CN101844955A - Method for sensitizing microporous smokeless firework explosive - Google Patents
Method for sensitizing microporous smokeless firework explosive Download PDFInfo
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- CN101844955A CN101844955A CN 201010178439 CN201010178439A CN101844955A CN 101844955 A CN101844955 A CN 101844955A CN 201010178439 CN201010178439 CN 201010178439 CN 201010178439 A CN201010178439 A CN 201010178439A CN 101844955 A CN101844955 A CN 101844955A
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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 the method for sensitizing of luxuriant technology, particularly a kind 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, be 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, 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 situations 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 by 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, in the microporous smokeless firework explosive preparation process or in last handling process, be incorporated into the sensitizing agent of suitable proportion in the medicine grain in some way, 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 by sensitization.And, the microporous smokeless firework explosive sensitization improves its ignition characteristic by 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, obtain being suspended in the medicine grain in the solution with little pore, the medicine grain with little pore that is suspended in the solution is separated, the medicine grain of separating from the solution of suspension medicine grain 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 separating from the solution of suspension medicine grain.Sensitizing agent is one or more a mixture of nitrate, perchlorate, can be nitrate, the perchlorate of basic metal or alkaline-earth 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, 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.Add in the military smokeless powder of scrapping before the solvent, can add a spot of water earlier or the aqueous solution disperses, reunite and bond on wall 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 ethyl 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 determines that according to raw material type and granular size dissolution time is 10-180min under room temperature or heating condition, is preferably 20-90min; Solvent temperature is determined 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 ethyl 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; Described emulsion foam process can be finished in the balling-up reactor, described balling-up reactor is the reactor of general installation anchor formula, oar blade type or spiral stirring rake, and the stirring velocity in the emulsion foam process is determined according to the volume of balling-up reactor 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 described aqueous solution as emulsification foaming agent or foam stabilizer, to guarantee that material disperses and the emulsion foam state is more even, described tensio-active agent can be a nonionic surface active agent, as alkylphenol office oxygen Vinyl Ether; Can also be aniorfic surfactant, as sodium lauryl sulphate or Sodium dodecylbenzene sulfonate etc.; Can also select cationic surfactant for use, as Dodecyl trimethyl ammonium chloride, cetyl trimethylammonium bromide etc.The add-on of tensio-active agent determines 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 described 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 determine that the tap density that needs is little, and then the water-soluble liquid measure of Jia Ruing should increase, but the add-on by volume of the aqueous solution is no more than the solvent cumulative volume.Carry out emulsion foam under room temperature or heating condition, 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 substantially; Temperature should keep 40 ℃-68 ℃ when adopting ethyl acetate to make solvent, is preferably 50 ℃-65 ℃.
The emulsion foam process can also be finished in emulsifying device, and as 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 finished.
(3) balling-up: in lacquer shape emulsion, add the aqueous solution, under whipped state, contain nitrocellulosic organic phase material because the effect of interfacial tension forms spherical droplets; The described aqueous solution can be the aqueous solution that contains dispersion agent, can also be the mother liquor that medicine grain moulding last time preparation 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, polyacrylamide, polyvinyl alcohol, 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 substantially, keeps 40 ℃-68 ℃ when adopting ethyl acetate solvent, 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 determined 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 to carry out under higher stirring velocity, otherwise then need carry out under low stirring velocity.
(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 described 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 that surpasses the boiling point of solvent or solvent and water when temperature is more than 10 ℃ the time, keeps can stopping to drive more than the 10min molten.When adopting ethyl acetate to make solvent, if it is molten to 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 the solvent expeling is finished, by the general type of cooling temperature of system is dropped near room temperature, or directly the aqueous solution is separated with solid particulate by common centrifugation or filtering mode, the filtrate of separating is called the balling-up mother liquor, contain 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, perchlorate, can be nitrate, the perchlorate of basic metal or alkaline-earth 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 determined 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 finish oven dry under the state of vacuumizing, vacuum tightness is determined 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 broken, the control particle diameter 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, whipped state adds 10 times down to the ethyl acetate solvent of drug grain quality, 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 that adds is 6 times of drug grain quality, 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 after temperature is raised to 85 ℃, continuing to stir 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, similarly do not adding preparation contrast sample 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 broken, the control particle diameter 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, whipped state adds 10 times down to the ethyl acetate solvent of drug grain quality, 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 that adds is 6 times of drug grain quality, 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 behind the continuation stirring 10min filters out ball after temperature is raised to 85 ℃.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 | The contrast sample | ??0 | ??41.7 |
| The sensitizing agent kind | Addition | Fire transmission rate | |
| 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 nitroglycerine 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%, 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 | The contrast 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;
(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.
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, perchlorate.
4. the method for sensitizing of microporous smokeless firework explosive according to claim 3 is characterized in that, sensitizing agent is nitrate, the perchlorate of basic metal or alkaline-earth 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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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101784395A CN101844955B (en) | 2010-05-21 | 2010-05-21 | Method for sensitizing microporous smokeless firework explosive |
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| CN2010101784395A CN101844955B (en) | 2010-05-21 | 2010-05-21 | Method for sensitizing microporous smokeless firework explosive |
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| CN101844955B CN101844955B (en) | 2012-06-06 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570480A (en) * | 2013-11-01 | 2014-02-12 | 南京理工大学 | Ultrafine dispersion method of water-soluble oxidizing agent in energetic composite material |
| CN105384589A (en) * | 2015-10-16 | 2016-03-09 | 南京理工大学 | Slight smoke type tricolor fireworks powder particles and application |
| CN115259977A (en) * | 2021-04-30 | 2022-11-01 | 南京理工大学 | Preparation method of loose-structure nitrocotton base powder for environment-friendly fireworks |
| CN116041122A (en) * | 2022-12-20 | 2023-05-02 | 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2010
- 2010-05-21 CN CN2010101784395A patent/CN101844955B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570480A (en) * | 2013-11-01 | 2014-02-12 | 南京理工大学 | Ultrafine dispersion method of water-soluble oxidizing agent in energetic composite material |
| CN105384589A (en) * | 2015-10-16 | 2016-03-09 | 南京理工大学 | Slight smoke type tricolor fireworks powder particles and application |
| 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 |
| CN115259977A (en) * | 2021-04-30 | 2022-11-01 | 南京理工大学 | Preparation method of loose-structure nitrocotton base powder for environment-friendly fireworks |
| 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 |
| CN116041122A (en) * | 2022-12-20 | 2023-05-02 | 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 |
| 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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