CN111039734A - Safe smokeless and sulfur-free cold firework chemical and preparation method thereof - Google Patents
Safe smokeless and sulfur-free cold firework chemical and preparation method thereof Download PDFInfo
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- CN111039734A CN111039734A CN201911255862.8A CN201911255862A CN111039734A CN 111039734 A CN111039734 A CN 111039734A CN 201911255862 A CN201911255862 A CN 201911255862A CN 111039734 A CN111039734 A CN 111039734A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000126 substance Substances 0.000 title description 8
- 239000000843 powder Substances 0.000 claims abstract description 82
- TZRXHJWUDPFEEY-UHFFFAOYSA-N Pentaerythritol Tetranitrate Chemical class [O-][N+](=O)OCC(CO[N+]([O-])=O)(CO[N+]([O-])=O)CO[N+]([O-])=O TZRXHJWUDPFEEY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002360 explosive Substances 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 229920002678 cellulose Polymers 0.000 claims abstract description 20
- 239000001913 cellulose Substances 0.000 claims abstract description 20
- ADCBKYIHQQCFHE-UHFFFAOYSA-N 1,3-dimethyl-1,3-diphenylurea Chemical compound C=1C=CC=CC=1N(C)C(=O)N(C)C1=CC=CC=C1 ADCBKYIHQQCFHE-UHFFFAOYSA-N 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004697 Polyetherimide Substances 0.000 claims abstract description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 10
- YCOWFDCCOFCZPM-UHFFFAOYSA-N n,n'-dihydroxyoxamide Chemical compound ONC(=O)C(=O)NO YCOWFDCCOFCZPM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920001601 polyetherimide Polymers 0.000 claims abstract description 10
- 239000000779 smoke Substances 0.000 claims abstract description 10
- 239000011593 sulfur Substances 0.000 claims abstract description 10
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 10
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 8
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 8
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 8
- XKORCTIIRYKLLG-ARJAWSKDSA-N methyl (z)-3-aminobut-2-enoate Chemical compound COC(=O)\C=C(\C)N XKORCTIIRYKLLG-ARJAWSKDSA-N 0.000 claims abstract description 8
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims abstract description 8
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 35
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000011259 mixed solution Substances 0.000 claims description 30
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 29
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 29
- 241001330002 Bambuseae Species 0.000 claims description 29
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 29
- 239000011425 bamboo Substances 0.000 claims description 29
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 21
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 17
- 229910052802 copper Inorganic materials 0.000 claims description 17
- 239000010949 copper Substances 0.000 claims description 17
- 239000012043 crude product Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 239000007921 spray Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 238000004898 kneading Methods 0.000 claims description 13
- 239000000693 micelle Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002216 antistatic agent Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 239000000026 Pentaerythritol tetranitrate Substances 0.000 claims description 9
- 239000000853 adhesive Substances 0.000 claims description 9
- 230000001070 adhesive effect Effects 0.000 claims description 9
- 239000003814 drug Substances 0.000 claims description 9
- 229960004321 pentaerithrityl tetranitrate Drugs 0.000 claims description 9
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000007822 coupling agent Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000009472 formulation Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 9
- 238000002485 combustion reaction Methods 0.000 abstract description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000460 chlorine Substances 0.000 abstract description 5
- 229910052801 chlorine Inorganic materials 0.000 abstract description 5
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 239000007800 oxidant agent Substances 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 description 6
- 230000008901 benefit Effects 0.000 description 4
- 239000004568 cement Substances 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- GDDNTTHUKVNJRA-UHFFFAOYSA-N 3-bromo-3,3-difluoroprop-1-ene Chemical compound FC(F)(Br)C=C GDDNTTHUKVNJRA-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 239000002699 waste material 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
- C06B21/0008—Compounding the ingredient
-
- 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 safe smokeless and sulfur-free cold firework explosive and a preparation method thereof, belonging to the field of environment-friendly pyrotechnic compositions. The components comprise: nano-magnesia-alumina powder, modified pentaerythritol tetranitrate, nitrobamboo cellulose, dihydroxy glyoxime, dimethyl diphenyl urea, zinc stearate, polyetherimide, ethyl cellulose, methyl 3-aminocrotonate and graphene. The invention adopts the nano magnesium-aluminum powder and the modified pentaerythritol tetranitrate powder as the main components, has low combustion temperature, and is safe and reliable; and the dihydroxyl glyoxime is introduced as an oxidant to ensure full combustion; the components do not contain chlorine element and sulfur element, so that no toxic and harmful smoke is generated; by adopting the polyetherimide and introducing the dimethyl diphenyl urea and the graphene, the compatibility and the mechanical property of the cold firework powder can be effectively improved, the antistatic capability and the safety performance of the cold firework powder are obviously improved, the safety and the reliability of the cold firework powder are ensured, and the cold firework powder has an excellent setting-off effect; and has excellent setting off effect.
Description
Technical Field
The invention relates to a safe smokeless and sulfur-free cold firework explosive and a preparation method thereof, belonging to the field of environment-friendly pyrotechnic compositions.
Background
When the cold firework is developed very rapidly, the environment-friendly and pollution-free firework is popular and hot for consumers. Moreover, the cold firework is a new trend of development of the future firework industry, and the development of the cold firework has strong market competitiveness; whether in large fireworks evening, wedding ceremony, stage sculpts, or in bars, KTVs, there are shadows of cold fireworks. The cold fireworks have wide market prospect and huge economic benefit.
The main components of the cold firework powder at present are ammonium perchlorate, nitrocotton, low ignition point metal powder and the like. Due to the strong oxidizing property and static electricity of the components, a plurality of potential safety hazards are brought, and the life and property safety of people is threatened. In recent years, various blasting accidents and serious safety accidents are caused due to the low stability and low stability of cold firework powder; moreover, the burning of the powder can generate chloride smoke and metal oxide dust, which can affect the normal function of human body and cause certain pollution to the environment; under the condition of larger smoke release amount, even more, the discomfort of audiences or guests can be caused, and the joyous effect and the purpose of increasing the color can not be achieved. Zhang Ming, Zhang Heng bin through designing the eruption and the controlling means of a colored cold fireworks, and adopt multiple metal powder to mix as the raw materials and replace the powder of generally using, and then effectively avoid the potential safety hazard and the air pollution that cold fireworks probably exist (CN201611057463.7), but the use of a large amount of metal powder and insufficient combustion have led to a large amount of metal oxide dusts, it is unfavorable to health and environmental protection, and it has only improved factor of safety through the additional device in the process of putting off of burning of cold fireworks, do not solve the problem from this source of cold fireworks explosive, the improvement of the security performance of cold fireworks still needs to arouse the attention of fireworks personage.
On the premise of ensuring the excellent firework effect of the cold firework, the environment pollution and the harm to the human body caused by the setting off of the cold firework are reduced, the safety performance is improved, and the potential safety hazard is eliminated, so that the main contradiction to be solved urgently in the whole firework industry is solved, the hot spot problem and the key problem on the development road of the firework industry are solved, certain requirements on the smoke and sulfur free and safety performance of the cold firework agent are provided, and the direction is pointed out for the development of the firework industry. Therefore, the provided safe smokeless and sulfur-free cold firework explosive and the preparation method thereof have great social, practical and economic significance.
Disclosure of Invention
The invention provides a safe smokeless and sulfur-free cold firework explosive and a preparation method thereof, aiming at solving the problems of smoke pollution and static accumulation after the conventional cold firework explosive is set off.
The purpose of the invention is realized by the following technical scheme.
The safe smokeless and sulfur-free cold firework explosive comprises the following components in percentage by mass:
the average grain diameter of the nano-magnesium-aluminum powder in the components is 100nm, wherein the mass percent of the nano-aluminum powder is 60 percent, and the mass percent of the nano-magnesium powder is 40 percent;
the nitrogen content of the nitrated bamboo cellulose in the components is 12 to 12.5 percent;
a preparation method of a stable-shaped smokeless and sulfur-free cold firework explosive comprises the following specific steps:
weighing nano magnesium-aluminum powder, modified pentaerythritol tetranitrate, nitrated bamboo cellulose, dihydroxy glyoxime, dimethyl diphenyl urea, zinc stearate, polyetherimide, ethyl cellulose, methyl 3-aminocrotonate and graphene according to the mass ratio of the formula;
step two, dividing the nitrated bamboo cellulose powder weighed in the step one into A, B groups according to the mass ratio of (1-5) to (10), dissolving the nitrated bamboo cellulose powder of the group A in ethyl acetate according to the mass ratio of 1:10, and stirring for 2-3 hours under the ultrasonic dispersion condition; then, continuously adding the methyl 3-aminocrotonate powder and the zinc stearate powder weighed in the step one under the stirring state, and uniformly stirring to obtain a mixed solution of the nitrated bamboo cellulose;
step three, mixing the polyetherimide particles, the ethyl cellulose powder and the graphene powder weighed in the step one to obtain a mixture D; adding the mixture D into an N-methyl pyrrolidone solution according to the mass ratio of 1:10, and stirring for 1-2 hours in an ultrasonic dispersion state to obtain a mixed solution E; then transferring the mixed solution E into a spray gun to prepare antistatic agent spray liquid;
step four, adding the modified pentaerythritol tetranitrate powder, the dihydroxy glyoxime powder and the B group of the nitrated bamboo cellulose obtained in the step two into the nitrated bamboo cellulose mixed sol obtained in the step two under the stirring and ultrasonic dispersion states, and uniformly mixing; uniformly spraying the antistatic agent spray liquid prepared in the third step for 3-7 times, and uniformly mixing once every time; then adding the dimethyl diphenyl urea powder and the nano-magnesia-alumina powder weighed in the step one into the mixture to be uniformly mixed; then kneading, wherein a proper amount of ethyl acetate 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, airing the obtained uniform micelle in a cool and ventilated place to be half-dry, and transferring the obtained uniform micelle into a blast oven at the temperature of 80-90 ℃ for drying for 2-3 hours to obtain a crude product of the safe and shaped smokeless and sulfur-free cold firework medicament;
and fifthly, crushing the crude product of the safe smokeless and sulfur-free cold firework explosive obtained in the fourth step by light pressure, sieving the crushed product through a 60-mesh copper sieve, removing screen residues with too small particles, then sieving the crushed product through a 30-mesh copper sieve, and taking the screen residues of the 30-mesh copper sieve to obtain the safe smokeless and sulfur-free cold firework explosive with uniform particles.
The preparation method of the modified pentaerythritol tetranitrate comprises the following steps: adding pentaerythritol tetranitrate powder and a titanate coupling agent into acetone according to the mass ratio of 1 (0.05-0.08) to 10, and performing ultrasonic dispersion for 30-50 minutes to obtain a mixed solution C; transferring the mixed solution C into an ice-water bath for stirring; then adding the polyvinyl butyral adhesive into the mixed solution C (wherein the mass ratio of pentaerythritol tetranitrate powder to the polyvinyl butyral adhesive is 1 (0.02-0.03)), and stirring for 3-5 hours; transferring the reaction device into an oil bath pan at the temperature of 60-80 ℃, standing for 20-40 minutes, and recovering the volatilized acetone; filtering, repeatedly washing for 3-5 times by using deionized water, and drying for 2-3 hours in a blast oven at 80-100 ℃; taking out, crushing under light pressure to obtain modified pentaerythritol tetranitrate powder;
the method for judging the moderate hardness comprises the following steps: after the micelle-shaped objects are extruded to pass through a 20-mesh copper sieve, the micelle-shaped objects are in a continuous thin strip shape, are not adhered with each other and have certain plasticity and tensile strength;
advantageous effects
1. The safe and stable smokeless sulfur-free cold firework powder adopts nano magnesium-aluminum powder and modified pentaerythritol tetranitrate powder as main components, has low combustion temperature, and is safe and reliable; and the dihydroxyl glyoxime is introduced as an oxidant to ensure full combustion; the components do not contain chlorine element and sulfur element, so that no toxic and harmful smoke is generated, and the preparation of the smokeless and sulfur-free cold firework explosive can be really realized;
2. the polyether imide is adopted, and the dimethyl diphenyl urea and the graphene are introduced, so that the compatibility and the mechanical property of the cold firework powder can be effectively improved, the antistatic capability and the safety performance of the cold firework powder are obviously improved, the safety and the reliability of the cold firework powder are ensured, and the cold firework powder has an excellent setting-off effect;
3. the preparation method of the safe and stable smokeless and sulfur-free cold firework explosive has the advantages of simple process, few steps, easily available raw materials, no three-waste discharge 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 described in detail with reference to examples.
Example 1
The safe smokeless and sulfur-free cold firework explosive comprises the following components in percentage by mass:
42.52g of nitrated bamboo cellulose powder is divided into A, B groups, wherein the A group is 12.52g, the B group is 30g, the nitrated bamboo cellulose powder of the A group is dissolved in 125.2g of ethyl acetate, the mixture is stirred for 2 hours under the ultrasonic dispersion condition, then 4.15g of 3-aminocrotonic acid methyl ester powder and 8.30g of zinc stearate powder are added under the stirring state, and the mixture is stirred uniformly to prepare a nitrated bamboo cellulose mixed sol;
adding 79g of pentaerythritol tetranitrate powder and 5.53g of titanate coupling agent into 790g of acetone, and performing ultrasonic dispersion for 35 minutes to obtain a mixed solution C; transferring the mixed solution C into an ice-water bath for stirring; then adding 1.62g of polyvinyl butyral adhesive into the mixed solution C, and stirring for 4 hours; transferring the reaction device into an oil bath kettle at the temperature of 75 ℃, standing for 30 minutes, and recovering the volatilized acetone; filtering, repeatedly washing with deionized water for 3 times, and drying in a 90 deg.C forced air oven for 2.5 hr; taking out, crushing by light pressure to obtain 81.49g of modified pentaerythritol tetranitrate powder;
mixing 7.14g of polyetherimide particles, 8.21g of ethylcellulose powder and 0.44g of graphene powder to obtain a mixture D; adding the mixture D into 157.9g of N-methylpyrrolidone solution, and stirring for 1.5 hours under an ultrasonic dispersion state to obtain a mixed solution E; then transferring the mixed solution E into a spray gun to prepare antistatic agent spray liquid;
under the stirring and ultrasonic dispersion state, adding 79.35g of modified pentaerythritol tetranitrate powder, 40.13g of dihydroxy glyoxime powder and B group of nitrated bamboo cellulose into the nitrated bamboo cellulose mixed sol, and uniformly mixing; then spraying antistatic agent spray liquid for 3 times, and uniformly mixing once every time; then adding 7.14g of dimethyl diphenyl urea powder and 117.12g of nano magnesium-aluminum powder into the mixture and uniformly mixing; then kneading, adding 13ml of ethyl acetate in the kneading process, and kneading until the mixture is a uniform micelle with moderate hardness;
granulating the uniform paste by using a double-screw granulator, airing the paste to be half-dry in a cool and ventilated place, and then transferring the paste to a blast oven at the temperature of 80 ℃ for drying for 2 hours to prepare 312.65g of a crude product of the setting smokeless and sulfur-free cold firework explosive;
312.65g of the crude product of the security-type smokeless sulfur-free cold firework medicament is lightly pressed and crushed, then the crude product is sieved by a 60-mesh copper sieve, the residue of the sieve with too small particles is removed, then the crude product is sieved by a 30-mesh copper sieve, the residue of the 30-mesh copper sieve is taken, and 310.47g of the security-type smokeless sulfur-free cold firework medicament with uniform particles is prepared, and the yield reaches 99.30%.
Tests show that the obtained safe smokeless sulfur-free cold firework explosive has 17% of impact sensitivity (the drop height is 250 +/-1 mm, the drop weight mass is 10.0 +/-0.1 kg), and 19% of friction sensitivity (the gauge pressure is 3.92MPa, the sample mass is 30mg, and the swing angle is 90 degrees); the finished product of the cold firework is freely dropped on a flat cement ground from a height of 12m, so that the phenomena of combustion, explosion and leakage of chemicals are avoided, and the safety performance is excellent; the ignition temperature of the prepared cold firework finished product is normal, the burning-off effect is excellent, the measured sound level value is 56dB, no sulfur and chlorine substances are discharged in the burning-off process, no residue is splashed, and the environment-friendly requirement of no smoke and no sulfur is met.
Example 2
The safe smokeless and sulfur-free cold firework explosive comprises the following components in percentage by mass:
dividing 8.63kg of nitrated bamboo cellulose powder into A, B groups, wherein the A group is 2.63kg, the B group is 6kg, dissolving the A group of nitrated bamboo cellulose powder in 26.3kg of ethyl acetate, stirring for 2.5 hours under the ultrasonic dispersion condition, then continuously adding 1.81kg of 3-aminocrotonic acid methyl ester powder and 3.21kg of zinc stearate powder under the stirring state, and uniformly stirring to obtain a nitrated bamboo cellulose mixed sol;
adding 20kg of pentaerythritol tetranitrate powder and 1.32kg of titanate coupling agent into 200kg of acetone, and performing ultrasonic dispersion for 35 minutes to obtain a mixed solution C; transferring the mixed solution C into an ice-water bath for stirring; then adding 0.5kg of polyvinyl butyral adhesive into the mixed solution C, and stirring for 3.5 hours; transferring the reaction device into an oil bath kettle at the temperature of 80 ℃, standing for 35 minutes, and recovering the volatilized acetone; filtering, repeatedly washing with deionized water for 4 times, and drying in a forced air oven at 85 deg.C for 3 hr; taking out, crushing under light pressure to obtain 21.04kg of modified pentaerythritol tetranitrate powder;
mixing 2.44kg of polyetherimide particles, 0.97kg of ethylcellulose powder and 0.2kg of graphene powder to obtain a mixture D; adding the mixture D into 36.1kg of N-methyl pyrrolidone solution, and stirring for 1.8 hours under an ultrasonic dispersion state to obtain a mixed solution E; then transferring the mixed solution E into a spray gun to prepare antistatic agent spray liquid;
under the stirring and ultrasonic dispersion state, adding 20.35kg of modified pentaerythritol tetranitrate powder, 10.41kg of dihydroxy glyoxime powder and B group of nitrated bamboo cellulose into the nitrated bamboo cellulose mixed sol, and uniformly mixing; then spraying antistatic agent spray liquid for 5 times, and uniformly mixing once every time; then 2.73kg of dimethyl diphenyl urea powder and 26.58kg of nano magnesium-aluminum powder are added and mixed evenly; then kneading, adding 1720ml of ethyl acetate in the kneading process, and kneading until the mixture is a uniform micelle with moderate hardness;
granulating the uniform paste by using a double-screw granulator, airing the paste to be half-dry in a cool and ventilated place, and then transferring the paste to a blast oven at 82 ℃ for drying for 2.7 hours to prepare 77.16kg of a stable smokeless and sulfur-free cold firework explosive crude product;
77.16kg of the crude product of the security-type smokeless sulfur-free cold firework medicament is lightly pressed and crushed, then the crude product is sieved by a 60-mesh copper sieve, the residue of the sieve with too small particles is removed, then the crude product is sieved by a 30-mesh copper sieve, the residue of the 30-mesh copper sieve is taken, and the security-type smokeless sulfur-free cold firework medicament with uniform particles is prepared, wherein the yield reaches 99.62%.
Tests show that the obtained safe smokeless sulfur-free cold firework explosive has 18% of impact sensitivity (the drop height is 250 +/-1 mm, the drop weight mass is 10.0 +/-0.1 kg), and 22% of friction sensitivity (the gauge pressure is 3.92MPa, the sample mass is 30mg, and the swing angle is 90 degrees); the finished product of the cold firework is freely dropped on a flat cement ground from a height of 12m, so that the phenomena of combustion, explosion and leakage of chemicals are avoided, and the safety performance is excellent; the ignition temperature of the prepared cold firework finished product is normal, the burning-off effect is excellent, the measured sound level value is 58dB, no sulfur and chlorine substances are discharged in the burning-off process, no residue is splashed, and the environment-friendly requirement of no smoke and no sulfur is met.
Example 3
The safe smokeless and sulfur-free cold firework explosive comprises the following components in percentage by mass:
dividing 26.81kg of nitrated bamboo cellulose powder into A, B groups, wherein the A group is 8.81kg, the B group is 18kg, dissolving the A group of nitrated bamboo cellulose powder in 88.1kg of ethyl acetate, stirring for 3 hours under the ultrasonic dispersion condition, then continuously adding 3.25kg of 3-aminocrotonic acid methyl ester powder and 4.85kg of zinc stearate powder under the stirring state, and uniformly stirring to obtain a nitrated bamboo cellulose mixed sol;
adding 55kg of pentaerythritol tetranitrate powder and 2.75kg of titanate coupling agent into 550kg of acetone, and performing ultrasonic dispersion for 50 minutes to obtain a mixed solution C; transferring the mixed solution C into an ice-water bath for stirring; then adding 1.25kg of polyvinyl butyral adhesive into the mixed solution C, and stirring for 4 hours; transferring the reaction device into an oil bath kettle at 78 ℃, standing for 40 minutes, and recovering the volatilized acetone; filtering, repeatedly washing with deionized water for 5 times, and drying in a 90 deg.C forced air oven for 2 hr; taking out, crushing under light pressure to obtain 55.87kg of modified pentaerythritol tetranitrate powder;
mixing 5.02kg of polyetherimide particles, 4.10kg of ethylcellulose powder and 0.43kg of graphene powder to obtain a mixture D; adding the mixture D into 95.5kg of N-methyl pyrrolidone solution, and stirring for 1.3 hours under an ultrasonic dispersion state to obtain a mixed solution E; then transferring the mixed solution E into a spray gun to prepare antistatic agent spray liquid;
under the stirring and ultrasonic dispersion states, 55.41kg of modified pentaerythritol tetranitrate powder, 20.34kg of dihydroxy glyoxime powder and B group of nitrated bamboo cellulose are added into the nitrated bamboo cellulose mixed sol and mixed uniformly; then spraying antistatic agent spray liquid for 5 times, and uniformly mixing once every time; then 8.67kg of dimethyl diphenyl urea powder and 59.13kg of nano magnesium-aluminum powder are added and mixed evenly; then kneading, adding 2110ml ethyl acetate in the kneading process, and kneading until the mixture is a uniform micelle with moderate hardness;
granulating the uniform paste by using a double-screw granulator, airing the paste to be half-dry in a cool and ventilated place, and then transferring the paste to a blast oven at 87 ℃ for drying for 2.8 hours to prepare 186.47kg of a stable smokeless and sulfur-free cold firework explosive crude product;
186.47kg of the crude product of the security-type smokeless sulfur-free cold firework medicament is lightly pressed and crushed, then the crude product is sieved by a 60-mesh copper sieve, the residue of the sieve with too small particles is removed, then the crude product is sieved by a 30-mesh copper sieve, the residue of the 30-mesh copper sieve is taken, and the 185.32kg of security-type smokeless sulfur-free cold firework medicament with uniform particles is prepared, and the yield reaches 99.38%.
Tests show that the obtained safe smokeless sulfur-free cold firework explosive has 17% of impact sensitivity (the drop height is 250 +/-1 mm, the drop weight mass is 10.0 +/-0.1 kg), and 20% of friction sensitivity (the gauge pressure is 3.92MPa, the sample mass is 30mg, and the swing angle is 90 degrees); the finished product of the cold firework is freely dropped on a flat cement ground from a height of 12m, so that the phenomena of combustion, explosion and leakage of chemicals are avoided, and the safety performance is excellent; the ignition temperature of the prepared cold firework finished product is normal, the burning-off effect is excellent, the measured sound level value is 57dB, no sulfur and chlorine containing substances are discharged in the burning-off process, no residue is splashed, and the environment-friendly requirement of no smoke and no sulfur 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 (5)
1. The utility model provides a cold fireworks medicament of safe no smoke and sulfur which characterized in that: the components and the occupied mass percentage are as follows:
the preparation method of the modified pentaerythritol tetranitrate comprises the following steps: adding pentaerythritol tetranitrate powder and a titanate coupling agent into acetone according to the mass ratio of 1 (0.05-0.08) to 10, and performing ultrasonic dispersion for 30-50 minutes to obtain a mixed solution C; transferring the mixed solution C into an ice-water bath for stirring; then adding the polyvinyl butyral adhesive into the mixed solution C (wherein the mass ratio of pentaerythritol tetranitrate powder to the polyvinyl butyral adhesive is 1 (0.02-0.03)), and stirring for 3-5 hours; transferring the reaction device into an oil bath pan at the temperature of 60-80 ℃, standing for 20-40 minutes, and recovering the volatilized acetone; filtering, repeatedly washing for 3-5 times by using deionized water, and drying for 2-3 hours in a blast oven at 80-100 ℃; taking out, crushing under light pressure to obtain modified pentaerythritol tetranitrate powder.
2. The safe smokeless and sulfur-free cold firework powder as claimed in claim 1, wherein: the average grain diameter of the nano-magnesium-aluminum powder in the components is 100nm, wherein the mass percent of the nano-aluminum powder is 60%, and the mass percent of the nano-magnesium powder is 40%.
3. The safe smokeless and sulfur-free cold firework powder as claimed in claim 1, wherein: the nitrogen content of the nitrated bamboo cellulose in the components is 12 to 12.5 percent.
4. The process for preparing the set of smokeless and sulfur-free cold firework formulation of claim 1, wherein: the method comprises the following specific steps:
weighing nano magnesium-aluminum powder, modified pentaerythritol tetranitrate, nitrated bamboo cellulose, dihydroxy glyoxime, dimethyl diphenyl urea, zinc stearate, polyetherimide, ethyl cellulose, methyl 3-aminocrotonate and graphene according to the mass ratio of the formula;
step two, dividing the nitrated bamboo cellulose powder weighed in the step one into A, B groups according to the mass ratio of (1-5) to (10), dissolving the nitrated bamboo cellulose powder of the group A in ethyl acetate according to the mass ratio of 1:10, and stirring for 2-3 hours under the ultrasonic dispersion condition; then, continuously adding the methyl 3-aminocrotonate powder and the zinc stearate powder weighed in the step one under the stirring state, and uniformly stirring to obtain a mixed solution of the nitrated bamboo cellulose;
step three, mixing the polyetherimide particles, the ethyl cellulose powder and the graphene powder weighed in the step one to obtain a mixture D; adding the mixture D into an N-methyl pyrrolidone solution according to the mass ratio of 1:10, and stirring for 1-2 hours in an ultrasonic dispersion state to obtain a mixed solution E; then transferring the mixed solution E into a spray gun to prepare antistatic agent spray liquid;
step four, adding the modified pentaerythritol tetranitrate powder, the dihydroxy glyoxime powder and the B group of the nitrated bamboo cellulose obtained in the step two into the nitrated bamboo cellulose mixed sol obtained in the step two under the stirring and ultrasonic dispersion states, and uniformly mixing; uniformly spraying the antistatic agent spray liquid prepared in the third step for 3-7 times, and uniformly mixing once every time; then adding the dimethyl diphenyl urea powder and the nano-magnesia-alumina powder weighed in the step one into the mixture to be uniformly mixed; then kneading, wherein a proper amount of ethyl acetate 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, airing the obtained uniform micelle in a cool and ventilated place to be half-dry, and transferring the obtained uniform micelle into a blast oven at the temperature of 80-90 ℃ for drying for 2-3 hours to obtain a crude product of the safe and shaped smokeless and sulfur-free cold firework medicament;
step five, crushing the crude product of the safe smokeless and sulfur-free cold firework explosive obtained in the step four by light pressure, sieving the crushed product through a 60-mesh copper sieve, removing screen residues with too small particles, then sieving the crushed product through a 30-mesh copper sieve, and taking the screen residues of the 30-mesh copper sieve to obtain the safe smokeless and sulfur-free cold firework explosive with uniform particles;
the method for judging the moderate hardness comprises the following steps: after the micelle is extruded to pass through a 20-mesh copper sieve, the micelle is in a continuous thin strip shape, is not adhered with each other, and has certain plasticity and tensile strength.
5. The method of claim 4, wherein: the preparation method of the modified pentaerythritol tetranitrate comprises the following steps: adding pentaerythritol tetranitrate powder and a titanate coupling agent into acetone according to the mass ratio of 1 (0.05-0.08) to 10, and performing ultrasonic dispersion for 30-50 minutes to obtain a mixed solution C; transferring the mixed solution C into an ice-water bath for stirring; then adding the polyvinyl butyral adhesive into the mixed solution C (wherein the mass ratio of pentaerythritol tetranitrate powder to the polyvinyl butyral adhesive is 1 (0.02-0.03)), and stirring for 3-5 hours; transferring the reaction device into an oil bath pan at the temperature of 60-80 ℃, standing for 20-40 minutes, and recovering the volatilized acetone; filtering, repeatedly washing for 3-5 times by using deionized water, and drying for 2-3 hours in a blast oven at 80-100 ℃; taking out, crushing under light pressure to obtain modified pentaerythritol tetranitrate powder.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5622698A (en) * | 1979-07-27 | 1981-03-03 | Radia Ind | Toy firework composition |
| CN103030483A (en) * | 2012-12-26 | 2013-04-10 | 南京理工大学 | Bright green cold firework composition and production method thereof |
| CN103121886A (en) * | 2012-12-26 | 2013-05-29 | 南京理工大学 | Multicolor cold-firework reagent and manufacturing method of cold fireworks |
-
2019
- 2019-12-10 CN CN201911255862.8A patent/CN111039734A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5622698A (en) * | 1979-07-27 | 1981-03-03 | Radia Ind | Toy firework composition |
| CN103030483A (en) * | 2012-12-26 | 2013-04-10 | 南京理工大学 | Bright green cold firework composition and production method thereof |
| CN103121886A (en) * | 2012-12-26 | 2013-05-29 | 南京理工大学 | Multicolor cold-firework reagent and manufacturing method of cold fireworks |
Non-Patent Citations (10)
| Title |
|---|
| 中国科学技术协会: "《2012-2013兵器科学技术学科发展报告（含能材料）》", 30 April 2014, 中国科学技术出版社 * |
| 全国安全生产教育培训教材编审委员会: "《烟火药制造作业》", 31 August 2013, 中国矿业大学出版社 * |
| 公安部治安管理局: "《爆炸物品安全监管执法手册》", 30 November 2014, 群众出版社 * |
| 国家安全生产应急救援指挥中心: "《烟花爆竹企业安全生产应急管理》", 30 June 2009, 煤炭工业出版社 * |
| 张明等: "石墨烯基材料对含能材料性能影响的研究进展", 《含能材料》 * |
| 潘功配: "《高等烟火学》", 31 October 2007, 哈尔滨工程大学出版社 * |
| 王正远: "《工程塑料实用手册》", 30 June 1994, 中国物资出版社 * |
| 王淑芬: "《化学故事》", 30 April 2013, 吉林教育出版社 * |
| 胡松启等: "《固体火箭发动机燃烧基础》", 31 August 2015, 西北工业大学出版社 * |
| 钟岩: "《理化检验鉴定》", 30 September 2005, 群众出版社 * |
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