CN110981666A - Smokeless and sulfur-free golden indoor setting-off type cold firework explosive and preparation method thereof - Google Patents
Smokeless and sulfur-free golden indoor setting-off type cold firework explosive and preparation method thereof Download PDFInfo
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- CN110981666A CN110981666A CN201911219298.4A CN201911219298A CN110981666A CN 110981666 A CN110981666 A CN 110981666A CN 201911219298 A CN201911219298 A CN 201911219298A CN 110981666 A CN110981666 A CN 110981666A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002360 explosive Substances 0.000 title claims description 34
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 43
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 39
- 239000000956 alloy Substances 0.000 claims abstract description 39
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 26
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims abstract description 18
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 16
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 16
- 241001330002 Bambuseae Species 0.000 claims abstract description 16
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 16
- 239000011425 bamboo Substances 0.000 claims abstract description 16
- 229920002678 cellulose Polymers 0.000 claims abstract description 16
- 239000001913 cellulose Substances 0.000 claims abstract description 16
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 13
- 239000003814 drug Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 13
- 238000004898 kneading Methods 0.000 claims abstract description 11
- 239000000693 micelle Substances 0.000 claims abstract description 11
- 229920001807 Urea-formaldehyde Polymers 0.000 claims abstract description 9
- 235000019359 magnesium stearate Nutrition 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000007873 sieving Methods 0.000 claims abstract description 8
- ZEYUSQVGRCPBPG-UHFFFAOYSA-N 4,5-dihydroxy-1,3-bis(hydroxymethyl)imidazolidin-2-one Chemical compound OCN1C(O)C(O)N(CO)C1=O ZEYUSQVGRCPBPG-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZGEJDJWVQDARMZ-UHFFFAOYSA-N prop-2-ene-1,1,2,3-tetrol urea Chemical compound NC(=O)N.OC(O)C(=CO)O ZGEJDJWVQDARMZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims description 28
- 239000002184 metal Substances 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 23
- 229910052802 copper Inorganic materials 0.000 claims description 23
- 239000010949 copper Substances 0.000 claims description 23
- 230000006698 induction Effects 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 13
- 229910052726 zirconium Inorganic materials 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 239000012043 crude product Substances 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 6
- 230000001680 brushing effect Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical compound [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 claims description 5
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 2
- 229940063655 aluminum stearate Drugs 0.000 claims description 2
- 238000009472 formulation Methods 0.000 claims description 2
- 239000000779 smoke Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000000446 fuel Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229920001220 nitrocellulos Polymers 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- GDDNTTHUKVNJRA-UHFFFAOYSA-N 3-bromo-3,3-difluoroprop-1-ene Chemical compound FC(F)(Br)C=C GDDNTTHUKVNJRA-UHFFFAOYSA-N 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 239000002085 irritant Substances 0.000 description 3
- 231100000021 irritant Toxicity 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 2
- 229910001092 metal group alloy Inorganic materials 0.000 description 2
- 238000005424 photoluminescence Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- MZFIXCCGFYSQSS-UHFFFAOYSA-N silver titanium Chemical compound [Ti].[Ag] MZFIXCCGFYSQSS-UHFFFAOYSA-N 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
- C06B33/08—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide with a nitrated organic compound
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0033—Shaping the mixture
- C06B21/0066—Shaping the mixture by granulation, e.g. flaking
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a preparation method of a smokeless sulfur-free golden indoor setting-off type cold firework medicament, and belongs to the field of environment-friendly pyrotechnic compositions. Weighing modified alloy type flame color agent, nitrated bamboo cellulose, magnesium stearate and dimethylol dihydroxy ethylene urea resin; adding the nitrated bamboo cellulose into polyethylene glycol, stirring, and adding magnesium stearate and dihydroxymethyl dihydroxy ethylene urea resin to obtain a solution A. And adding the modified golden flame agent into the solution A, stirring, drying and kneading to obtain a uniform micelle, granulating and drying to obtain a crude smokeless sulfur-free golden indoor setting-off type cold firework agent, and crushing and sieving to obtain the smokeless sulfur-free golden indoor setting-off type cold firework agent. The method of the invention is safe and reliable, has no toxic and harmful smoke, simple preparation process and no three-waste emission in the production process.
Description
Technical Field
The invention relates to a preparation method of a smokeless sulfur-free golden indoor setting-off type cold firework medicament, and belongs to the field of environment-friendly pyrotechnic compositions.
Background
The development of cold fireworks marks that the firework industry is advancing towards a new stage, has the advantages of environmental protection, low setting temperature and the like, is a new trend of the development of the firework industry in the future, and has strong competitiveness in the market.
Patent CN108218644A discloses a smokeless cool light firework explosive with fragrance, which comprises the following components: the cold light firework powder can achieve an ideal eruption effect by adjusting the proportion of the components of nitrocellulose, ferrocene, a stabilizer, essence and titanium powder, but the cold light firework powder disclosed by the patent has a single color in the setting off process and cannot achieve the effect of fantasy color.
For colorful cold light fireworks, there are some patents describing them. Patent CN103121886A discloses a colorful cold firework agent and a cold firework manufacturing method, and the agent comprises the following components: 20-30% of ammonium perchlorate, 20-30% of nitrocotton, 30-35% of silver titanium powder, 15-20% of photoluminescent material and 5-10% of fluororubber. However, the photoluminescence material can not achieve stable multicolor effect, and the white light has more variegated colors when the photoluminescence material is set off. Patent CN103030483A discloses a bright green cold firework explosive and a preparation method thereof, wherein the explosive comprises the following components in percentage by weight: 25-40% of boron powder, 5-15% of magnesium aluminum alloy powder, 6-12% of titanium powder, 8-15% of barium nitrate, 6-10% of 52# chlorinated paraffin, 15-20% of nitrocotton and 15-20% of ammonium perchlorate, and the preparation method of the medicament comprises the steps of fuel mixing, fuel granulation, fuel granule drying, medicament mixing and the like. The bright green cold firework powder prepared by the method is difficult to achieve complete and uniform mixing in the fuel mixing process, and the illusion-color effect is not ideal in the setting-off process. Patent CN109913697A discloses a metal alloy powder for multi-wavelength cold light fireworks and a preparation method thereof, the method takes metal zirconium as a main body, other metal combustible agents are added to prepare the metal alloy combustible agent, and the aim of coloring the cold light fireworks is achieved by adjusting the radiation wave band when the powder is burnt.
As is well known, the main components of the cold firework powder at present are ammonium perchlorate, sulfur, nitrocotton, low ignition point metal powder and the like. The burning of the powder can generate chloride, sulfide smoke and metal oxide dust, which can affect the health of human bodies and cause certain pollution to the environment; especially when the indoor is set off, the smoke release amount is large, the brightness effect is not obvious, the color is not bright or residues are generated, the counter feeling of audiences can be caused, and the joyous effect and the purpose of increasing the color can not be achieved. In addition, the lack of effective formula and preparation method of golden cold firework explosive in the market is a weak field for preparing cold firework explosive, and also limits the application diversity of cold firework explosive.
On the premise of ensuring the excellent setting-off effect of the cold fireworks, the environmental pollution and the harm to the human body caused by setting-off of the cold fireworks are reduced, the smoke release amount of the cold fireworks is effectively controlled, the gloss effect of the cold fireworks is enhanced, the hot spot problem and the key problem on the development road of the firework industry are solved, the cold fireworks are one of the main contradictions to be solved urgently in the whole firework industry, a certain demand is provided for the smokeless and sulfur-free performance and the luminous performance of the cold fireworks chemical, and the direction is pointed out for the development of the firework industry. Therefore, the prepared golden smokeless sulfur-free cold firework explosive has great social significance, practical significance and economic significance.
Disclosure of Invention
The invention aims to provide a preparation method of a smokeless sulfur-free golden indoor setting off type cold firework medicament, and realizes efficient preparation of the smokeless sulfur-free golden indoor setting off type cold firework medicament. The smokeless and sulfur-free golden indoor setting-off type cold firework explosive reserves the characteristics of low setting-off temperature and safe use of the existing cold firework explosive, does not generate irritant smoke in the setting-off process, increases golden magical color, and meets the market demand.
The purpose of the invention is realized by the following technical scheme.
A smokeless sulfur-free golden indoor setting off type cold firework medicament comprises the following components in percentage by mass:
the nitrogen content of the nitrated bamboo cellulose in the components is 12 to 12.5 percent;
a preparation method of a smokeless sulfur-free golden indoor setting-off type cold firework explosive comprises the following specific steps:
step one, weighing the modified alloy type flame color agent, the nitrated bamboo cellulose, the magnesium stearate and the dimethylol dihydroxy ethylene urea resin according to the formula mass ratio;
step two, adding the nitrated bamboo cellulose in the step one into polyethylene glycol, wherein the mass ratio of the nitrated bamboo cellulose to the polyethylene glycol is 1 (5-10), stirring the mixed solution at the speed of 60-100 rpm by using aluminum stearate, respectively adding magnesium stearate and dihydroxymethyl dihydroxy ethylene urea resin under the stirring state, and stirring for 30-60 minutes to obtain a solution A;
step three, adding the modified golden flame color agent obtained in the step one into the solution A under the stirring state of 60-100 rpm, stirring for 1-2 hours, and drying for 30-50 minutes in a cool and ventilated place; then kneading, wherein a proper amount of polyethylene glycol can be added in the kneading process, and the mixture is kneaded to form uniform micelle with moderate hardness;
the method for judging the moderate hardness comprises the following steps: extruding the paste through a 20-mesh copper net to form continuous thin strips which are not adhered to each other;
step four, granulating the uniform micelle with moderate hardness obtained in the step three by using a double-screw granulator, and drying for 12-24 hours at the temperature of 70-80 ℃ to obtain a smokeless sulfur-free golden indoor burning type cold firework explosive crude product;
and step five, crushing the crude alloy type golden cold firework explosive obtained in the step four by light pressure, sieving the crushed crude alloy type golden cold firework explosive through a 80-mesh copper sieve, removing screen remnants with too small particles, then sieving the crushed crude alloy type golden cold firework explosive through a 60-mesh copper sieve, and taking screen remnants of the 60-mesh copper sieve to obtain the smokeless and sulfur-free golden indoor burning type cold firework explosive with uniform particles.
The preparation method of the modified golden flame agent comprises the following steps:
firstly, brushing an oxide layer on the surface of a metal ingot A by using a steel brush, placing the metal ingot A in an ultrasonic cleaning instrument, cleaning by using absolute ethyl alcohol for 10-15 minutes, after cleaning, placing the metal ingot A in a condition of 40 ℃ for vacuum drying for 5-10 minutes, and then accurately weighing the metal ingot A;
step two, placing the metal ingot A obtained in the step one, the light generating agent and the light assisting agent at the bottom of a crucible of a vacuum induction furnace, wherein the mass ratio of the metal ingot A to the light generating agent is 1 (1-3), the mass ratio of the metal ingot A to the light assisting agent is 1 (1-3), sealing the vacuum induction furnace, starting a vacuum pump, and when the vacuum degree reaches 2.2 multiplied by 10-2～2.6×10-2After Pa, closing the vacuumizing port, heating, and preserving heat for 2-4 hours to obtain uniform alloy liquid after the temperature reaches 1870-2310 ℃;
and step three, under the protection of argon atmosphere, opening a flow guide pipe stop valve at the bottom of the crucible of the vacuum induction furnace, spraying the derived liquid by using high-pressure argon gas flow, atomizing the alloy liquid drops, cooling and solidifying the atomized liquid drops to form alloy powder, then feeding the alloy powder into a collecting tank, and sieving the alloy powder by using a 300-mesh copper sieve to obtain the modified golden flame toner larger than 300 meshes.
The pressure of the argon gas flow is 3-5 MPa;
in the first step, the metal ingot A is one of a zirconium ingot and a titanium ingot.
The purity of the metal ingot A in the first step is more than 99.8 percent.
The light-producing agent in the second step comprises the following components in percentage by weight:
54-73% of iron powder
10-15% of iron oxide
15-35% of manganic manganous oxide
And in the second step, the components of the light assisting agent comprise tin powder and aluminum powder, wherein the mass ratio of the tin powder to the aluminum powder is 1 (1.8-3.5).
Advantageous effects
1. A smokeless and sulfur-free golden indoor setting off type cold firework explosive adopts a modified golden flame colorant as a main component, and is safe and reliable; the components do not contain chlorine element and sulfur element, and no toxic and harmful smoke is generated;
2. the preparation method of the smokeless sulfur-free golden indoor setting-off type cold firework medicament has the advantages of simple process, few steps, no three-waste emission in the production process, suitability for flow line operation of factories, suitability for large-scale industrial production and remarkable economic and social benefits.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A smokeless sulfur-free golden indoor setting off type cold firework medicament comprises the following components in percentage by mass:
the nitrogen content of the nitrated bamboo cellulose in the components is 12 to 12.5 percent;
adding 400g of nitrated bamboo cellulose into 2000g of polyethylene glycol, stirring the mixed solution at the speed of 60rpm, respectively adding 140g of magnesium stearate and 60g of dimethylol dihydroxy ethylene urea resin under the stirring state, and stirring for 30 minutes to obtain a solution A;
brushing an oxide layer on the surface of a zirconium ingot by using a steel brush, putting the zirconium ingot into an ultrasonic cleaning instrument, cleaning by using absolute ethyl alcohol, after cleaning for 15 minutes, putting the zirconium ingot into a condition of 40 ℃ for vacuum drying for 5 minutes, and then weighing 320g of the zirconium ingot; placing 320g of zirconium ingot, 610g of light-producing agent and 670g of light-assisting agent at the bottom of a crucible of a vacuum induction furnace, sealing the vacuum induction furnace, starting a vacuum pump until the vacuum degree reaches 2.6 multiplied by 10-2After Pa, closing the vacuumizing port, heating, and preserving heat for 4 hours to obtain uniform alloy liquid after the temperature reaches 1940 ℃; under the protection of argon atmosphere, a flow guide pipe stop valve at the bottom of a crucible of the vacuum induction furnace is opened, 3MPa high-pressure argon gas flow is used for spraying the guided liquid, so that alloy liquid drops are atomized, the atomized liquid drops are cooled and solidified to form alloy powder, the alloy powder enters a collecting tank, and the alloy powder passes through a 300-mesh copper sieve to obtain 1487g of modified golden flame toner larger than 300 meshes.
The light-producing agent comprises the following components in percentage by weight:
iron powder 70%
10 percent of ferric oxide
Manganic manganous oxide 20%
The light assistant comprises tin powder and aluminum powder, wherein the mass ratio of the tin powder to the aluminum powder is 1: 1.9;
adding 1400g of the modified golden flame agent into the solution A under the stirring state of 60rpm, stirring for 1 hour, and then drying for 30 minutes in a cool and ventilated place; then kneading, wherein a proper amount of polyethylene glycol can be added in the kneading process, and the mixture is kneaded to form uniform micelle with moderate hardness;
granulating the obtained uniform micelle with moderate hardness by using a double-screw granulator, and drying for 12 hours at 70 ℃ to obtain 1880g of crude smokeless sulfur-free golden indoor setting-off type cold firework explosive;
1880g of the crude smokeless sulfur-free golden indoor setting-off type cold firework explosive is crushed by light pressure, then the crude product is sieved by a 80-mesh copper sieve, screen residue with too small particles is removed, then the crude product is sieved by a 60-mesh copper sieve, screen residue of the 60-mesh copper sieve is taken, and 1794g of smokeless sulfur-free golden indoor setting-off type cold firework explosive with uniform particles is obtained.
Example 2
A smokeless sulfur-free golden indoor setting off type cold firework medicament comprises the following components in percentage by mass:
the nitrogen content of the nitrated bamboo cellulose in the components is 12 to 12.5 percent;
adding 2.04kg of nitrated bamboo cellulose into 12.24kg of polyethylene glycol, stirring the mixed solution at the speed of 70rpm, respectively adding 0.6kg of magnesium stearate and 0.36kg of dimethylol dihydroxy ethylene urea resin under the stirring state, and stirring for 30 minutes to obtain a solution A;
brushing an oxide layer on the surface of a zirconium ingot by using a steel brush, putting the zirconium ingot into an ultrasonic cleaning instrument, cleaning by using absolute ethyl alcohol, after cleaning for 15 minutes, putting the zirconium ingot into a condition of 40 ℃ for vacuum drying for 5 minutes, and then weighing 2.04kg of the zirconium ingot; placing 2.04kg zirconium ingot, 3.58kg light generating agent and 4.58kg light assistant agent at the bottom of a crucible of a vacuum induction furnace, sealing the vacuum induction furnace, starting a vacuum pump until the vacuum degree reaches 2.6 multiplied by 10-2After Pa, closing the vacuumizing port, heating, and preserving heat for 3 hours to obtain uniform alloy liquid after the temperature reaches 1885 ℃; under the protection of argon atmosphere, a flow guide pipe stop valve at the bottom of a crucible of the vacuum induction furnace is opened, 4MPa high-pressure argon gas flow is used for spraying the guided liquid, so that alloy liquid drops are atomized, the atomized liquid drops are cooled and solidified to form alloy powder, the alloy powder enters a collecting tank, and the alloy powder passes through a 300-mesh copper sieve to obtain 9.24kg of modified golden flame toner larger than 300 meshes.
The light-producing agent comprises the following components in percentage by weight:
iron powder 65%
13 percent of ferric oxide
Manganic manganous oxide 22%
The light assistant comprises tin powder and aluminum powder, wherein the mass ratio of the tin powder to the aluminum powder is 1: 2.7;
adding 9kg of modified golden flame agent into the solution A under the stirring state of 70rpm, stirring for 1 hour, and then drying for 30 minutes in a cool and ventilated place; then kneading, wherein a proper amount of polyethylene glycol can be added in the kneading process, and the mixture is kneaded to form uniform micelle with moderate hardness;
granulating the obtained uniform micelle with moderate hardness by using a double-screw granulator, and drying for 12 hours at 70 ℃ to obtain 11.61kg of smokeless sulfur-free golden indoor burning type cold firework explosive crude product;
the method comprises the steps of crushing 11.61kg of crude smokeless sulfur-free golden indoor burning type cold firework explosive under light pressure, screening the crude product through a 80-mesh copper screen, removing screen residues with too small particles, screening the crude product through a 60-mesh copper screen, and taking screen residues of the 60-mesh copper screen to obtain 11.23kg of smokeless sulfur-free golden indoor burning type cold firework explosive with uniform particles, wherein the burning point of the cold firework explosive is as low as 73 ℃, the external temperature in the burning process is lower than 36 ℃, no irritant gas is generated during burning, bright golden magical colors appear, and no increase of sulfur element is found in indoor air sampling detection after burning, so that the market demand is met.
Example 3
A smokeless sulfur-free golden indoor setting off type cold firework medicament comprises the following components in percentage by mass:
the nitrogen content of the nitrated bamboo cellulose in the components is 12 to 12.5 percent;
adding 3.5kg of nitrated bamboo cellulose into 18.3kg of polyethylene glycol, stirring the mixed solution at the speed of 100rpm, respectively adding 0.7kg of magnesium stearate and 0.7kg of dimethylol dihydroxy ethylene urea resin under the stirring state, and stirring for 40 minutes to obtain a solution A;
brushing an oxide layer on the surface of a titanium ingot by using a steel brush, putting the titanium ingot into an ultrasonic cleaning instrument, cleaning by using absolute ethyl alcohol, after cleaning for 15 minutes, putting the titanium ingot at 40 ℃ for vacuum drying for 5 minutes, and then weighing 2.52kg of the titanium ingot; placing 2.52kg titanium ingot, 5.04kg light generating agent and 2.52kg light assistant agent at the bottom of a crucible of a vacuum induction furnace, sealing the vacuum induction furnace, starting a vacuum pump until the vacuum degree reaches 2.6 multiplied by 10-2After Pa, closing the vacuumizing port, heating, and preserving heat for 4 hours to obtain uniform alloy liquid after the temperature reaches 2185 ℃; under the protection of argon atmosphere, a flow guide pipe stop valve at the bottom of a crucible of the vacuum induction furnace is opened, 4MPa high-pressure argon gas flow is used for spraying the guided liquid, so that alloy liquid drops are atomized, the atomized liquid drops are cooled and solidified to form alloy powder, the alloy powder enters a collecting tank, and the alloy powder passes through a 300-mesh copper sieve to obtain 9.94kg of modified golden flame toner larger than 300 meshes.
The light-producing agent comprises the following components in percentage by weight:
iron powder 54%
11 percent of ferric oxide
Manganic manganous oxide 35%
The light assistant comprises tin powder and aluminum powder, wherein the mass ratio of the tin powder to the aluminum powder is 1: 3.2;
adding 9.1kg of modified golden flame agent into the solution A under the stirring state of 80rpm, stirring for 1 hour, and then drying for 50 minutes in a cool and ventilated place; then kneading, wherein a proper amount of polyethylene glycol can be added in the kneading process, and the mixture is kneaded to form uniform micelle with moderate hardness;
granulating the obtained uniform micelle with moderate hardness by using a double-screw granulator, and drying for 12 hours at the temperature of 80 ℃ to obtain 13.62kg of smokeless sulfur-free golden indoor burning type cold firework explosive crude product;
13.62kg of crude smokeless sulfur-free golden indoor burning type cold firework explosive is crushed by light pressure, then the crude product is sieved by a 80-mesh copper sieve, screen residue with too small particles is removed, then the crude product is sieved by a 60-mesh copper sieve, and screen residue of the 60-mesh copper sieve is taken, so that 12.57kg of smokeless sulfur-free golden indoor burning type cold firework explosive with uniform particles is obtained, the burning point of the cold firework explosive is as low as 77 ℃, the external temperature in the burning process is lower than 35 ℃, no irritant gas is generated during burning, bright golden magical color appears, and no increase of sulfur element is found by sampling and detecting indoor air after burning, so that the market demand is met.
The above detailed description is intended to illustrate the objects, aspects and advantages of the present invention, and it should be understood that the above detailed description is only exemplary of the present invention and is not intended to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. A smokeless sulfur-free golden indoor setting off type cold firework medicament comprises the following components in percentage by mass:
the preparation method of the modified golden flame agent comprises the following steps:
firstly, brushing an oxide layer on the surface of a metal ingot A by using a steel brush, placing the metal ingot A in an ultrasonic cleaning instrument, cleaning by using absolute ethyl alcohol for 10-15 minutes, after cleaning, placing the metal ingot A in a condition of 40 ℃ for vacuum drying for 5-10 minutes, and then accurately weighing the metal ingot A;
step two, placing the metal ingot A obtained in the step one, the light generating agent and the light assisting agent at the bottom of a crucible of a vacuum induction furnace, wherein the mass ratio of the metal ingot A to the light generating agent is 1 (1-3), the mass ratio of the metal ingot A to the light assisting agent is 1 (1-3), sealing the vacuum induction furnace, starting a vacuum pump, and when the vacuum degree reaches 2.2 multiplied by 10-2～2.6×10-2After Pa, closing the vacuumizing port, heating, and preserving heat for 2-4 hours to obtain uniform alloy liquid after the temperature reaches 1870-2310 ℃;
and step three, under the protection of argon atmosphere, opening a flow guide pipe stop valve at the bottom of the crucible of the vacuum induction furnace, spraying the derived liquid by using high-pressure argon gas flow, atomizing the alloy liquid drops, cooling and solidifying the atomized liquid drops to form alloy powder, then feeding the alloy powder into a collecting tank, and sieving the alloy powder by using a 300-mesh copper sieve to obtain the modified golden flame toner larger than 300 meshes.
2. The medicament of claim 1, wherein: the nitrogen content of the nitrified bamboo cellulose is 12-12.5%.
3. The method of preparing the smokeless sulfur-free golden indoor setting off type cold firework formulation of claim 1, wherein: the method comprises the following specific steps:
step one, weighing the modified alloy type flame color agent, the nitrated bamboo cellulose, the magnesium stearate and the dimethylol dihydroxy ethylene urea resin according to the formula mass ratio;
step two, adding the nitrated bamboo cellulose in the step one into polyethylene glycol, wherein the mass ratio of the nitrated bamboo cellulose to the polyethylene glycol is 1 (5-10), stirring the mixed solution at the speed of 60-100 rpm by using aluminum stearate, respectively adding magnesium stearate and dihydroxymethyl dihydroxy ethylene urea resin under the stirring state, and stirring for 30-60 minutes to obtain a solution A;
step three, adding the modified golden flame color agent obtained in the step one into the solution A under the stirring state of 60-100 rpm, stirring for 1-2 hours, and drying for 30-50 minutes in a cool and ventilated place; then kneading, wherein a proper amount of polyethylene glycol can be added in the kneading process, and the mixture is kneaded to form uniform micelle with moderate hardness;
step four, granulating the uniform micelle with moderate hardness obtained in the step three by using a double-screw granulator, and drying for 12-24 hours at the temperature of 70-80 ℃ to obtain a smokeless sulfur-free golden indoor burning type cold firework explosive crude product;
and step five, crushing the crude alloy type golden cold firework explosive obtained in the step four by light pressure, sieving the crushed crude alloy type golden cold firework explosive through a 80-mesh copper sieve, removing screen remnants with too small particles, then sieving the crushed crude alloy type golden cold firework explosive through a 60-mesh copper sieve, and taking screen remnants of the 60-mesh copper sieve to obtain the smokeless and sulfur-free golden indoor burning type cold firework explosive with uniform particles.
4. The method of claim 3, wherein: the method for judging the moderate hardness comprises the following steps: after the paste is extruded through a 20-mesh copper net, the paste is formed into continuous thin strips which are not adhered to each other.
5. The method of claim 3, wherein: the preparation method of the modified golden flame agent comprises the following steps:
firstly, brushing an oxide layer on the surface of a metal ingot A by using a steel brush, placing the metal ingot A in an ultrasonic cleaning instrument, cleaning by using absolute ethyl alcohol for 10-15 minutes, after cleaning, placing the metal ingot A in a condition of 40 ℃ for vacuum drying for 5-10 minutes, and then accurately weighing the metal ingot A;
step two, placing the metal ingot A obtained in the step one, the light generating agent and the light assisting agent at the bottom of a crucible of a vacuum induction furnace, wherein the mass ratio of the metal ingot A to the light generating agent is 1 (1-3), the mass ratio of the metal ingot A to the light assisting agent is 1 (1-3), sealing the vacuum induction furnace, starting a vacuum pump, and when the vacuum degree reaches 2.2 multiplied by 10-2～2.6×10-2After Pa, closing the vacuumizing port, heating, and preserving heat for 2-4 hours to obtain uniform alloy liquid after the temperature reaches 1870-2310 ℃;
opening a flow guide pipe stop valve at the bottom of a crucible of the vacuum induction furnace under the protection of argon atmosphere, spraying the derived liquid by using high-pressure argon gas flow to atomize alloy liquid drops, cooling and solidifying the atomized liquid drops to form alloy powder, then feeding the alloy powder into a collecting tank, and sieving the alloy powder by using a 300-mesh copper sieve to obtain a modified golden flame toner larger than 300 meshes;
the argon gas flow pressure is 3-5 MPa.
6. The method of claim 5, wherein: in the first step, the metal ingot A is one of a zirconium ingot and a titanium ingot.
7. The method of claim 5 or 6, wherein: the purity of the metal ingot A in the first step is more than 99.8 percent.
8. The method of claim 5, wherein: the light-producing agent in the second step comprises the following components in percentage by weight:
54-73% of iron powder
10-15% of iron oxide
15-35% of manganic manganous oxide.
9. The method of claim 5, wherein: and in the second step, the components of the light assisting agent comprise tin powder and aluminum powder, wherein the mass ratio of the tin powder to the aluminum powder is 1 (1.8-3.5).
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| CN111923271A (en) * | 2020-08-04 | 2020-11-13 | 北京理工大学 | Granulation process method of nitrified bamboo cellulose |
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