CN115650811B - Micro-smoke lead agent for fireworks - Google Patents
Micro-smoke lead agent for fireworks Download PDFInfo
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- CN115650811B CN115650811B CN202211400499.6A CN202211400499A CN115650811B CN 115650811 B CN115650811 B CN 115650811B CN 202211400499 A CN202211400499 A CN 202211400499A CN 115650811 B CN115650811 B CN 115650811B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a firework micro-smoke lead agent, which belongs to the technical field of firework lead agents and comprises the following raw materials in parts by weight: 20-30 parts of coated ammonium perchlorate, 60-90 parts of single-base powder, 2-10 parts of carbon powder and 5-8 parts of metal powder; the coated ammonium perchlorate is prepared by the following steps: adding triethoxysilane modified polybutadiene into chloroform to obtain a coating solution, adding ammonium perchlorate into a mortar, adding the coating solution, rapidly stirring, and drying to obtain an intermediate product; mixing the intermediate product, the mercapto ferrocene compound, the azodiisobutyronitrile and the chloroform, heating to 60-65 ℃ under the protection of nitrogen under the magnetic stirring, reacting for 8-10h, and performing rotary steaming; the micro-smoke lead medicament prepared by the invention has the advantages of micro smoke, no sulfur smell, no sulfur dioxide generation, no harm to human body, low hygroscopicity, easy storage, capability of controlling the combustion speed and high safety performance by adjusting the proportion of the components.
Description
Technical Field
The invention belongs to the technical field of firework lead agents, and particularly relates to a firework micro-smoke lead agent.
Background
The existing micro-smoke firework lead can generate a large amount of smoke after being ignited, because the lead agent mainly takes potassium nitrate or potassium perchlorate, sulfur, charcoal and potassium hydrogen phthalate as main components, and generates a large amount of nitrogen oxides, sulfur dioxide, potassium sulfide, potassium sulfate, potassium carbonate and other hygroscopic substances after combustion, and the moisture is absorbed in the air to form acid mist, thereby seriously polluting the environment.
Therefore, it is necessary to provide a firework lead agent with lower smoke, and chinese patent CN101481286B announces a "firework smokeless lead agent composition", which is mainly composed of moistureproof ammonium perchlorate, single-double base powder, metal powder, perlite powder and carbon powder, wherein salt mist generated by burning the lead agent is less than 30% of the existing agent, and the burning rate of the lead is about 1cm/s, although moistureproof ammonium perchlorate is adopted as an oxidizing agent, the moistureproof effect is poor, hygroscopicity is still high during the preparation and storage of the lead, and the burning time and ignition effect of the lead are affected.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides a firework micro-smoke lead medicament.
The aim of the invention can be achieved by the following technical scheme:
a firework micro-smoke lead agent comprises the following raw materials in parts by weight: 20-30 parts of coated ammonium perchlorate, 60-90 parts of single-base powder, 2-10 parts of carbon powder and 5-8 parts of metal powder;
and (3) uniformly mixing the raw materials in parts by weight, and sieving the mixture through a 160-mesh sieve to obtain the firework micro-smoke lead medicament.
Further, the coated ammonium perchlorate is prepared by the steps of:
step A1, adding triethoxysilane modified polybutadiene into chloroform to obtain a coating solution, adding ammonium perchlorate into a mortar, adding the coating solution, rapidly and uniformly stirring, and then drying in a vacuum oven to obtain an intermediate product;
wherein the dosage ratio of the triethoxysilane modified polybutadiene to the chloroform is 0.03-0.05g:2.4mL, the dosage ratio of ammonium perchlorate to coating solution was 3g:2.4mL of triethoxysilane modified polybutadiene is a commercial product, both ends of a molecular chain are of a siloxane structure, and the molecule contains allyl and unsaturated double bonds;
step A2, adding an intermediate product, a sulfhydryl ferrocene compound, azodiisobutyronitrile and trichloromethane into a round-bottom flask, heating to 60-65 ℃ under the protection of nitrogen under the magnetic stirring, reacting for 8-10h, and removing a solvent by adopting a rotary evaporation evaporator after the reaction is finished to obtain coated ammonium perchlorate;
wherein the dosage ratio of the intermediate product, the sulfhydryl ferrocene compound and the chloroform is 3g:0.05-0.1g:30-40mL, and the azodiisobutyronitrile consumption is 1.5-2% of the sum of the intermediate product and the mercapto ferrocene compound.
In order to solve the problems that ammonium perchlorate has high hygroscopicity in firework lead agent and reduces the combustion effect of firework, the invention firstly utilizes triethoxysilane modified polybutadiene to form a hydrophobic organic coating layer on the surface of ammonium perchlorate, forms physical adsorption and shielding effects on the surface of ammonium perchlorate to reduce the hygroscopicity, and then utilizes unsaturated double bonds in triethoxysilane modified polybutadiene molecules and mercapto of mercapto ferrocene compound to carry out grafting reaction under the action of an initiator to obtain coated ammonium perchlorate with ferrocene on the surface.
The sulfhydryl ferrocene compound is prepared by the following steps:
adding L-cysteine into absolute ethyl alcohol, controlling the temperature to be 50-60 ℃, dropwise adding an absolute ethyl alcohol solution of ferrocenyl formaldehyde under stirring, carrying out heat preservation reaction for 4-5h, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying to obtain a sulfhydryl ferrocene compound; the dosage ratio of the L-cysteine, the absolute ethyl alcohol and the absolute ethyl alcohol solution of ferrocene formaldehyde is 1mmol:10mL: the dosage ratio of ferrocene to absolute ethyl alcohol in 10mL of absolute ethyl alcohol solution of ferrocene formaldehyde is 1mmol:10mL, -NH using L-cysteine 2 And ferrocenyl formaldehyde-CHO reaction to obtain mercapto ferrocene compound.
Further, the metal powder is one of titanium powder, iron powder, zirconium powder, aluminum powder, chromium powder and nickel powder.
The invention has the beneficial effects that:
1. the micro-smoke lead medicament provided by the invention has the advantages of micro smoke, no sulfur smell during combustion, no sulfur dioxide generation, environment protection, no harm to human body, low hygroscopicity, easiness in storage, capability of controlling the combustion speed and high safety performance by adjusting the proportion of the components.
2. The coated ammonium perchlorate disclosed by the invention has the advantages that the moisture absorption rate is low, the organic matter coating layer on the surface of the coated ammonium perchlorate is in a molten state under heating, and polymer reaction is generated between macromolecules to form long-chain polymers, so that the long-chain polymers float on the surface of a medicine, the blocking effect is obvious, the eruption of the combustion products of a lead medicine can be reduced, the smoke generation of fireworks is reduced, the ferrocene on the organic matter coating layer has a catalytic effect on one hand, and on the other hand, the hydrogen chloride gas generated by the ammonium perchlorate is quickly absorbed in the combustion process, so that the pungent smell of the lead medicine is greatly reduced, the setting-off effect is improved, and meanwhile, the environmental pollution and harm are reduced.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The triethoxysilane modified polybutadiene is a product of EVONIK company and has the trade name ofEPST-E100, chemical name triethoxysilane modified polybutadiene.
Example 1
The sulfhydryl ferrocene compound is prepared by the following steps:
1mmol L-cysteine is added into 10mL absolute ethyl alcohol, the temperature is controlled to be 55 ℃, 10mL absolute ethyl alcohol solution containing 1mmol ferrocene formaldehyde is added dropwise under stirring, the reaction is carried out for 4.5h under the condition of heat preservation, after the reaction is finished, filtration is carried out, the absolute ethyl alcohol is used for washing, and the sulfhydryl ferrocene compound is obtained after drying.
Example 2
The coated ammonium perchlorate is prepared by the following steps:
step A1, adding 0.03g of triethoxysilane modified polybutadiene into 2.4mL of chloroform to obtain a coating solution, adding 3g of ammonium perchlorate into a mortar, adding the coating solution, uniformly stirring within 5min, and then drying in a vacuum oven to obtain an intermediate product;
step A2, adding 3g of intermediate product, 0.05g of mercapto ferrocene compound of example 1, azobisisobutyronitrile and 30mL of chloroform into a round bottom flask, heating to 60 ℃ under the protection of nitrogen under the magnetic stirring, reacting for 8h, and removing the solvent by adopting a rotary evaporation evaporator to obtain coated ammonium perchlorate, wherein the amount of the azobisisobutyronitrile is 1.5% of the sum of the amounts of the intermediate product and the mercapto ferrocene compound.
Example 3
The coated ammonium perchlorate is prepared by the following steps:
step A1, adding 0.05g of triethoxysilane modified polybutadiene into 2.4mL of chloroform to obtain a coating solution, adding 3g of ammonium perchlorate into a mortar, adding the coating solution, uniformly stirring within 5min, and then drying in a vacuum oven to obtain an intermediate product;
step A2, adding 3g of intermediate product, 0.1g of mercapto ferrocene compound of example 1, azobisisobutyronitrile and 40mL of chloroform into a round bottom flask, heating to 65 ℃ under the protection of nitrogen under the magnetic stirring, reacting for 10h, and removing the solvent by adopting a rotary evaporation evaporator to obtain coated ammonium perchlorate, wherein the amount of the azobisisobutyronitrile is 2% of the sum of the amounts of the intermediate product and the mercapto ferrocene compound.
Comparative example 1
The coated ammonium perchlorate is prepared by the following steps:
0.03g of triethoxysilane modified polybutadiene is added into 2.4mL of chloroform to obtain a coating solution, 3g of ammonium perchlorate is added into a mortar, the coating solution is added, the mixture is rapidly and uniformly stirred, and then the mixture is placed into a vacuum oven for drying, so that coated ammonium perchlorate is obtained.
Comparative example 2
The coated ammonium perchlorate is prepared by the following steps:
0.03g of silane coupling agent KH-550 is added into 2.4mL of chloroform to obtain a coating solution, 3g of ammonium perchlorate is added into a mortar, the coating solution is added, the mixture is rapidly and uniformly stirred, and then the mixture is placed into a vacuum oven for drying, so as to obtain the coated ammonium perchlorate.
Example 4
A firework micro-smoke lead agent comprises the following raw materials in parts by weight: 20 parts of coated ammonium perchlorate, 60 parts of single base powder, 2 parts of carbon powder and 5 parts of titanium powder in example 2;
and uniformly mixing the raw materials in parts by weight, and sieving with a 160-mesh sieve to obtain the firework micro-smoke lead medicament.
Example 5
A firework micro-smoke lead agent comprises the following raw materials in parts by weight: 25 parts of coated ammonium perchlorate, 70 parts of single base powder, 5 parts of carbon powder and 7 parts of iron powder in example 3;
and uniformly mixing the raw materials in parts by weight, and sieving with a 160-mesh sieve to obtain the firework micro-smoke lead medicament.
Example 6
A firework micro-smoke lead agent comprises the following raw materials in parts by weight: 30 parts of coated ammonium perchlorate, 90 parts of single-base powder, 10 parts of carbon powder and 8 parts of zirconium powder in example 2;
and (3) mixing the raw materials in parts by weight, and sieving with a 160-mesh sieve to obtain the firework micro-smoke lead medicament.
Comparative example 3
The procedure of example 4 was followed except that the coated ammonium perchlorate in example 4 was replaced with the material of comparative example 1 and the remaining materials and preparation were the same.
Comparative example 4
The procedure of example 4 was followed except that the coated ammonium perchlorate in example 4 was replaced with the material of comparative example 2.
The firework lead agents prepared in examples 4-6 and comparative examples 3-4 were tested for hygroscopicity by a method of QB/T1914.5, each group of lead agents to be tested was wrapped with lead paper and twisted into a wire shape according to a conventional method of manufacturing leads, the amount of the lead agents was 3 g/1 m of the lead paper, and then a firing line was obtained by sizing and drying, and the burning rate was tested; salt mist amount: 1000mg of each group of the medicaments to be detected is taken and placed in a volume of 0.25m 3 The mass of PM2.5 or PM10 in the same volume environment is subtracted from the mass of solid particles collected by an ambient air particulate matter sampler BTPM-HSS, and the mass of PM2.5 or PM10 generated per 1000mg sample is calculated by the following formula, wherein m3=m2-m0-m null)/m1×1000, wherein: m is blank experimental quality, g; m0 is the mass of the filter membrane before filtration, g; m1 is the mass of the sample to be measured, g; m2 is the mass of the filter membrane after filtration, g; m3 is the mass of PM2.5 or PM10 generated by burning 1000mg of the tested sample, and mg; the test results are shown in table 1:
TABLE 1
| Project | Example 4 | Example 5 | Example 6 | Comparative example 3 | Comparative example 4 |
| Moisture absorption Rate (%) | 0.22 | 0.18 | 0.25 | 0.42 | 0.75 |
| Combustion speed (cm/s) | 5.6 | 4.5 | 6.2 | 6.9 | 6.5 |
| PM2.5(mg) | 171.5 | 165.6 | 183.3 | 194.4 | 215.6 |
| PM10(mg) | 179.1 | 174.7 | 186.5 | 198.7 | 217.9 |
As can be seen from Table 1, the firework lead powder prepared in examples 4 to 6 was low in moisture absorption rate, low in salt spray amount and good in combustion efficiency as compared with comparative examples 3 to 4.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (2)
1. The firework micro-smoke lead agent is characterized by comprising the following raw materials in parts by weight: 20-30 parts of coated ammonium perchlorate, 60-90 parts of single-base powder, 2-10 parts of carbon powder and 5-8 parts of metal powder;
wherein the coated ammonium perchlorate is prepared by the following steps:
step A1, adding triethoxysilane modified polybutadiene into chloroform to obtain a coating solution, adding ammonium perchlorate into a mortar, adding the coating solution, stirring and drying to obtain an intermediate product;
step A2, mixing an intermediate product, a sulfhydryl ferrocene compound, azodiisobutyronitrile and chloroform, heating to 60-65 ℃ under the protection of nitrogen under the magnetic stirring, reacting for 8-10h, and performing rotary evaporation to obtain coated ammonium perchlorate;
the usage ratio of the triethoxysilane modified polybutadiene to the chloroform is 0.03-0.05g:2.4mL, the dosage ratio of ammonium perchlorate to coating solution was 3g:2.4mL;
the dosage ratio of the intermediate product, the mercaptoferrocene compound and the chloroform is 3g:0.05-0.1g:30-40mL, wherein the dosage of the azodiisobutyronitrile is 1.5-2% of the sum of the intermediate product and the mercapto ferrocene compound;
the sulfhydryl ferrocene compound is prepared by the following steps:
adding L-cysteine into absolute ethyl alcohol, controlling the temperature to be 50-60 ℃, dropwise adding an absolute ethyl alcohol solution of ferrocenyl formaldehyde under stirring, and reacting for 4-5h under heat preservation to obtain a sulfhydryl ferrocene compound;
the dosage ratio of the L-cysteine, the absolute ethyl alcohol and the absolute ethyl alcohol solution of ferrocene formaldehyde is 1mmol:10mL: the dosage ratio of ferrocene to absolute ethyl alcohol in 10mL of absolute ethyl alcohol solution of ferrocene formaldehyde is 1mmol:10mL.
2. The firework micro-smoke lead agent according to claim 1, wherein the metal powder is one of titanium powder, iron powder, zirconium powder, aluminum powder, chromium powder and nickel powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211400499.6A CN115650811B (en) | 2022-11-09 | 2022-11-09 | Micro-smoke lead agent for fireworks |
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| CN202211400499.6A CN115650811B (en) | 2022-11-09 | 2022-11-09 | Micro-smoke lead agent for fireworks |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5458706A (en) * | 1993-12-29 | 1995-10-17 | Societe Nationale Des Poudres Et Explosifs | Solid pyrotechnic compositions with a thermoplastic binder and a polybutadiene silylferrocene plasticizer |
| CN103214322A (en) * | 2013-05-15 | 2013-07-24 | 浏阳市合力高科发展有限公司 | Sulfur-smoke-free powder composition and preparation method thereof |
| CN110845285A (en) * | 2018-08-20 | 2020-02-28 | 南京理工大学 | Method for reducing hygroscopicity of ammonium perchlorate |
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- 2022-11-09 CN CN202211400499.6A patent/CN115650811B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5458706A (en) * | 1993-12-29 | 1995-10-17 | Societe Nationale Des Poudres Et Explosifs | Solid pyrotechnic compositions with a thermoplastic binder and a polybutadiene silylferrocene plasticizer |
| CN103214322A (en) * | 2013-05-15 | 2013-07-24 | 浏阳市合力高科发展有限公司 | Sulfur-smoke-free powder composition and preparation method thereof |
| CN110845285A (en) * | 2018-08-20 | 2020-02-28 | 南京理工大学 | Method for reducing hygroscopicity of ammonium perchlorate |
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