite solid propellant.
TABLE 2
Note that "○" represents a test sample outbreak, and "X" represents a test sample not outbreak.
Claims (1)
1. A high-pressure gas impact loading safety performance testing method for energetic materials comprises the following detection steps: preparing a sample, selecting conditions, detecting and implementing, and processing data; the method is characterized in that:
in the sample preparation process, the dosage of the liquid and powder detected sample is 100 mg, and the solid detected sample is made into a cylindrical tablet with the diameter of 10mm multiplied by 3 mm;
in the condition selection process, the detection equipment conditions are as follows: the high-pressure gas generating device is provided with a low-temperature gas generating agent, the low-temperature gas generating agent is a non-azide gas generating agent capable of generating a large amount of gas during fast combustion, and the low-temperature gas generating agent mainly comprises 43.5% of Guanidine Nitrate (GN), 38.8% of Ammonium Perchlorate (AP), 3.5% of copper oxide (CuO) and iron oxide (Fe)2O3) 2.5% of calcium carbonate (CaCO)3)3.6 percent of dihydroxyethyl Dioxime (DHG), 2.0 percent of fluororubber adhesive, 4.8 percent of fluororubber adhesive and 1.3 percent of stabilizing agent, wherein the chemical reaction is very quick, 30-600MPa ultrahigh pressure gas can be generated within 100ms, quick combustion and explosion are realized, the chemical reaction is quick, the effective gas production is large, the solid residues are few, and a chemical cooling agent is added into the low-temperature gas generating agent to facilitate the reduction of the gas production temperature, so that normal-temperature, clean and stable high-pressure gas can be provided for the detection process of the gas pressure detection device;
the detection environmental conditions were: the detection equipment has good air tightness and obvious filtering and cooling effects, the maximum deviation of the pressure value of the generated gas is +/-0.25 MPa, and the pressure attenuation in 100ms is less than 10 percent;
in the detection implementation process, the technical means for the detected sample is as follows: the method comprises the following steps of condition calibration, grouping detection, result judgment and data recording, in order to determine the required gas generating agent loading amount during different pressure tests, at least 6 groups of calibration tests are required to be carried out on the adopted low-temperature gas generating agent, single-group three-cycle repeated detection is respectively carried out, the average pressure peak value of the generated gas is measured and calculated when the low-temperature gas generating agent is different in loading amount, and a relation curve graph of the gas amount and the pressure value is drawn by adopting a least square method according to the calibration result; in order to obtain a gas pressure value with 50% explosion probability, a group of constant step length effective test times of not less than 25 tests are carried out on a tested sample according to a lifting method, or in order to obtain a minimum explosion gas pressure value, the tested sample is subjected to 5 repeated tests in each pressure stage until the minimum gas pressure value when at least one explosion occurs is found;
in the data processing process, a test record table is drawn according to the test result of the tested sample, the gas pressure value with 50% explosion probability is calculated according to a mathematical statistics 'lifting method', or the minimum explosion gas pressure value is determined, and the safety performance of the tested sample under the high-pressure gas impact loading condition is represented according to the minimum explosion gas pressure value.
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| CN110231363B (en) * | 2019-05-23 | 2020-07-28 | 西安交通大学 | Method for researching reaction mechanism of energetic material and evaluating safety |
| CN110486191A (en) * | 2019-07-01 | 2019-11-22 | 中国人民解放军96901部队24分队 | A kind of large-sized solid rocket Structural Integrity of Propellant Grains test method and device |
| CN112083040A (en) * | 2020-10-20 | 2020-12-15 | 南京理工大学 | Method for testing flash point of flammable liquid under high-pressure environment |
| CN112067659A (en) * | 2020-10-20 | 2020-12-11 | 南京理工大学 | Test device for testing high-pressure flash point of flammable liquid |
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