CN105606649A - High-activity aluminum powder combustion heat measurement method - Google Patents
High-activity aluminum powder combustion heat measurement method Download PDFInfo
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- CN105606649A CN105606649A CN201610132623.3A CN201610132623A CN105606649A CN 105606649 A CN105606649 A CN 105606649A CN 201610132623 A CN201610132623 A CN 201610132623A CN 105606649 A CN105606649 A CN 105606649A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 47
- 230000000694 effects Effects 0.000 title claims abstract description 14
- 238000000691 measurement method Methods 0.000 title abstract 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 19
- 239000001301 oxygen Substances 0.000 claims abstract description 19
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000005711 Benzoic acid Substances 0.000 claims abstract description 7
- 235000010233 benzoic acid Nutrition 0.000 claims abstract description 7
- JSOGDEOQBIUNTR-UHFFFAOYSA-N 2-(azidomethyl)oxirane Chemical compound [N-]=[N+]=NCC1CO1 JSOGDEOQBIUNTR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229920000642 polymer Polymers 0.000 claims abstract description 5
- 239000004411 aluminium Substances 0.000 claims description 50
- 229910052782 aluminium Inorganic materials 0.000 claims description 50
- 239000000843 powder Substances 0.000 claims description 48
- 238000003556 assay Methods 0.000 claims description 6
- 238000007707 calorimetry Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 239000003380 propellant Substances 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract description 2
- 238000009472 formulation Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000006213 oxygenation reaction Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002671 adjuvant Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 241000669618 Nothes Species 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- NNBFNNNWANBMTI-UHFFFAOYSA-M brilliant green Chemical group OS([O-])(=O)=O.C1=CC(N(CC)CC)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](CC)CC)C=C1 NNBFNNNWANBMTI-UHFFFAOYSA-M 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004200 deflagration Methods 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/22—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures
- G01N25/26—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures using combustion with oxygen under pressure, e.g. in bomb calorimeter
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/22—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures
- G01N25/44—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures the heat developed being transferred to a fixed quantity of fluid
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention discloses a high-activity aluminum powder combustion heat measurement method. The method includes the following steps of firstly, calibrating a heat metering system of an oxygen bomb calorimeter through benzoic acid so as to obtain the thermal capacity of the system; secondly, mixing aluminum powder with glycidyl azide polymer (GAP) to form a sample; thirdly, weighing the mixed combustion sample, putting the sample in a calorimetric bomb, introducing oxygen, putting the calorimetric bomb in water, making the sample combust in the calorimetric bomb, and accurately measuring the water temperature values before and after combustion; fourthly, calculating the combustion heat value of aluminum powder according to the formula. The method is high in accuracy, safe and feasible, and the experiment basis is provided for thermodynamic calculation and formulation design of aluminum-contained propellant.
Description
Technical field
The present invention relates to the assay method of substance combustion heat, be applicable to the mensuration of the high activity aluminium powder combustion heat.
Background technology
Micro-/ nano aluminium powder, owing to having higher combustion heat value, is commonly used the high-energy metals incendiary agent that does propellant, noThe combustion speed that has only improved solid propellant, has increased specific impulse, can also reduce Pressure Exponent simultaneously. Aluminium powder in air very easily byOxidation, forms Al2O3, the aluminium powder that surface is oxidized, its chemical potential (combustion heat) has also reduced, and different-grain diameter, shapeAnd the aluminium powder combustion heat that preparation technology obtains also there are differences, if only use theoretical numerical value often to have larger error, this alsoBring larger difficulty to calculation of thermodynamics and the formula Design of aluminized propellant. Therefore, use aluminium powder before to its combustion heatIt is necessary that value is measured.
Go back neither one method accurately, National University of Defense technology's space flight and material for the combustion heat value test of aluminium powder at presentThe Liu Xiang of engineering college is emerald green to be waited (" nanometer aluminium powder and the research of nanometer aluminium powder/kerosene gel rubber system energy characteristics ", solid-rocket technology,2005) utilize oxygen-bomb calorimeter, directly get aluminium powder sample in oxygen bomb, burn obtain the combustion heat. But with this traditional calorimetricThere is following problem in the instrument method of testing test aluminium powder combustion heat: the combustion process of (1) aluminium powder is as easy as rolling off a log reunites, builds up, coagulatesThe phenomenons such as knot, directly light and just there will be incomplete combustion, thereby cause test result unstable, poor repeatability; (2) high activityAluminium powder, due to its powder morphology, makes it to be different from common propellant, and deflagration phenomenon can occur ignition point, makes oxygen bomb insidePressure moment raise, simultaneously the high temperature of moment also can cause ablation phenomen, cannot obtain valid data, simultaneously also can be to experimentInstrument component causes damage.
Summary of the invention
In order to overcome the deficiencies in the prior art and defect, the invention provides a kind of degree of accuracy high, safe, easy rowThe assay method of the high activity aluminium powder combustion heat.
Glycidyl azide polymer (GAP), as one in recent years in propellant effect preferably containing can adhesive,There is good compatibility with aluminium powder. The present invention utilizes the first law of thermodynamics, in adiabatic constant volume reactor, uses GAP to doFor combustion adjuvant and aluminium powder carry out after certain proportion mixes burning again, thereby indirectly obtain the combustion heat of aluminium powder. GAP on the one handMacromolecule mesh skeleton can be scattered in fine aluminium powder wherein effectively, has avoided agglomeration; GAP plays on the other handReduce the effect of aluminium powder burn rate, aluminium powder can steadily be burnt completely, thereby ensures that experiment safety enters smoothlyOK.
The assay method of the high activity metal aluminium powder combustion heat provided by the invention, step is as follows: (1) with benzoic acid to oxygen bomb heatThe Calorimetry system of amount meter is demarcated, and obtains the thermal capacity E of system; (2) by newly aluminium powder and the glycidyl azide polymer GAP in Kaifeng pressEvenly mix sample preparation according to mass ratio 1:2～10; (3) taking quality is that the mixed combustion sample of 0.20～0.35g is placed in calorimetricIn bullet, be filled with oxygen, then calorimetric bomb is placed in to water, measure the initial temperature T of water0, allow sample burn in calorimetric bomb, Accurate Determining combustionWater temperature value T after burningn; (4) according to the combustion heat Q of the intensification value of water and GAPGAP, according to formulaCalculate the combustion heat value of high activity aluminium powder.
The pressure that is filled with oxygen described in step (3) is 1.5～2.0MPa.
A preferred embodiment of the present invention, described aluminium powder and glycidyl azide polymer GAP mass ratio are selected 1:4, calorimetricMixed combustion sample in bullet is 0.25g, and oxygenation pressure is 1.5MPa.
Compared with prior art, the invention has the advantages that:
(1) by adding GAP skeleton structure to avoid the agglomeration of aluminium powder as combustion adjuvant, thereby it can be fired completelyBurn, than direct method of testing, data result is more reliable, and efficiency of combustion can reach 99.03%, and (documents is only78.4％)。
(2) by adding GAP to reduce the burn rate of aluminium powder, avoided moment to fire instrument has been caused to damage, ensuredExperiment safety carries out smoothly.
Detailed description of the invention
Describe in detail below by specific embodiment Dui Zuo Jin of the present invention ー step, but it should be noted that not limit of the present inventionBe formed on this, all technology that realize according to the present invention are all within the present invention protects category. In the embodiment of the present invention, all useGR-3500 type oxygen bomb calorimeter is measured. Efficiency of combustion computing formula is measured value/theoretical value × 100%.
Embodiment 1
With benzoic acid, the calorimetric Calorimetry system of oxygen bomb is repeatedly demarcated, got extreme difference and be no more than testing for 5 times of 40J/KThe mean value of result, as the thermal capacity of system, obtains E=14511.2J/K; By the aluminium powder (50nm, the active aluminium content that newly break a seal82%) evenly mix sample preparation with GAP according to 1:3 (mass ratio), the burning sample that takes 0.2501g is placed in calorimetric bomb,Be filled with excessive oxygen, then calorimetric bomb is placed in to a certain amount of water, allow sample burn in calorimetric bomb, the intensification of Accurate Determining waterValue (Tn-T0); Again according to formulaCalculate the combustion heat value of aluminium powder. Wherein oxygenation pressure is1.5MPa. Test two groups and get the combustion heat of its mean value as aluminium powder, the results are shown in Table 1.
Embodiment 2
With benzoic acid, the calorimetric Calorimetry system of oxygen bomb is repeatedly demarcated, got extreme difference and be no more than testing for 5 times of 40J/KThe mean value of result, as the thermal capacity of system, obtains E=14511.2J/K; By the aluminium powder (50nm, the active aluminium content that newly break a seal82%) evenly mix sample preparation with GAP according to 1:4 (mass ratio), the burning sample that takes 0.2504g is placed in calorimetric bomb,Be filled with excessive oxygen, then calorimetric bomb is placed in to a certain amount of water, allow sample burn in calorimetric bomb, the intensification of Accurate Determining waterValue (Tn-T0); Again according to formulaCalculate the combustion heat value of aluminium powder. Wherein oxygenation pressure is1.5MPa. Test three groups and get the combustion heat of its mean value as aluminium powder, the results are shown in Table 1.
Embodiment 3
With benzoic acid, the calorimetric Calorimetry system of oxygen bomb is repeatedly demarcated, got extreme difference and be no more than testing for 5 times of 40J/KThe mean value of result, as the thermal capacity of system, obtains E=14511.2J/K; By the aluminium powder (50nm, the active aluminium content that newly break a seal82%) evenly mix sample preparation with GAP according to 1:4 (mass ratio), the burning sample that takes 0.3019g is placed in calorimetric bomb,Be filled with excessive oxygen, then calorimetric bomb is placed in to a certain amount of water, allow sample burn in calorimetric bomb, the intensification of Accurate Determining waterValue (Tn-T0); Again according to formulaCalculate the combustion heat value of aluminium powder. Wherein oxygenation pressure is1.5MPa. Test three groups and get the combustion heat of its mean value as aluminium powder, the results are shown in Table 1.
Embodiment 4
With benzoic acid, the calorimetric Calorimetry system of oxygen bomb is repeatedly demarcated, got extreme difference and be no more than testing for 5 times of 40J/KThe mean value of result, as the thermal capacity of system, obtains E=14511.2J/K; By the aluminium powder (50nm, the active aluminium content that newly break a seal82%) evenly mix sample preparation with GAP according to 1:4 (mass ratio), the burning sample that takes 0.2511g is placed in calorimetric bomb,Be filled with excessive oxygen, then calorimetric bomb is placed in to a certain amount of water, allow sample burn in calorimetric bomb, the intensification of Accurate Determining waterValue (Tn-T0); Again according to formulaCalculate the combustion heat value of aluminium powder. Wherein oxygenation pressure is2.0MPa. Test three groups and get the combustion heat of its mean value as aluminium powder, the results are shown in Table 1.
The measurement result of the high activity aluminium powder combustion heat of the present invention and theoretical value comparison:
Table 1 the present invention records the combustion heat data of aluminium powder
Each embodiment and theoretical value are compared, as shown above, find the aluminium powder burning that the inventive method recordsCalorific value and calculated value are very approaching, and efficiency of combustion can reach 99.03%. Confirm the survey of high activity metal aluminium powder of the present inventionDetermine not only easily row of safety of method, and there is higher efficiency of combustion.
Claims (2)
1. an assay method for the high activity aluminium powder combustion heat, is characterized in that step is as follows:
(1) with benzoic acid, the calorimetric Calorimetry system of oxygen bomb is demarcated, obtained the thermal capacity E of system;
(2) according to mass ratio 1:X mixing aluminium powder and glycidyl azide polymer GAP, obtain mixed combustion sample, wherein X be 2～10；
(3) taking quality is that the mixed combustion sample of m is put into calorimetric bomb, is filled with oxygen, and being placed in initial temperature is ToWater in, measure combustionWater temperature value T after burningn, wherein m is 0.20～0.35g;
(4) according to formulaCalculate the combustion heat of high activity aluminium powder, wherein QGAPFor the combustion of GAPBurn heat.
2. the assay method of the high activity aluminium powder combustion heat according to claim 1, is characterized in that described in step (3)The pressure that is filled with oxygen is 1.5～2.0MPa.
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| CN201610132623.3A CN105606649A (en) | 2016-03-09 | 2016-03-09 | High-activity aluminum powder combustion heat measurement method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107247074A (en) * | 2017-06-20 | 2017-10-13 | 江苏和顺环保有限公司 | The assay method of low heat value industry dangerous waste combustion heat value |
| CN108106755A (en) * | 2017-12-07 | 2018-06-01 | 中国神华能源股份有限公司 | calorimeter acceptance method |
| CN109060875A (en) * | 2018-08-17 | 2018-12-21 | 西安近代化学研究所 | The test method of active aluminium content in a kind of aluminium powder |
| CN110261435A (en) * | 2019-06-05 | 2019-09-20 | 中国建筑科学研究院有限公司 | A method for measuring the calorific value of combustion of thermosetting composite polystyrene board |
| CN114113210A (en) * | 2021-11-19 | 2022-03-01 | 华能国际电力股份有限公司 | A method to improve the accuracy of fuel calorific value determination |
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| CN110261435A (en) * | 2019-06-05 | 2019-09-20 | 中国建筑科学研究院有限公司 | A method for measuring the calorific value of combustion of thermosetting composite polystyrene board |
| CN114113210A (en) * | 2021-11-19 | 2022-03-01 | 华能国际电力股份有限公司 | A method to improve the accuracy of fuel calorific value determination |
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Application publication date: 20160525 |