CN101844955B - Method for sensitizing microporous smokeless firework explosive - Google Patents
Method for sensitizing microporous smokeless firework explosive Download PDFInfo
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- CN101844955B CN101844955B CN2010101784395A CN201010178439A CN101844955B CN 101844955 B CN101844955 B CN 101844955B CN 2010101784395 A CN2010101784395 A CN 2010101784395A CN 201010178439 A CN201010178439 A CN 201010178439A CN 101844955 B CN101844955 B CN 101844955B
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Abstract
The invention discloses a method for sensitizing microporous smokeless firework explosive, which comprises the following steps of: dissolving scrapped military smokeless explosive containing nitrated cellulose into a solvent to form macromolecular sol, emulsifying and foaming the sol to form paint emulsion, dispersing the paint emulsion into a non-solvent medium under stirring action to form balls, then driving the solvent to obtain explosive particles suspended in the solution and provided with micropores, separating the explosive particles suspended in the solution and provided with micropores, sensitizing the explosive particles separated from the solution of the suspended explosive particles and provided with micropores, and drying the explosive particles to obtain an explosive particle finished product, wherein the sensitizing mode is to add a sensitizing agent into the explosive particles separated from the solution of the suspended explosive particles in a form of aqueous solution or solid. The sensitizing process improves the fire transfer speed of the explosive particles and improves the ignition performance thereof, and the fire transfer speed of the explosive particles is improved by 10 to 200 percent under a normal pressure condition.
Description
Technical field
The invention belongs to fireworks propelling charge and fireworks display and flick bud technology, particularly a kind of method for sensitizing of microporous smokeless firework explosive.
Background technology
The military smokeless powder that to scrap is that useless gunpowder is carried out pulverization process as fireworks with the propelling charge main method, if the granularity of medicine grain is too big after the pulverization process, is easy to generate residual medicine; Result of use is not ideal enough, but the gunpowder that will give up is crushed to below 100 orders, and difficulty is bigger; Production efficiency is also lower, has the high inadequately defective of combustion speed, replace black gunpowder comprehensively under normal pressure and the low pressure condition in addition; A lot of situation are to mix with black powder to use, and can't thoroughly solve the denseer problem of smog.
Adopt the solvent method thoroughly moulding again after the dissolving of gunpowder of will giving up; Be prepared into smoke less fire cracker medicine with micro-pore structure; Combustionvelocity and fire transmission rate increase substantially, but owing to almost do not have solid components in the products of combustion, compare ignition characteristic with black powder and also have a certain distance.
Summary of the invention
The object of the present invention is to provide a kind of safe, reliable, pollution-free, method for sensitizing of microporous smokeless firework explosive cheaply.
The technical solution that realizes the object of the invention may further comprise the steps:
(1) material dissolution: under whipped state, will contain and nitrocellulosicly scrap military smokeless powder and be dissolved into and form polymeric sol in the solvent;
(2) emulsion foam: water or the aqueous solution joined carry out emulsion foam in the material, form lacquer shape emulsion;
(3) balling-up: in lacquer shape emulsion, add the aqueous solution, under whipped state, contain nitrocellulosic organic phase material and form spherical droplets, add an amount of dispersion agent drop is protected;
(4) solvent is driven away: the intensification conditioned disjunction vacuumizes under the state, perhaps progressively solvent is distilled heating up and vacuumize under the condition simultaneously;
(5) feed separation: solvent after driving away end is separated the particulate state medicine grain that obtains;
(6) sensitization is handled: the medicine grain of separating in the step (5) with little pore is carried out sensitization handle;
(7) oven dry: adopt conventional method to dry processing the solid medicine grain, obtain the finished medicines grain.
Prepare at solvent method and to introduce the sensitizing agent that can improve its igniting property in the moulding process of little pore fireworks medicine, sensitizing agent will be adsorbed onto in the surface and internal void of medicine grain in medicine grain oven dry back.Sensitizing agent can all be dissolved in the aqueous solution, and through osmosis absorption or be distributed in the fireworks medicine particle, sensitizing agent will be retained in the hole and the surface of sample after medicine grain drying.
The present invention compared with prior art; Its remarkable advantage: 1) utilize the inventive method; The sensitizing agent of suitable proportion is prepared in the process or in last handling process, is incorporated in the medicine grain in some way at microporous smokeless firework explosive; Improved the fire transmission rate of medicine grain and improved its ignition characteristic, the fire transmission rate under its condition of normal pressure improves 10%-200%.2) the smoke less fire cracker propelling charge after the sensitization processing is used to do spraying decoration, ground fireworks display and display shell propelling charge, but the traditional black powder of replacing whole, dosage is far below traditional black powder explosive load, and consumption can reduce 50%-80% than black powder consumption.
Embodiment
The present invention handles the fire transmission rate that increases substantially microporous smokeless firework explosive through sensitization.And, the microporous smokeless firework explosive sensitization improves its ignition characteristic through being handled.
At first will contain and nitrocellulosicly scrap military smokeless powder and be dissolved into and form polymeric sol in the solvent; Form lacquer shape emulsion through emulsion foam again; And under stirring action, will coat with lacquer the balling-up in the non-solvent medium of shape emulsion dispersion; Then solvent is driven away, obtained being suspended in the medicine grain in the solution, the medicine grain with little pore that is suspended in the solution is separated with little pore; The medicine grain of from the solution of suspension medicine grain, separating with little pore is carried out sensitization handle, oven dry afterwards obtains the finished medicines grain; The mode that sensitization is handled is that form or the solid form of sensitizing agent with the aqueous solution joined in the medicine grain of from the solution of suspension medicine grain, separating.Sensitizing agent is one or more a mixture of nitrate salt, perchlorate, can be nitrate salt, the perchlorate of basic metal or earth alkali metal, perhaps ammoniumper chlorate.The quality of sensitizing agent is the 0.2-10% of bulk drug quality.Be specially:
(1) material dissolution: under whipped state, will contain and nitrocellulosicly scrap military smokeless powder and be dissolved into and form polymeric sol in the solvent; At first, will contain the nitrocellulosic military smokeless powder of scrapping and join in material dissolution groove or the balling-up reactor drum, the 3-15 solvent doubly that adds the bulk drug quality carries out material dissolution.Under whipped state, bulk drug adopts solvent dispersion and dissolving to form polymeric sol in molding device.In the military smokeless powder of scrapping, add before the solvent, can add a spot of water earlier or the aqueous solution disperses, reunite and on wall, bond to prevent material, the ratio that institute adds the water or the aqueous solution is 0-2 times of useless gunpowder quality.Solvent for use can be a kind of in ETHYLE ACETATE, butylacetate, acetone, butanone, ethanol, the methyl alcohol or several mixture, preferably select for use to bulk drug have good solubility can solvent; The material dissolution time confirms that according to raw material type and particle size dissolution time is 10-180min under room temperature or heating condition, is preferably 20-90min; Solvent temperature is confirmed according to used solvent species, should not be higher than the azeotropic point of the boiling point or the mixed solvent of solvent; When adopting ETHYLE ACETATE to make solvent, solvent temperature is preferably at 40-68 degree centigrade, and 50-65 degree centigrade better; The dissolution process of material also can not add the water or the aqueous solution and directly adopt dissolution with solvents.The adding of material dissolution process bulk drug and solvent can once add or repeatedly add in batches, can adopt independent dissolver batch process in addition or prepare continuously to contain the polymeric sol of scrapping military smokeless powder.
(2) emulsion foam: water or the aqueous solution joined carry out emulsion foam in the material, form lacquer shape emulsion; Said emulsion foam process can be accomplished in the balling-up reactor drum; Said balling-up reactor drum is the reactor drum of general installation anchor formula, oar blade type or spiral stirring rake, and the stirring velocity in the emulsion foam process is confirmed according to the volume of balling-up reactor drum and the type of agitating vane.In the emulsion foam process; Under whipped state, in polymeric sol, add the entry or the aqueous solution; Can add tensio-active agent in the said aqueous solution as emulsification foaming agent or foam stabilizer; To guarantee that material disperses and the emulsion foam state is more even, said tensio-active agent can be a non-ionics, like alkylphenol office oxygen Vinyl Ether; Can also be aniorfic surfactant, like sodium lauryl sulphate or X 2073 etc.; Can also select cationic surfactant for use, like DTAC, cetyl trimethylammonium bromide etc.The add-on of tensio-active agent confirms that according to its kind add-on is preferably the 0.01%-0.2% of the water yield for adding the 0.01%-0.5% of the water yield usually.The adding of the said water or the aqueous solution can once add or repeatedly add, and can also add continuously.The emulsion foam process joins the aqueous solution in the system, can also be isolated mother liquor after balling-up last time.The add-on of the aqueous solution can finished product tap density as required confirm that the tap density that needs is little, and the water-soluble liquid measure that then adds should increase, but the add-on by volume of the aqueous solution is no more than the solvent TV.Under room temperature or heating condition, carry out emulsion foam, the temperature of heating is not higher than the azeotropic point of the boiling point or the mixed solvent of solvent, and the emulsion foam time is preferably 10min-240min; The temperature of emulsion foam process system is consistent with dissolution process basically; Temperature should keep 40 ℃-68 ℃ when adopting ETHYLE ACETATE to make solvent, is preferably 50 ℃-65 ℃.
The emulsion foam process can also be accomplished in emulsifying device, and like various intermittences or continuous emulsifying equipment, material changed over to and carries out the balling-up processing in the balling-up equipment after emulsion foam was accomplished.
(3) balling-up: in lacquer shape emulsion, add the aqueous solution, under whipped state, contain nitrocellulosic organic phase material because the effect of IT forms spherical droplets; The said aqueous solution can be the aqueous solution that contains dispersion agent, can also be that medicine grain moulding last time prepares the mother liquor that process reclaims, and adds an amount of dispersion agent in the aqueous solution spherical droplets is protected to prevent mutual gathering.The amount that the aqueous solution or mother liquor add is 2-10 a times of bulk drug quality, can disposablely add, and also can add in batches.Dispersion agent can also directly be added in the system in the balling-up process.The kind of dispersion agent can be selected water-soluble natural polymers such as gelatin, gelatine, gum arabic for use, also can select water-soluble synthetic macromolecules such as polyoxyethylene glycol, SEPIGEL 305, Z 150PH, methylcellulose gum for use.Dispersant dosage is for adding the 0.05%-2% of total usefulness quality, preferably 0.05%-1%.Used time of balling-up process, 20min-60min was better preferably at 10min-90min; System temperature is consistent with dissolution process basically, when adopting ethyl acetate solvent, keeps 40 ℃-68 ℃, is preferably 50 ℃-65 ℃, and the balling-up process temperature can slowly promote, but should not surpass the boiling point of solvent for use.Stirring velocity is confirmed according to the volume of balling head, the shape of agitating vane and the medicine particle size of needs, needs the finished medicines grain of small particle size under higher stirring velocity, to carry out, otherwise then need under low stirring velocity, carry out.
(4) solvent is driven away: the intensification conditioned disjunction vacuumizes under the state, perhaps progressively solvent is distilled heating up and vacuumize under the condition simultaneously; The main operating parameters that said solvent is driven away process is: the time is at 20min-240min, and temperature is along with the recovery of solvent progressively improves, and the azeotropic point of boiling point or solvent and water that surpasses solvent when temperature can stop to drive molten more than 10 ℃ the time more than the maintenance 10min.When adopting ETHYLE ACETATE to make solvent, to dissolve if adopt normal pressure to steam, temperature reaches 85 ℃ and keeps can stopping to drive more than the 10min molten.
(5) feed separation: solvent after driving away end is separated the particulate state medicine grain that obtains; After solvent is driven away completion; Through the general type of cooling temperature of system is dropped near room temperature; Or directly through common spinning or filtering mode the aqueous solution is separated with solid particulate, the filtrating of separating is called the balling-up mother liquor, contains a spot of dispersion agent and solvent in the mother liquor; Can be saved in the fixed container when next balling-up as the dispersion medium recycle, also can concentrate through handling qualified back qualified discharge.
(6) sensitization is handled: the medicine grain of separating in the step (5) with little pore is carried out sensitization handle; The mode that sensitization is handled is for to join form or the solid form of sensitizing agent with the aqueous solution in the medicine grain with little pore.Sensitizing agent is one or more a mixture of nitrate salt, perchlorate, can be nitrate salt, the perchlorate of basic metal or earth alkali metal, perhaps ammoniumper chlorate.Add sensitizing agent quality be the 0.2-10% of bulk drug quality.If sensitizing agent adds with aqueous solution form, the concentration of solution is confirmed according to its solubleness size in water, but must be guaranteed that sensitizing agent all dissolves, and can make it to be distributed to more equably in the medicine grain like this.
(7) oven dry: adopt conventional method to dry processing the solid medicine grain, obtain the finished medicines grain.Used drying plant preferably adopts warm air, hot water etc. as the heating thermal source, and top temperature is preferably lower than 100 ℃, should not adopt the direct-fired baking oven of naked light and electrothermal tube, to guarantee safety.Also can under the state of vacuumizing, accomplish oven dry, vacuum tightness is confirmed according to solvent species.When moisture content is following less than 2%, can stop oven dry.Can also adopt the continuous drying device processes.About the oven dry and dehydration equipment the good anti-static measure should be arranged to guarantee safety.
Below in conjunction with embodiment the present invention is done further detailed description:
Embodiment 1:
Adopting the nitrocotton cellulose content is bulk drug greater than the basic useless gunpowder of 85% list, through preliminary fragmentation, controls particle diameter and is no more than 3mm; Wet medicine grain and 2 times of water to drug grain quality of band water are joined in the molding device, and whipped state adds 10 times to the ethyl acetate solvent of drug grain quality down, stirring and dissolving 30-60min under 45 ℃ of-50 ℃ of temperature; The tap water that in 30min, adds in the system continuously then; Under whipped state, carry out the emulsion foam operation, the water yield of adding is 6 times of drug grain quality, and after water injection 30min is continued to stir in the back under 50-60 ℃ of temperature; When system temperature is adjusted to 65 ℃-68 ℃; 5 times of aqueous dispersants that contain to the bulk drug quality are joined and disperse balling-up in the system, and gelatin is as dispersion agent, and the add-on of gelatin is 0.5% of a water total mass.Continue to keep 65 ℃-68 ℃ of temperature, and under the mixing speed of 300-350rpm, disperse the 30min clock, contain nitrocellulosic micelle and progressively be dispersed into spherical drop uniformly.Then, progressively heating up steams solvent to come lentamente, and ball hardens gradually.After temperature is raised to 85 ℃ of continued stirring 10min, the solid medicine grain is filtered out.Next carrying out sensitization handles; Press 0.2% of bulk drug quality and in wet medicine grain, add the saltpetre powder; The granularity of saltpetre powder is 100 order screen underflows, and with sample 50 ℃ of dryings 24 hours in the safety baking oven, the sample tap density that obtains is 0.18g.cm behind the mixing
-3Adopting internal diameter is the paper web of 16mm height 200mm one end sealing; Choose and light test after the part filling of 20-40 order size range and pass rate at top speed; Record and pass at top speed that rate is 42mm/s, likewise prepare comparison sample not adding under the sensitizing agent condition, the sample tap density that obtains is 0.17g.cm
-3, the biography of same particle size scope rate at top speed is 36mm/s.
Embodiment 2:
Adopting the nitrocotton cellulose content is bulk drug greater than the basic useless gunpowder of 85% list, through preliminary fragmentation, controls particle diameter and is no more than 3mm; Wet medicine grain and 2 times of water to drug grain quality of band water are joined in the molding device, and whipped state adds 10 times to the ethyl acetate solvent of drug grain quality down, stirring and dissolving 30-60min under 45 ℃ of-50 ℃ of temperature; The tap water that in 30min, adds in the system continuously then; Under whipped state, carry out the emulsion foam operation, the water yield of adding is 6 times of drug grain quality, and after water injection 30min is continued to stir in the back under 50-60 ℃ of temperature; When system temperature is adjusted to 65 ℃-68 ℃; 5 times of aqueous dispersants that contain to the bulk drug quality are joined and disperse balling-up in the system, and gelatin is as dispersion agent, and the add-on of gelatin is 0.5% of a water total mass.Continue to keep 65 ℃-68 ℃ of temperature, and under the mixing speed of 300-350rpm, disperse 30min, contain nitrocellulosic micelle and progressively be dispersed into spherical drop uniformly.Then, progressively heating up steams solvent to come lentamente, and ball hardens gradually.Discharging after temperature is raised to 85 ℃ of continued to stir 10min filters out ball.Next carrying out sensitization handles; 1.0% saltpetre that will be equivalent to the bulk drug quality is made into 10% the aqueous solution; Again this saltpetre aqueous solution and medicine grain are mixed and carry out sensitization and handle, then the medicine grain was obtained final sample down in dry 24 hours in 50 ℃ in the safety baking oven.Adopting internal diameter is the paper web of 16mm height 200mm one end sealing, directly loads the medicine grain after sensitization is handled, and lights test and passes rate at top speed, records to pass at top speed that rate is 48mm/s.
Embodiment 3-9
Adopt the technological process identical with embodiment 1; Adopting the nitrocotton cellulose content is that raw material carries out specimen preparation greater than the basic useless gunpowder of 85% list; Only be that solvent adding amount is reduced to 6 times of drug grain quality, the water yield that the emulsion foam operating process adds reduces to 4 times of drug grain quality.Adopting different sensitizing agents to carry out sensitization handles; Adding proportion is 5%, and the adding mode contrasts the fire transmission rate of gained sample for different sensitizing agents is made into the aqueous solution; And the sample that same not sensitization is handled compares test result such as following table (25 ℃ of probe temperatures).At last, the sample tap density that obtains is 0.24g.cm
-3, particle diameter mainly concentrates on 300-2000um, filters out 20 orders-40 purpose after the oven dry and partly fires the speed test.
| The sensitizing agent kind | Addition | Fire transmission rate | |
| Embodiment 3 | Comparison sample | 0 | 41.7 |
| Embodiment 4 | Potassium perchlorate | 5％ | 48.0 |
| Embodiment 5 | Saltpetre | 5％ | 56.9 |
| Embodiment 6 | Strontium nitrate | 5％ | 45.9 |
| Embodiment 7 | Nitrate of baryta | 5％ | 43.5 |
| Embodiment 8 | Potassium perchlorate and mixture of potassium nitrate, mass ratio 1: 1 | 5％ | 50.0 |
| Embodiment 9 | Ammoniumper chlorate and mixture of potassium nitrate, mass ratio 1: 1 | 5％ | 65.4 |
Embodiment 10-17
Adopt the technological process identical with embodiment 1; Adopting the useless gunpowder of double-basis of soup content 20% and nitrocotton cellulose content 75% is raw material; Adopting different sensitizing agents to carry out sensitization handles; Adding proportion is 5% and 10%, and the adding mode is for to be made into the aqueous solution with different sensitizing agents, and the sample tap density that makes is 0.25g.cm
-3, filter out 20 orders-40 purpose and partly contrast its fire transmission rate, and compare test result such as following table (8 ℃ of probe temperatures) with the sample of not sensitization processing.
| The sensitizing agent kind | Addition | Fire transmission rate | |
| Embodiment 10 | Comparison sample | 0 | 15.5 |
| Embodiment 11 | Potassium perchlorate | 5％ | 32.1 |
| Embodiment 12 | Saltpetre | 5％ | 33.0 |
| Embodiment 13 | Strontium nitrate | 5％ | 25.9 |
| Embodiment 14 | Nitrate of baryta | 5％ | 22.7 |
| Embodiment 15 | Ammoniumper chlorate | 5％ | 38.2 |
| Embodiment 16 | Saltpetre | 10％ | 48.0 |
| Embodiment 17 | Ammoniumper chlorate | 10％ | 52.4 |
Claims (5)
1. the method for sensitizing of a microporous smokeless firework explosive is characterized in that, may further comprise the steps:
(1) material dissolution: under whipped state, will contain and nitrocellulosicly scrap military smokeless powder and be dissolved into and form polymeric sol in the solvent;
(2) emulsion foam: water or the aqueous solution joined carry out emulsion foam in the material, form lacquer shape emulsion, the said aqueous solution is the aqueous solution of tensio-active agent;
(3) balling-up: in lacquer shape emulsion, add the aqueous solution; Under whipped state, contain nitrocellulosic organic phase material and form spherical droplets; Add an amount of dispersion agent drop is protected, the said aqueous solution is that the aqueous solution or medicine grain moulding last time that contain dispersion agent prepare the mother liquor that process reclaims;
(4) solvent is driven away: the intensification conditioned disjunction vacuumizes under the state, perhaps progressively solvent is distilled heating up and vacuumize under the condition simultaneously;
(5) feed separation: solvent after driving away end is separated the particulate state medicine grain that obtains;
(6) sensitization is handled: the medicine grain of separating in the step (5) with little pore is carried out sensitization handle;
(7) oven dry: adopt conventional method to dry processing the solid medicine grain, obtain the finished medicines grain.
2. the method for sensitizing of microporous smokeless firework explosive according to claim 1 is characterized in that, the sensitization that step (6) is carried out is handled and is specially: form or the solid form of sensitizing agent with the aqueous solution joined in the medicine grain with little pore.
3. the method for sensitizing of microporous smokeless firework explosive according to claim 2 is characterized in that, sensitizing agent is one or more a mixture of nitrate salt, perchlorate.
4. the method for sensitizing of microporous smokeless firework explosive according to claim 3 is characterized in that, sensitizing agent is nitrate salt, the perchlorate of basic metal or earth alkali metal, perhaps ammoniumper chlorate.
5. according to the method for sensitizing of claim 2,3 or 4 described microporous smokeless firework explosives, it is characterized in that the quality of sensitizing agent is the 0.2-10% of bulk drug quality.
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| CN103570480B (en) * | 2013-11-01 | 2015-09-30 | 南京理工大学 | The super-refinement dispersing method of a kind of water-soluble oxidizers in composite material containing energy |
| CN105384589B (en) * | 2015-10-16 | 2017-12-08 | 南京理工大学 | A kind of micro- cigarette type three primary colours cigarette pollen grains and application |
| CN115259977B (en) * | 2021-04-30 | 2023-09-05 | 南京理工大学 | Preparation method of loose-structure nitrocotton base powder for environment-friendly fireworks |
| CN116041122B (en) * | 2022-12-20 | 2024-02-23 | 本溪钢铁（集团）矿业有限责任公司 | Method for controlling residual explosive in ground station matrix bin of emulsion explosive |
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| CN1526687A (en) * | 2003-09-22 | 2004-09-08 | 中国北方化学工业总公司 | Smokeless gun propellant for fireworks and its prepn |
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