CN102004119B - Method for measuring combustion heat value of boron powder - Google Patents
Method for measuring combustion heat value of boron powder Download PDFInfo
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- CN102004119B CN102004119B CN201010535657A CN201010535657A CN102004119B CN 102004119 B CN102004119 B CN 102004119B CN 201010535657 A CN201010535657 A CN 201010535657A CN 201010535657 A CN201010535657 A CN 201010535657A CN 102004119 B CN102004119 B CN 102004119B
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- acetone
- boron
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 78
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 78
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 77
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000003814 drug Substances 0.000 claims abstract description 35
- 239000011812 mixed powder Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000012545 processing Methods 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 238000005507 spraying Methods 0.000 claims abstract description 5
- 229910052796 boron Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000007800 oxidant agent Substances 0.000 claims description 15
- 238000012360 testing method Methods 0.000 claims description 15
- 239000011521 glass Substances 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- 239000012153 distilled water Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 230000037452 priming Effects 0.000 claims description 9
- 239000000320 mechanical mixture Substances 0.000 claims description 8
- 239000003380 propellant Substances 0.000 claims description 8
- 238000007707 calorimetry Methods 0.000 claims description 7
- 238000002474 experimental method Methods 0.000 claims description 6
- 238000003384 imaging method Methods 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 241001269238 Data Species 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims description 3
- 230000010354 integration Effects 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 230000005484 gravity Effects 0.000 claims description 2
- 238000009434 installation Methods 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000004804 winding Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 13
- 239000002671 adjuvant Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000012847 fine chemical Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000004449 solid propellant Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000013022 venting Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002817 coal dust Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910001120 nichrome Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001915 proofreading effect Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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Abstract
The invention discloses a method for measuring the combustion heat value of boron powder. The method comprises the following steps of: mixing SQ-2 powder and the boron powder and weighing; spraying standard acetone onto mixed powder for bonding into a pharmacophore; drying the pharmacophore in the air, weighing once again and cutting the dried pharmacophore into a plurality of sample medicament strips; winding the medicament strips on an ignition thread and connecting the ignition thread to an ignition electrode in an oxygen bullet; observing the sealing status of the oxygen bullet and recording initial temperature data; igniting the medicament strips to observe the variation curve of the temperature data; and integrating, cooling, correcting and processing the temperature data of inner and outer barrels by a cooling and correcting method so as to finally obtain the combustion heat value of a boron powder sample. The method ensures full combustion of the boron powder.
Description
Technical field
The present invention relates to a kind of combustion heat value measuring method; Especially being applicable in existing combustion heat value measurement mechanism can not boron powder sample perfect combustion, that burning-point is very high, also can be applicable to the mensuration of combustion heat value of other sample such as coal dust, boracic high-energy solid propellant or other fuel material that is difficult to perfect combustion of similar boron powder.
Background technology
In the prior art field, measure in the instrument of material thermal value and often adopt oxygen bomb calorimeter, the just usually said oxygen bomb system in sample combustion chamber wherein, as shown in Figure 1: the oxygen bomb system comprises body 1; Bullet 2, venting valve 3, electrode 4, gas admittance valve 5; Gas-filled tube 6, crucible 7, crucible holder 8; Nickel-cadmium ignition wire 9, oxidizer SQ-2 tablet (or medicinal powder) 10, boron powder sample 11.Oxygen gets into oxygen bomb through gas admittance valve 5 and gas-filled tube 6, and the gas after the burning is discharged by venting valve 3, insulation between electrode 4 and the bullet 2.Another electrode is by air intake valve 5 and gas-filled tube 6 double as.Boron powder sample 11 all is placed in the crucible 7 with oxidizer SQ-2 tablet (medicinal powder) 10, and oxidizer SQ-2 tablet (medicinal powder) 10 is put on the boron powder sample 11, and the helical buckling of nickel-cadmium ignition wire 9 igniting position is embedded among the oxidizer SQ-2 tablet (medicinal powder) 10.During test; Feed the DC voltage about 20v through electrode 4 and gas admittance valve 5 to ignition wire; The ignition wire heating oxidizer SQ-2 tablet (medicinal powder) 10 that ignites by oxidizer SQ-2 tablet (medicinal powder) the 10 boron powder that ignites, burns boron powder sample again in the hot environment of crucible.
The patent No. is ZL2006100429328's " detector for boron containing lean oxygen propellant heat value " patented technology; Be to be directed against boron containing lean oxygen propellant, mainly solved ignition difficulties and oxygen bomb, crucible and parts ablation problem thereof in the boron containing lean oxygen propellant heat value test process.Boron containing lean oxygen propellant self has flammable inflammable constituents such as bonding agent, oxygenant, and in test process, these flammable inflammable constituents can ensure the boron particles igniting, and simple boron powder is difficult for lighting, and this patented technology is not suitable for the combustion heat value test of boron powder.
People such as Pan Kuang Zhi of Northwestern Polytechnical University are published in the Acta Astronautica " measurement of boron powder heating power " literary composition and also report and once used oxygen bomb formula calorimeter; Adopt SQ-2 as combustion adjuvant; The measure theory calorific value is the boron powder of 52.929MJ/Kg, and the highest test value is 43.2349MJ/Kg, and burning efficiency is merely 81.68%; This article has solved the ignition problem of boron powder, but problem that can not perfect combustion still exists.
For the pure boron powder, its fusing point and boiling point very high (being respectively 2430K and 2823K), the burning of boron is the burning between a kind of solid phase and gas phase media, wants slow many with respect to the burning between gas phase media, the boron particles surface is coated with because the B that the boron oxidation forms
2O
3, its boiling point higher (about 2133K), if the environment temperature of burning is not high enough, B
2O
3Can't gasify fast, can only be fused into the B of thickness
2O
3Liquid is coated on the surface of boron particles, has hindered the diffusion of oxygen to boron particles and liquid oxidatively bed interface thereof, cause the boron particles ignition to lag behind (difficulty), and boron particles only could perfect combustion in oxidizing atmosphere and in the environment of continuous high temperature.The oxygen bomb calorimeter is as a good heat-exchange system of heat conductivility, and heat wherein scatters and disappears rapidly, and temperature can be reduced to below the 2133K, the B that causes the boron oxidation to generate
2O
3Can not vaporize but be coated on boron surface with liquid state; Hindered the diffusion of oxygen to boron particles and liquid oxidatively bed interface; The burning situation of cold and oxygen deficient causes the part of boron can not perfect combustion in the oxygen bomb of existing calorimeter, and the test calorific value that causes the boron powder is far below its theoretical calorific value.
Summary of the invention
In order to solve the problem that boron powder in the prior art can not perfect combustion; The present invention provides a kind of measuring method of boron powder combustion heat value; Can effectively ensure the perfect combustion of boron powder sample in oxygen bomb, thereby make the actual measurement combustion heat value calorific value theoretical of boron powder match with it.
The technical solution adopted for the present invention to solve the technical problems may further comprise the steps:
(1) back is ground in the turning of SQ-2 propellant charge and filter with 80 order stainless steel sifts, it is subsequent use to collect the SQ-2 powder that sieves.
(2) pour beaker into after SQ-2 powder and boron powder sample are mixed with 10: 1～16: 1 mass ratio, use glass bar to stir pulverous mixture, make it become the uniform mixed-powder of mechanical mixture.With beaker, mixed-powder and glass bar weighing together and write down its gross mass M
1
(3) being 99.9% standard acetone with mass concentration is sprayed on the mixed-powder with the speed of 2～5ml/s, constantly stirs simultaneously, when treating all mixed-powder bonding patent medicine groups, stops the acetone of spraying.The consumption of making sure to keep in mind acetone in this step reaches the mixed-powder patent medicine group that bonds is got final product; If it is too much that acetone adds, the dissolved patent medicine slurry of the SQ-2 particle in the mixed-powder is insoluble to the boron powder particles of acetone because density is bigger; Can precipitate, cause the mixing of sample inhomogeneous.
(4) beaker, bonding medicine group and glass bar being placed on temperature together is in 20 ± 5 ℃, the indoor environment of humidity≤45%, and the acetone volatilization is done until bonding medicine Tuanfeng County.With air-dry beaker, bonding medicine group and glass bar weighing together and write down its gross mass M
2
If M
1-0.05≤M
2≤M
1+ 0.05, it is air-dry then to regard as bonding medicine group, and acetone has volatilized and finished;
If
, then think in the bonding medicine group acetone not volatilization finish, continue volatilization after air-dry 48 hours, if satisfy M
1-0.05≤M
2≤M
1+ 0.05, it is air-dry then to regard as bonding medicine group, and acetone has volatilized and finished; If do not satisfy M
1-0.05≤M
2≤M
1+ 0.05 but satisfy M
1+ 0.05≤M
2≤M
1+ 0.1, just assert has (M
2-M
1) acetone of g can't evaporate under existence conditions fully, then thinks the mass M of mixing medicine group
3=M
SQ-2+ M
Boron+ (M
2-M
1), M wherein
SQ-2Be the quality of SQ-2, M
BoronBe the quality of boron, (M
2-M
1) be the acetone quality that remains in the sample.In the back during the data processing of test result, (M wherein
2-M
1) calorific value that produces of the acetone burning of g deducts as the calorific value of oxidizer, the combustion heat value that calculates the boron powder again gets final product that (calorific value of standard acetone is: 30.854MJ/Kg).
(5) the medicine group of air-dry curing to be cut into some quality be 3.0～4.5g, be shaped as 5mm*5mm*15mm, and tolerance is the sample medicinal strip of 1mm, use to be tested.
(6) measure the ignition wire of the known calorific value of 10～20cm,, the ignition wire hoop twined embed in the slit,, also be convenient to improve the igniting reliability so that suspension is reliable in medicinal strip specimen surface hoop delineation to be measured slit, 3～5 road.Terminate on the spark electrode in the oxygen bomb head ignition wire two fixing again.
(7) crucible is placed on the crucible holder; And crucible put into oxygen bomb with crucible holder; Installation oxygen bomb lid is adjusted the position of medicinal strip sample through crooked ignition wire, make the medicinal strip sample that is suspended on oxygen bomb lid below be positioned at crucible directly over; Guarantee that promptly medicinal strip sample freely falling body drops in the crucible, the oxygen bomb lid will be tightened and guarantee sealing.
(8) the each several part system of connection and debugging calorimetric instrument, the distilled water of can 8000～10000g in the urceolus of Calorimetry system, the distilled water of can 4000～5000g in the inner core of Calorimetry system.
(9) after the oxygen bomb assembling, charge into the sufficient amount of oxygen that can guarantee sample perfect combustion, then oxygen bomb is put into the distilled water of bucket, oxygen bomb can be immersed in the water fully.With firing cable priming supply is linked to each other with the electrode of oxygen bomb.Observe the oxygen bomb lid seals at bubble situation in the inner core,, oxygen bomb gas leakage is described, re-assembly oxygen bomb and behind the oxygen bomb good seal, can carry out next step experiment if the bubble generating rate surpasses 3/minute.
(10) start electric mixer through power controling box, and setting is the temperature data of the inside and outside tube of sampling time interval record with 5s in computer data acquiring imaging processing system.
(11) first record initial stage temperature data; After treating that the inner/outer tube system temperature reaches balance; Gather 50～80 groups of stable temperature datas, just can apply ignition signal through the switch of priming supply, ignition wire is lighted the medicinal strip sample rapidly; After ignition wire was blown, the medicinal strip sample that is burning fell under gravity into and burns away in the crucible until burnouting.
(12) observe the change curve of temperature data, treat that the inner core temperature curve reaches maximal value after, cooling is proofreaied and correct and is used when writing down one section decrease of temperature segment data in order to data processing again, descending branch decrease of temperature value should be not less than 0.2 ℃.
(13) adopt cooling method of correcting temperature data internal, urceolus to carry out integration cooling treatment for correcting, finally obtain the combustion heat value of boron powder sample.
The invention has the beneficial effects as follows: the present invention has selected for use the heating power behind the simplified structure to test special-purpose oxygen bomb system, and is as shown in Figure 2, compares with existing testing apparatus; One of the air-filled pore of this oxygen bomb system, vent port, electrode all combine; And is connected with oxygen bomb lid insulation, another electrode is held a concurrent post by the oxygen bomb housing, owing to having reduced the perforate that covers at oxygen bomb; Strengthened the sealing of oxygen bomb; In addition, ignition wire was screwed in oxygen bomb through a word screw threads and covered by being wrapped in originally to change on two electrodes, had improved the reliability of igniting.
When the present invention works; Apply the DC voltage of 15～25V between two electrodes, ignition wire energising heating is burnt the recombined sample medicinal strip that forms through mix casting, the cutting of air-dry back, and sample medicinal strip quality is about 3.0g～4.5g; After the burning some time; Ignition wire is blown voluntarily, and unburnt sample medicinal strip drops to the heat release that burns away in the crucible subsequently, up to perfect combustion.In this process, the boron powder of high heat value, high combustion temperature is in the hot environment that oxidizer SQ-2 burning provides always, has ensured the perfect combustion of boron powder.
The present invention is simple in structure, and stable performance is easy to operate, and reliable results has a good application prospect.
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Description of drawings
Fig. 1 is the oxygen bomb structural representation of the oxygen bomb calorimeter of prior art;
Fig. 2 is the oxygen bomb structural representation of the oxygen bomb calorimeter of the present invention's use;
Fig. 3 is an intermolecular mixed structure synoptic diagram of the present invention;
Fig. 4 is the high power electron microscope of the mechanical mixture of the present invention picture of taking pictures.
The calorimeter syndeton synoptic diagram that Fig. 5 uses for this method;
Label declaration among the figure: 1-body, 2-bullet, the 3-valve of exitting, 4-electrode, 5-gas admittance valve, 6-gas-filled tube; The 7-crucible, 8-crucible holder, 9-nickel-cadmium ignition wire, 10-oxidizer SQ-2 tablet (or medicinal powder), 11-boron powder sample; The 12-needle valve system, 13-insulator, 14-electrode, 15-medicinal strip sample, 16-SQ-2 cross-linked structure; 17-boron powder, 18-SQ-2 particle, 19-boron powder, 20-boron powder, 21-boron powder; 22-boron powder, 23-boron powder, 24-boron powder, 25-boron powder, 26-boron powder.
Embodiment
Fig. 2 has showed the modifying device of this method of testing, and this device is to be increased income after YDI-00 type oxygen bomb that Instr Ltd. produces removed the crucible suspended structure by Changsha, adds to screw that screw forms again.Fig. 3 has showed among the present invention the SQ-2 combustion adjuvant and the intermolecular structure of mixing of boron powder particles through acetone solution, and Fig. 4 has taken pictures photo display with the high power electron microscope and do not passed through the structure that the SQ-2 combustion adjuvant of acetone solution mixes with boron powder handset tool with graininess.Fig. 5 has showed the device syndeton of this method of testing; This device is based on the GR3500 type oxygen bomb formula calorimeter that Chinese state-run Changsha Instruments Factory makes, and the computer data acquiring imaging processing system that forms with parts such as thermopair, precision digital temperature-difference instrument, data collecting cards has replaced the Beckman thermometer amount temperature system of the artificial read-record of GR3500 Central Plains cause.
The present invention selected for use a kind of on existing oxygen bomb basis improved airtight burner, as shown in Figure 2, comprise body 1, it is that volume is 300 milliliters a thick cyclinder; Bullet 2 has needle valve system 12 on it, be tightly connected through insulator 13 and bullet 2, and electrode 14 is connected with needle valve system 12 through air inlet-outlet pipe, and electrode 14 is tightly connected with it through screw thread; Connect ignition wire 9 between electrode 4 and the electrode 14, ignition wire is the nichrome wire of diameter 0.1mm, and calorific value is 3.2J/cm.Sample 15 is the recombined sample medicinal strip of 3.0～4.5g, twines through ignition wire 9 to be suspended on directly over the crucible 7, is about 15mm apart from crucible bottom, and crucible 7 is supported in the oxygen bomb by crucible holder 8.
The present invention has adopted between new hybrid mode a part of a kind of oxidizer and boron powder sample and has mixed; As shown in Figure 3; In the gap of boron powder 17, with graininess and boron powder 17 simple mechanical mixture, intermolecular mixing is more even than SQ-2 combustion adjuvant 18 with the cross-linked structure compact arrangement for dissolved SQ-2 oxidizer 16; Tightr, the height of mechanical mixture show take pictures as shown in Figure 4.Among the present invention, carry out mechanical mixture to the oxidizer SQ-2 powder of crossing 80 order stainless steel sifts and boron powder sample with 15: 1 mass ratio, and stir; Then with micro-sprayer with acetone being sprayed on the mixed-powder sample gradually; The stirring that does not stop is treated that it bonds and is stopped the acetone of spraying when agglomerating, after stirring; Air-dryly fall volatile acetone it is solidified, cut the medicinal strip sample that is shaped like 5mm*5mm*15mm then.Adopt this hybrid mode, oxidizer SQ-2 and boron powder sample have reached the uniformity coefficient of mechanical mixture at least, and have the tightness degree of intermolecular mixing, help the perfect combustion of boron powder.
This method has been made the medicinal strip sample of 3.216g quality; The mass ratio 15: 1 of oxidizer SQ-2 and boron powder sample in this sample medicinal strip; Recording sample boron powder calorific value is 53.47MJ/Kg, and wherein the boron powder is 92 grades of boron powder that the north, Yingkou City Fine Chemical Works is produced, and products of combustion is a large amount of white powder B
2O
3And low amounts of water, there is not residue.Its theoretical calorific value of 92 grades of boron powder that Yingkou produces is 58.81*92%=54.12MJ/Kg; The actual measurement calorific value is 98.80% of a theoretical value; Compare with existing testing level top efficiency 81.68%; Boron powder actual measurement calorific value increase rate is bigger, and this test result is owing to the burning efficiency that has improved the boron powder improves, so this result's reliability is very high.This test experiments step is following:
1, will grow and be 300mm; Diameter is right cylinder standard SQ-2 solid propellant turning processing on lathe of 100mm, holds the cutter amount and is set to 1.0～0.6mm, collects the SQ-2 medicine bits that turning goes out; In ceramic mortar, grind; Filter with 80 purpose stainless steel sifts then, collect SQ-2 medicinal powder, as the combustion adjuvant of this experiment through the steel sieve.SQ-2 is classical double base propellant, and as the testing standard medicine of propellant, its theoretical calorific value is 11.2MJ/kg;
2, according to 15: 1 mixing quality ratio; Weighing 30.00g SQ-2 medicinal powder; Add 92 grades of boron powder that 2.00g is produced by the north, Yingkou City Fine Chemical Works again, grinding makes it become the big as far as possible mixed-powder sample of mechanical mixture uniformity coefficient in the mortar of suitable size; Pour the combined grinding sample glass beaker of 400ml into, and stir, with beaker, glass bar, mixed-powder sample weighing together and write down its gross mass M with the glass bar of long 200mm diameter 5mm
1=188.53g.
3, to use manual micro-sprayer be 99.9% standard acetone with mass concentration is sprayed on the mixed-powder with the speed of 4ml/s, constantly stirs with glass bar simultaneously, when treating all mixed-powder bonding patent medicine groups, stops the acetone of spraying.The consumption of making sure to keep in mind acetone in this step reaches the mixed-powder patent medicine group that bonds is got final product; If it is too much that acetone adds; The dissolved patent medicine slurry of SQ-2 particle in the mixed-powder, the boron powder particles that is insoluble to acetone can precipitate because density is bigger; Cause the mixing of sample inhomogeneous, can influence the collimation of experiment.
4, beaker, bonding medicine group and glass bar are placed on together that room temperature is that 23 ℃, humidity are 40%, in the room of the natural ventilation of windowing, acetone volatilizes 48 hours naturally, observation discovery medicine piece has cured.With the beaker that solidifies, bonding medicine group and glass bar weighing together and write down its gross mass M
2=188.89g, it is air-dry to think that bonding medicine group does not have, and acetone not volatilization finishes, and continues volatilization 48 hours; Weighing and write down its gross mass M once more
3=188.61g assert that bonding medicine group is air-dry basically, through calculating, learns still residual 0.08g acetone in the bonding medicine group of curing.
5, through calculating, the theoretical calorific value of 92 grades of boron powder is 54.12MJ/kg, the Calorimetry system of having demarcated before the experiment water equivalent be 15000J/K.Cut the sample medicinal strip that is shaped as 5mm*5mm*15mm from the bonding medicine group of air-dry curing, its quality is 3.216g, through calculating, learns and contains SQ-2 combustion adjuvant 3.0075g in this sample medicinal strip, contains boron powder sample 0.2005g, contains acetone 0.008g.Learn that through calculating SQ-2 combustion adjuvant thermal discharge is 336840J in this medicinal strip sample, the acetone thermal discharge is 246.8320J, writes down when these data are handled in order to late time data and uses.
6, measure that 15cm is long, calorific value is a 3.2J/cm nickel-cadmium ignition wire, delineate slit, 4 road, the ignition wire hoop is twined embed in the slit, again the ignition wire two ends are connected on the spark electrode of oxygen bomb head inner face with screw threads at medicinal strip specimen surface hoop to be measured.Deduction falls aphlogistic 2cm ignition wire length in the screw crack, and the calorific value that the burning of calculating ignition wire is emitted is 41.6J.
7, crucible is placed on the crucible holder, then crucible is put into oxygen bomb with crucible holder, the oxygen bomb lid is installed; Adjust the position of medicinal strip sample through crooked ignition wire; Make the medicinal strip sample that is suspended on oxygen bomb lid below be positioned at crucible directly over, guarantee that promptly medicinal strip sample freely falling body drops in the crucible, guaranteeing that ignition wire and medicinal strip sample do not touch under the prerequisite of oxygen bomb and crucible; Medicinal strip slips into 10mm in the crucible, tightens oxygen bomb and guarantees the oxygen bomb sealing.
8, the each several part system that connects and debug the calorimetric instrument with reference to figure 5,19 is the urceolus of Calorimetry system, interior filling has the distilled water of 9582.6g; 20 is the inner core of Calorimetry system, in the distilled water of 4321g is housed; The oxygen bomb system 21 that has assembled is submerged in the distilled water of inner core; 22 is electronic stirring system, by its switch of power controling box control; 23 for providing the priming supply of 20V DC voltage, controls the heating igniting of ignition wire in the oxygen bomb through the ignition signal line; 24 is the precision digital temperature-difference instrument, and the thermopair 25 that it is 0.001k that binding has two precision, the other end link computer data acquiring imaging processing system 26.
9, in the oxygen bomb that assembles, charge into the oxygen of 2.0MPa, then oxygen bomb is put into the distilled water of bucket, guarantee that oxygen bomb is submerged in the water fully, and connect with the spark electrode of firing cable with priming supply and oxygen bomb.Confirmed that through observing the oxygen bomb sealing is all right.
10, start electric mixer through power controling box, and start computer data acquiring imaging processing system, being provided with 5s is the temperature data of sampling time interval record inner/outer tube.
11, the temperature curve through computer data acquiring imaging processing software observes inner/outer tube, treat that the inner/outer tube system temperature reaches balance after, gather 72 groups of stable temperature datas, the initial stage temperature data of proofreading and correct as cooling; The switch of opening priming supply applies ignition signal, after the signal lamp indication ignition wire fusing of priming supply, closes priming supply.
12, observe the change curve of temperature data, the igniting back finds that the temperature curve of inner core sharply rises, and explains that the sample medicinal strip burns.After treating that the inner core temperature curve reaches maximal value, write down one section decrease of temperature segment data again, the temperature data in latter stage that cooling is proofreaied and correct during as data processing, descending branch decrease of temperature value is 0.274 ℃, this image data is effective.
13, through software systems, adopt cooling method of correcting temperature data internal, urceolus to carry out integration cooling treatment for correcting, the combustion heat value that finally obtains boron powder sample is 53.47MJ/Kg.The cleaning experimental facilities is opened the oxygen bomb lid, finds a large amount of white powder B
2O
3And low amounts of water, there is not residue, judge the perfect combustion of boron powder sample, this test result is effective.
Claims (1)
1. the measuring method of a boron powder combustion heat value is characterized in that comprising the steps:
(1) back is ground in the turning of SQ-2 propellant charge and filter with 80 order stainless steel sifts, it is subsequent use to collect the SQ-2 powder that sieves;
(2) pour beaker into after SQ-2 powder and boron powder sample are mixed with 10: 1～16: 1 mass ratio, use glass bar to stir pulverous mixture, make it become the uniform mixed-powder of mechanical mixture; With beaker, mixed-powder and glass bar weighing together and write down its gross mass M
1G;
(3) being 99.9% standard acetone with mass concentration is sprayed on the mixed-powder with the speed of 2～5ml/s, constantly stirs simultaneously, when treating all mixed-powder bonding patent medicine groups, stops the acetone of spraying;
(4) beaker, bonding medicine group and glass bar being placed on temperature together is in 20 ± 5 ℃, the indoor environment of humidity≤45%, and the acetone volatilization is done until bonding medicine Tuanfeng County; With air-dry beaker, bonding medicine group and glass bar weighing together and write down its gross mass M
2G;
If M
1-0.05≤M
2≤M
1+ 0.05, it is air-dry then to regard as bonding medicine group, and acetone has volatilized and finished;
If
, then think in the bonding medicine group acetone not volatilization finish, continue volatilization after air-dry 48 hours, if satisfy M
1-0.05≤M
2≤M
1+ 0.05, it is air-dry then to regard as bonding medicine group, and acetone has volatilized and finished; If do not satisfy M
1-0.05≤M
2≤M
1+ 0.05 but satisfy M
1+ 0.05≤M
2≤M
1+ 0.1, just assert has (M
2-M
1) acetone of g can't evaporate under existence conditions fully, then thinks the mass M of mixing medicine group
3=M
SQ-2+ M
Boron+ (M
2-M
1) g, wherein M
SQ-2Be the quality of SQ-2, M
BoronBe the quality of boron, (M
2-M
1) g is the acetone quality that remains in the sample; In the back during the data processing of test result, (M wherein
2-M
1) calorific value that produces of the acetone burning of g deducts as the calorific value of oxidizer, the combustion heat value that calculates the boron powder again gets final product;
(5) the medicine group of air-dry curing to be cut into some quality be 3.0～4.5g, be shaped as 5mm*5mm*15mm, and tolerance is the medicinal strip sample of 1mm, use to be tested;
(6) measure the ignition wire of the known calorific value of 10～20cm,, the ignition wire hoop twined embed in the slit, terminate on the spark electrode in the oxygen bomb head ignition wire two fixing again in medicinal strip specimen surface hoop delineation to be measured slit, 3～5 road;
(7) crucible is placed on the crucible holder; And crucible put into oxygen bomb with crucible holder; Installation oxygen bomb lid; Adjust the position of medicinal strip sample by crooked ignition wire; Make the medicinal strip sample that is suspended on oxygen bomb lid below be positioned at crucible directly over; Guarantee that promptly medicinal strip sample freely falling body drops in the crucible, the oxygen bomb lid will be tightened and guarantee sealing;
(8) the each several part system of connection and debugging calorimetric instrument, the distilled water of can 8000～10000g in the urceolus of Calorimetry system, the distilled water of can 4000～5000g in the inner core of Calorimetry system;
(9) after the oxygen bomb assembling, charge into the sufficient amount of oxygen that to guarantee sample perfect combustion, then oxygen bomb is put into the distilled water of bucket; Oxygen bomb can be immersed in the water fully; With firing cable priming supply is linked to each other with the electrode of oxygen bomb, observe the oxygen bomb lid seals at bubble situation in the inner core, if the bubble generating rate surpasses 3/minute words; Oxygen bomb gas leakage is described, is re-assemblied oxygen bomb and behind the oxygen bomb good seal, can carry out next step experiment;
(10) start electric mixer through power controling box, and setting is the temperature data of the inside and outside tube of sampling time interval record with 5s in computer data acquiring imaging processing system;
(11) first record initial stage temperature data; After treating that the inner/outer tube system temperature reaches balance; Gather 50～80 groups of stable temperature datas, just can apply ignition signal through the switch of priming supply, ignition wire is lighted the medicinal strip sample rapidly; After ignition wire was blown, the medicinal strip sample that is burning fell under gravity into and burns away in the crucible until burnouting;
(12) observe the change curve of temperature data, treat that the inner core temperature curve reaches maximal value after, cooling is proofreaied and correct and is used when writing down one section decrease of temperature segment data in order to data processing again, descending branch decrease of temperature value is not less than 0.2 ℃;
(13) adopt cooling method of correcting temperature data internal, urceolus to carry out integration cooling treatment for correcting, finally obtain the combustion heat value of boron powder sample.
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