CN111018635B - Explosion type firecracker agent and preparation method thereof - Google Patents
Explosion type firecracker agent and preparation method thereof Download PDFInfo
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- CN111018635B CN111018635B CN201911321705.2A CN201911321705A CN111018635B CN 111018635 B CN111018635 B CN 111018635B CN 201911321705 A CN201911321705 A CN 201911321705A CN 111018635 B CN111018635 B CN 111018635B
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B25/00—Compositions containing a nitrated organic compound
- C06B25/18—Compositions containing a nitrated organic compound the compound being nitrocellulose present as 10% or more by weight of the total composition
- C06B25/20—Compositions containing a nitrated organic compound the compound being nitrocellulose present as 10% or more by weight of the total composition with a non-explosive or a non-explosive or a non-thermic component
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
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Abstract
The invention relates to a firecracker agent for breaking explosion and a preparation method thereof, belonging to the technical cross field of material processing preparation and pyrotechnic compositions. The invention provides a plurality of groups of formulas, namely, a formula I, fine sand, nitrifying bamboo cellulose, a stabilizer, potassium benzoate, melamine and a substance A; formula II, expanded perlite, nitrocellulose, stabilizer, stearic acid, melamine and substance A; the invention does not select the raw materials with poor stability such as silver nitrate, has the characteristics of no smoke, no sulfur, environment protection and environment protection in the setting-off process, is safe to people, has excellent working state, has no problems of advanced or delayed explosion and the like, is smokeless and nontoxic in the setting-off process, and the formula of the obtained drop explosion type firecracker powder is safer and more environment-friendly than the traditional formula.
Description
Technical Field
The invention relates to a firecracker agent for breaking explosion and a preparation method thereof, belonging to the technical cross field of material processing preparation and pyrotechnic compositions.
Background
The firecracker is also called as a firecracker. The product is positioned on the fireworks and crackers of toys according to GB10631-2013 safety and quality of fireworks and crackers, and is suitable for outdoor open space setting off and close range setting off products. During entertainment and playing, the explosion firecracker does not need to be ignited, and can make crisp sound when being thrown or stepped on by hand, and the firecracker is highly interesting and is popular with various groups such as children at home and abroad.
Along with the strengthening of the national environment-friendly industry management and the execution of the firework and firecracker forbidden discharge command, the whole firework and firecracker industry is affected and gradually goes to a downhill. At present, the preparation method of the throwing gun powder still mainly adopts the traditional preparation method, and the method still has the problems of uneven medicine mixing, uneven granulation size, dangerous preparation and the like, and is difficult to achieve the purposes of safe production, safe transportation, safe use and safe storage. In order to solve the existing problems, patent CN201710832505.8, li Shucun et al proposes a production method of a children's throwing gun, which adopts silver nitrate and the like as raw materials and achieves the aim of product safety through the process preparation flow of dissolution, filtration, deacidification and the like. Wang Junming in its patent CN92102524.6, a new type of pressure firecracker and a method for producing the same are proposed, in which a membrane is used to seal the gas, and when the membrane is pressed, the explosion of the membrane produces a detonating sound. Although the method achieves the aim of safety and environmental protection, most films have air permeability, so that the falling explosion type film has short shelf life, is extremely easy to lose efficacy in the playing process, has reduced entertainment performance and is difficult to market. Zhang Hongliang in its 200420117202.6 patent, a new type of "thunderbolt tadpole" is proposed, its medicine is sand 99%, silver salt 0.2%, nitric acid 0.3% and alcohol 0.5%. However, the intermediate product of this process is silver nitrate, which is extremely toxic to long-term contact. Among them, silver nitrate is an environmental pollutant, and has poor stability, which is extremely dangerous in entertainment. Therefore, development of a drop explosion type firecracker agent and a preparation method thereof are urgently needed.
Disclosure of Invention
The invention aims to solve the problems of production, use safety and environmental pollution of the existing drop-explosion type firecracker and provides a drop-explosion type firecracker medicament and a preparation method thereof. The invention provides a new formula of the firecracker agent, and the preparation method is simple to operate, environment-friendly, safe and feasible.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a firecracker agent for breaking and explosion comprises the following components:
formula one, fine sand, nitrified bamboo cellulose, stabilizer, potassium benzoate, melamine and substance A, wherein the mass ratio is (25-40): (10-16): (7-10): (10-16): (12-20): (8-15);
formula II, expanded perlite, nitrocellulose, stabilizer, stearic acid, melamine and substance A, wherein the mass ratio is (20-28): (12-15): (15-18): (12-18): (15-20): (10-16);
the substance A is one of starch, phenolic resin, rosin, lactose or white latex;
the stabilizer is one of sodium carbonate and sodium bicarbonate;
the preparation method of the nitrified bamboo cellulose comprises the following steps:
step (1): placing the bamboo fiber or bamboo fiber product in a drying oven, wherein the temperature of the oven is controlled to be lower than 100 ℃ until the moisture content of the bamboo fiber or bamboo fiber product is less than 7%;
step (2): preparing a mixed acid solution from concentrated sulfuric acid with the concentration of 60-95% and concentrated nitric acid with the concentration of 70-92%; the mass ratio of the concentrated sulfuric acid to the concentrated nitric acid is as follows: (2.2-3.5): 1.0-2.0);
step (3): adding the bamboo fiber or bamboo fiber product dried in the step (1) into the mixed acid solution in the step (2); controlling the reaction temperature to be lower than 60 ℃, controlling the feeding speed to be 30-180 g/min, controlling the stirring speed to be 60-1200 r/min, taking out after reacting for 5-45 min, and cleaning with cold water to obtain the nitrified bamboo cellulose; the mass ratio of the bamboo fiber or bamboo fiber product to the concentrated nitric acid in the mixed acid solution is (2-20) (6-80);
step (4): putting the nitrified bamboo cellulose obtained in the step (3) into a container, and pouring sodium carbonate solution with the concentration not higher than 18mol/L or sodium bicarbonate solution with the concentration not higher than 25mol/L into the container until the solution is neutral;
step (5): taking out the nitrified bamboo cellulose in the step (4), placing the nitrified bamboo cellulose in a wall breaking machine filled with distilled water or ethanol, preparing the nitrified bamboo cellulose into powder, filtering, drying the powder, and storing the powder in a polyethylene tank or jar; adding distilled water or ethanol into a polyethylene tank or jar; the distilled water content is not less than 11%; the ethanol content is not less than 25%.
The bamboo fiber product is bamboo fiber paper or bamboo fiber yarn.
A preparation method of a shatter-explosion type firecracker agent comprises the following specific preparation steps: (1) selecting sand; (2) glue preparation; (3) dispensing and granulating; (4) mixing materials.
Step (1): selecting fine sand with the grain diameter of 15-100 meshes;
step (2): and (3) weighing the substance A, and preparing the A glue with the mass percentage concentration of 2% -42%.
Step (3): other raw materials except fine sand are weighed according to a formula. Firstly, placing the nitrocellulose in a wall breaking machine containing 2/3 distilled water or ethanol, beating the nitrocellulose into cotton floc, filtering to obtain the nitrocellulose, and regulating the humidity of the nitrocellulose to be not less than 10% by using distilled water or ethanol. Uniformly mixing the nitrified bamboo cellulose with other raw materials to obtain a mixture, slowly dripping the adhesive A obtained in the step (2), granulating, and sieving with a 15-150-mesh sieve after finishing.
The glue A in the step (3) has viscosity, and in actual use, the glue head dropper and the container wall have loss. For the accurate formula, the quantity of the adhesive A is more in actual preparation, the adhesive A is added by adopting a differential method, the dripping termination is determined according to the adhesive A allowance, and the adhesive A allowance is determined by the following formula:
M dosage of A glue =M Total amount of A glue -M Adhesive margin A 。
Wherein m is A In order to break the dosage of the substance A in the gun formula, a percent is the percentage concentration of the mass of the colloid A obtained in the step (2), M Total amount of A glue The weight obtained from step (2) is known.
Step (4): uniformly mixing the mixture particles obtained in the step (3) with the fine sand obtained in the step (1), placing the mixture particles in a shady and ventilated place, and airing until the humidity is lower than 5%, thereby obtaining the drop-explosion type firecracker agent;
a preparation method of a shatter-explosion type firecracker agent comprises the following steps: (1) glue preparation; (2) dispensing and granulating; (3) drying in the shade.
Step (1): and (3) weighing the substance A, and preparing the A glue with the mass percentage concentration of 2% -42%.
Step (2): the step (2) is consistent with the step (3) in the preparation step of the formula.
Step (3): and (3) uniformly mixing the mixture particles obtained in the step (2) with expanded perlite, placing the mixture particles in a shady and ventilated place, and airing until the humidity is lower than 5%, thereby obtaining the drop-explosion type firecracker medicament.
Advantageous effects
1. The drop explosion type firecracker medicament and the preparation method thereof have low equipment requirement and simple production process, and are beneficial to industrial production. The preparation prepared by the method has good stability and stability, and is easy to store and transport.
2. The explosion type firecracker agent and the preparation method thereof are safe to people and environment-friendly in the processing process.
3. The drop explosion type firecracker agent and the preparation method thereof are different from the traditional formula, raw materials with poor stability such as silver nitrate and the like are not selected, the drop explosion type firecracker agent has the characteristics of no smoke, no sulfur, environmental protection and environment friendliness in the setting-off process, is safe to people, has an excellent working state, does not have the problems of early or delayed explosion and the like, is free of smoke and non-toxicity in the setting-off process, and the obtained drop explosion type firecracker powder formula is safer and more environment-friendly than the traditional formula.
Detailed Description
The technical solution of the present invention is further described below with reference to the embodiments, and the described embodiments are only some embodiments of the present invention, but not all embodiments. Based on the embodiments in the invention, all are within the protection scope of the invention.
Example 1
A firecracker agent for breaking and explosion comprises the following components:
fine sand, nitrifying bamboo cellulose, sodium bicarbonate, potassium benzoate, melamine and starch, wherein the mass ratio is 25:15:10:15:20:15.
the preparation method of the nitrified bamboo cellulose comprises the following steps:
step (1): placing the bamboo fibers in a drying oven, and controlling the temperature of the oven to 90 ℃ until the moisture content of the bamboo fibers is 6%;
step (2): preparing a mixed acid solution from concentrated sulfuric acid with the concentration of 75% and concentrated nitric acid with the concentration of 85%; the mass ratio of the concentrated sulfuric acid to the concentrated nitric acid is as follows: 3:1.2;
step (3): adding the dried bamboo fibers in the step (1) into the mixed acid solution in the step (2); controlling the reaction temperature to 50 ℃, controlling the feeding speed to be 80g/min, stirring the mixture at the speed of 100r/min, taking out the mixture after reacting for 20min, and cleaning the mixture with cold water to obtain the nitrified bamboo cellulose; the mass ratio of the bamboo fiber to the concentrated nitric acid in the mixed acid solution is 3:9.8;
step (4): putting the nitrified bamboo cellulose obtained in the step (3) into a container, and pouring sodium bicarbonate solution with the concentration of 16mol/L into the container until the solution is neutral;
step (5): taking out the nitrocellulose in the step (4), placing the nitrocellulose in a wall breaking machine filled with distilled water, preparing the nitrocellulose into powder, filtering, drying and storing in a jar; adding distilled water into the jar to ensure that the distilled water content in the nitrocellulose is 12%;
a preparation method of a firecracker agent comprises the following specific preparation steps: (1) selecting sand; (2) glue preparation; (3) dispensing and granulating; (4) mixing materials.
Step (1): weighing 250g of clean and dried 60-mesh fine sand for later use;
step (2): 160g of starch is weighed and slowly added into distilled water to be stirred, and starch gum with the mass percent concentration of 20 percent is prepared and obtained, M Total amount of starch gum 800g for use.
Step (3): 15g of nitrified bamboo cellulose, 100g of sodium bicarbonate, 150g of potassium benzoate and 200g of melamine are weighed according to a formula. Placing the nitrocellulose in a wall breaking machine containing 2/3 distilled water, beating the nitrocellulose into cotton floc, filtering to obtain the nitrocellulose, and regulating the humidity of the nitrocellulose to 15% by using distilled water. Uniformly mixing the nitrified bamboo cellulose with other raw materials to obtain a mixture, slowly dripping the adhesive A obtained in the step (2), granulating, and sieving with a 80-mesh sieve after finishing.
Adding the starch glue obtained in the step (2) according to a differential method, and granulating. The starch glue in the step (2) is always placed on an electronic balance, and the adding amount of the starch is 150g according to the formula, and the amount of the starch glue to be added is as follows:when the electronic balance shows +> And (3) finishing the addition of the starch glue. After the granulating process is finished, selecting a 30-mesh sieve and a 60-mesh sieve to obtain the intermediate grain size.
Step (4): uniformly mixing the mixture particles obtained in the step (3) with the sand obtained in the step (1), placing the mixture particles in a cool and ventilated place, and airing the mixture particles until the humidity is 3%, thereby obtaining the drop-explosion type firecracker medicament;
weighing 5g of firecracker breaking sample from the firecracker breaking agent crude product, charging, testing, falling height higher than 150cm, and the result shows that: the flame retardant type smoke-free flame retardant plastic has the advantages of no smoke, no pungent smell and no dangerousness during the firing, simple and quick processing technology, no dangerousness during the processing, excellent raw material and product stability, good working state and no phenomenon of advanced or delayed explosion.
Example 2
A firecracker agent for breaking and explosion comprises the following components:
fine sand, nitrifying bamboo cellulose, sodium bicarbonate, potassium benzoate, melamine and starch, wherein the mass ratio is 40:10:10:13:16:11.
the preparation method of the nitrified bamboo cellulose comprises the following steps:
step (1): placing the bamboo fibers in a drying oven, and controlling the temperature of the oven to 80 ℃ until the moisture content of the bamboo fibers is 5%;
step (2): preparing a mixed acid solution from concentrated sulfuric acid with the concentration of 85% and concentrated nitric acid with the concentration of 70%; the mass ratio of the concentrated sulfuric acid to the concentrated nitric acid is as follows: 2.8:1;
step (3): adding the dried bamboo fibers in the step (1) into the mixed acid solution in the step (2); controlling the reaction temperature to 50 ℃, controlling the feeding speed to be 40g/min, stirring the mixture at a speed of 40r/min, taking out the mixture after the mixture reacts for 25min, and cleaning the mixture with cold water to obtain the nitrified bamboo cellulose; the mass ratio of the bamboo fiber to the concentrated nitric acid in the mixed acid solution is 3:8;
step (4): putting the nitrocellulose obtained in the step (3) into a container, and pouring sodium bicarbonate solution with the concentration of 20mol/L into the container until the solution is neutral;
step (5): taking out the nitrocellulose in the step (4), placing the nitrocellulose in a wall breaking machine filled with distilled water, preparing the nitrocellulose into powder, filtering, drying and storing in a jar; adding distilled water into the jar to ensure that the distilled water content in the nitrocellulose is 15%;
a preparation method of a firecracker agent comprises the following specific preparation steps: (1) selecting sand; (2) glue preparation; (3) dispensing and granulating; (4) mixing materials.
Step (1): weighing 400g of clean and dried 100-mesh fine sand for later use;
step (2): 120g of starch is weighed and slowly added into distilled water to be stirred, and starch gum with the mass percent concentration of 20 percent is prepared and obtained, M Total amount of starch gum 600g was used.
Step (3): 100g of nitrified bamboo cellulose, 100g of sodium bicarbonate, 130g of sodium benzoate and 160g of melamine are weighed according to a formula. Placing the nitrocellulose in a wall breaking machine containing 2/3 distilled water, beating the nitrocellulose into cotton floc, filtering to obtain the nitrocellulose, and regulating the humidity of the nitrocellulose to 15% by using distilled water. Uniformly mixing the nitrified bamboo cellulose with other raw materials to obtain a mixture, slowly dripping the adhesive A obtained in the step (2), granulating, and sieving with a 100-mesh sieve after finishing.
Adding the starch glue obtained in the step (2) according to a differential method, and granulating. The starch glue in the step (2) is always placed on an electronic balance, and the adding amount of the starch is 110g according to the formula, and the amount of the starch glue to be added is as follows:when the electronic balance shows +> And (3) finishing the addition of the starch glue. After the granulation process is finished, selecting a 100-mesh sieve particle size.
Step (4): uniformly mixing the mixture particles obtained in the step (3) with the sand obtained in the step (1), placing the mixture particles in a cool and ventilated place, and airing the mixture particles until the humidity is 4%, thereby obtaining the drop-explosion type firecracker medicament;
weighing 5g of firecracker breaking sample from the firecracker breaking agent crude product, charging, testing, falling to a height higher than 160cm, and displaying the result: the flame retardant type smoke-free flame retardant plastic has the advantages of no smoke, no pungent smell and no dangerousness during the firing, simple and quick processing technology, no dangerousness during the processing, excellent raw material and product stability, good working state and no phenomenon of advanced or delayed explosion.
Example 3
A firecracker agent for breaking and explosion comprises the following components:
fine sand, nitrifying bamboo cellulose, sodium bicarbonate, potassium benzoate, melamine and starch, wherein the mass ratio of the fine sand to the nitrifying bamboo cellulose to the sodium bicarbonate to the potassium benzoate to the melamine to the starch is 33:13:9:15:18:12.
the preparation method of the nitrified bamboo cellulose comprises the following steps:
step (1): placing the bamboo fibers in a drying oven, and controlling the temperature of the oven to be 90 ℃ until the moisture content of the bamboo fibers is 5%;
step (2): preparing a mixed acid solution from concentrated sulfuric acid with the concentration of 90% and concentrated nitric acid with the concentration of 70%; the mass ratio of the concentrated sulfuric acid to the concentrated nitric acid is as follows: 2.2:1;
step (3): adding the dried bamboo fibers in the step (1) into the mixed acid solution in the step (2); controlling the reaction temperature to 55 ℃, controlling the feeding speed to be 60g/min, stirring the mixture at the speed of 100r/min, taking out the mixture after reacting for 18min, and cleaning the mixture with cold water to obtain the nitrified bamboo cellulose; the mass ratio of the bamboo fiber to the concentrated nitric acid in the mixed acid solution is 3:8;
step (4): putting the nitrocellulose obtained in the step (3) into a container, and pouring sodium bicarbonate solution with the concentration of 20mol/L into the container until the solution is neutral;
step (5): taking out the nitrocellulose in the step (4), placing the nitrocellulose in a wall breaking machine filled with ethanol, preparing the nitrocellulose into powder, filtering, drying, and storing in a jar; adding ethanol into the jar to ensure that the ethanol content in the nitrified bamboo cellulose is 18%;
a preparation method of a firecracker agent comprises the following specific preparation steps: (1) selecting sand; (2) glue preparation; (3) dispensing and granulating; (4) mixing materials.
Step (1): weighing 330g of clean and dried 100-mesh fine sand for later use;
step (2): weighing 150g of starch, slowly adding into distilled water, and stirring to obtain starch gum with mass percentage concentration of 20%, M Total amount of starch gum 750g for use.
Step (3): 130g of nitrified bamboo cellulose, 90g of sodium bicarbonate, 150g of sodium benzoate and 180g of melamine are weighed according to a formula. Placing the nitrocellulose in a wall breaking machine containing 2/3 distilled water, beating the nitrocellulose into cotton floc, filtering to obtain the nitrocellulose, and regulating the humidity of the nitrocellulose to 15% by using distilled water. Uniformly mixing the nitrified bamboo cellulose with other raw materials to obtain a mixture, slowly dripping the adhesive A obtained in the step (2), granulating, and sieving with a 100-mesh sieve after finishing.
Adding the starch glue obtained in the step (2) according to a differential method, and granulating. The starch glue in the step (2) is always placed on an electronic balance, and the adding amount of the starch is 120g according to the formula, and the amount of the starch glue to be added is as follows:when the electronic balance shows +> And (3) finishing the addition of the starch glue. After the granulation process is finished, selecting a 100-mesh sieve particle size.
Step (4): uniformly mixing the mixture particles obtained in the step (3) with the sand obtained in the step (1), placing the mixture particles in a cool and ventilated place, and airing the mixture particles until the humidity is 4%, thereby obtaining the drop-explosion type firecracker medicament;
weighing 5g of firecracker breaking sample from the firecracker breaking agent crude product, charging, testing, falling height higher than 150cm, and the result shows that: the flame retardant type smoke-free flame retardant plastic has the advantages of no smoke, no pungent smell and no dangerousness during the firing, simple and quick processing technology, no dangerousness during the processing, excellent raw material and product stability, good working state and no phenomenon of advanced or delayed explosion.
Example 4
A firecracker agent for breaking and explosion comprises the following components:
the weight ratio of the expanded perlite to the nitrogenated bamboo cellulose to the stabilizer to the stearic acid to the melamine to the starch is 20:15:15:16:18:16.
the preparation method of the nitrified bamboo cellulose comprises the following steps:
step (1): placing the bamboo fibers in a drying oven, and controlling the temperature of the oven to be 90 ℃ until the moisture content of the bamboo fibers is 5%;
step (2): preparing a mixed acid solution from concentrated sulfuric acid with the concentration of 90% and concentrated nitric acid with the concentration of 70%; the mass ratio of the concentrated sulfuric acid to the concentrated nitric acid is as follows: 2.2:1;
step (3): adding the dried bamboo fibers in the step (1) into the mixed acid solution in the step (2); controlling the reaction temperature to 55 ℃, controlling the feeding speed to be 60g/min, stirring the mixture at the speed of 100r/min, taking out the mixture after reacting for 18min, and cleaning the mixture with cold water to obtain the nitrified bamboo cellulose; the mass ratio of the bamboo fiber to the concentrated nitric acid in the mixed acid solution is 3:8;
step (4): putting the nitrocellulose obtained in the step (3) into a container, and pouring sodium bicarbonate solution with the concentration of 20mol/L into the container until the solution is neutral;
step (5): taking out the nitrocellulose in the step (4), placing the nitrocellulose in a wall breaking machine filled with ethanol, preparing the nitrocellulose into powder, filtering, drying, and storing in a jar; adding ethanol into the jar to ensure that the ethanol content in the nitrified bamboo cellulose is 18%;
a preparation method of a firecracker agent comprises the following specific preparation steps: (1) glue preparation; (2) dispensing and granulating; (3) drying in the shade.
Step (1): weighing 170g of starch, slowly adding into distilled water, and stirring to obtain starch gum with mass percent concentration of 20%, M Total amount of starch gum 850g for use.
Step (2): 150g of nitrified bamboo cellulose, 150g of sodium bicarbonate, 160g of stearic acid and 180g of melamine are weighed according to a formula. Placing the nitrocellulose in a wall breaking machine containing 2/3 distilled water, beating the nitrocellulose into cotton floc, filtering to obtain the nitrocellulose, and regulating the humidity of the nitrocellulose to 15% by using distilled water. Uniformly mixing the nitrified bamboo cellulose with other raw materials to obtain a mixture, slowly dripping the adhesive A obtained in the step (2), granulating, and sieving with a 100-mesh sieve after finishing.
Adding the starch glue obtained in the step (2) according to a differential method, and granulating. The starch glue in the step (2) is always placed on an electronic balance, and the adding amount of the starch is 160g according to the formula, and the amount of the starch glue to be added is as follows:when the electronic balance shows +> And (3) finishing the addition of the starch glue. After the granulation process is finished, selecting a 100-mesh sieve particle size. />
Step (3): uniformly mixing the mixture particles obtained in the step (2) with 200g of expanded perlite, placing the mixture particles in a shady and ventilated place, and airing the mixture particles until the humidity is 5%, thereby obtaining the drop-explosion type firecracker medicament;
weighing 5g of firecracker breaking sample from the firecracker breaking agent crude product, charging, testing, falling height higher than 150cm, and the result shows that: the flame retardant type smoke-free flame retardant plastic has the advantages of no smoke, no pungent smell and no dangerousness during the firing, simple and quick processing technology, no dangerousness during the processing, excellent raw material and product stability, good working state and no phenomenon of advanced or delayed explosion.
Example 5
A firecracker agent for breaking and explosion comprises the following components:
the weight ratio of the expanded perlite, the nitrogenated bamboo cellulose, the stabilizer, the stearic acid, the melamine and the starch is 28:12:15:15:16:14.
the preparation method of the nitrified bamboo cellulose comprises the following steps:
step (1): placing the bamboo fibers in a drying oven, and controlling the temperature of the oven to be 80 ℃ until the moisture content of the bamboo fibers is 2%;
step (2): preparing a mixed acid solution from concentrated sulfuric acid with the concentration of 85% and concentrated nitric acid with the concentration of 75%; the mass ratio of the concentrated sulfuric acid to the concentrated nitric acid is as follows: 3.5:2;
step (3): adding the dried bamboo fibers in the step (1) into the mixed acid solution in the step (2); controlling the reaction temperature to 55 ℃, controlling the feeding speed to be 50g/min, stirring the mixture at 80r/min, taking out the mixture after reacting for 8min, and cleaning the mixture with cold water to obtain the nitrified bamboo cellulose; the mass ratio of the bamboo fiber to the concentrated nitric acid in the mixed acid solution is 3:7;
step (4): putting the nitrocellulose obtained in the step (3) into a container, and pouring sodium bicarbonate solution with the concentration of 25mol/L into the container until the solution is neutral;
step (5): taking out the nitrocellulose in the step (4), placing the nitrocellulose in a wall breaking machine filled with distilled water, preparing the nitrocellulose into powder, filtering, drying and storing in a jar; distilled water is added into the jar to ensure that the water content of the nitrocellulose is 12 percent;
a preparation method of a firecracker agent comprises the following specific preparation steps: (1) glue preparation; (2) dispensing and granulating; (3) drying in the shade.
Step (1): weighing 150g of starch, slowly adding into distilled water, and stirring to obtain starch gum with mass percentage concentration of 20%, M Total amount of starch gum 750g for use.
Step (2): 120g of nitrified bamboo cellulose, 150g of sodium bicarbonate, 150g of stearic acid and 160g of melamine are weighed according to a formula. Placing the nitrocellulose in a wall breaking machine containing 2/3 distilled water, beating the nitrocellulose into cotton floc, filtering to obtain the nitrocellulose, and regulating the humidity of the nitrocellulose to 12% by using distilled water. Uniformly mixing the nitrified bamboo cellulose with other raw materials to obtain a mixture, slowly dripping the adhesive A obtained in the step (2), granulating, and sieving with a 100-mesh sieve after finishing.
Adding the starch glue obtained in the step (2) according to a differential method, and granulating. The starch glue in the step (2) is always placed on an electronic balance, and the adding amount of the starch is 140g according to the formula, and the amount of the starch glue to be added is as follows:when the electronic balance shows +> And (3) finishing the addition of the starch glue. After the granulation process is finished, selecting a 100-mesh sieve particle size.
Step (3): uniformly mixing the mixture particles obtained in the step (2) with 280g of expanded perlite, placing the mixture particles in a shady and ventilated place, and airing the mixture particles until the humidity is 5%, thereby obtaining the drop-explosion type firecracker medicament;
weighing 5g of firecracker breaking sample from the firecracker breaking agent crude product, charging, testing, falling to a height higher than 140cm, and displaying the result: the flame retardant type smoke-free flame retardant plastic has the advantages of no smoke, no pungent smell and no dangerousness during the firing, simple and quick processing technology, no dangerousness during the processing, excellent raw material and product stability, good working state and no phenomenon of advanced or delayed explosion.
Example 6
A firecracker agent for breaking and explosion comprises the following components:
the weight ratio of the expanded perlite to the nitrogenated bamboo cellulose to the stabilizer to the stearic acid to the melamine to the starch is 24:13.5:16:16:17.5:13.
the preparation method of the nitrified bamboo cellulose comprises the following steps:
step (1): placing the bamboo fibers in a drying oven, and controlling the temperature of the oven to be 85 ℃ until the moisture content of the bamboo fibers is 4%;
step (2): preparing a mixed acid solution from concentrated sulfuric acid with the concentration of 80% and concentrated nitric acid with the concentration of 80%; the mass ratio of the concentrated sulfuric acid to the concentrated nitric acid is as follows: 3:2;
step (3): adding the dried bamboo fibers in the step (1) into the mixed acid solution in the step (2); controlling the reaction temperature to 45 ℃, controlling the feeding speed to be 100g/min, stirring the mixture at 120r/min, taking out the mixture after reacting for 15min, and cleaning the mixture with cold water to obtain the nitrified bamboo cellulose; the mass ratio of the bamboo fiber to the concentrated nitric acid in the mixed acid solution is 5:12;
step (4): putting the nitrocellulose obtained in the step (3) into a container, and pouring sodium bicarbonate solution with the concentration of 25mol/L into the container until the solution is neutral;
step (5): taking out the nitrocellulose in the step (4), placing the nitrocellulose in a wall breaking machine filled with distilled water, preparing the nitrocellulose into powder, filtering, drying and storing in a jar; distilled water is added into the jar to ensure that the water content of the nitrocellulose is 15 percent;
a preparation method of a firecracker agent comprises the following specific preparation steps: (1) glue preparation; (2) dispensing and granulating; (3) drying in the shade.
Step (1): weighing 150g of starch, slowly adding into distilled water, and stirring to obtain starch gum with mass percentage concentration of 25%, M Total amount of starch gum 600g was used.
Step (2): 135g of nitrified bamboo cellulose, 160g of sodium carbonate, 160g of stearic acid and 175g of melamine are weighed according to a formula. Placing the nitrocellulose in a wall breaking machine containing 2/3 distilled water, beating the nitrocellulose into cotton floc, filtering to obtain the nitrocellulose, and regulating the humidity of the nitrocellulose to 15% by using distilled water. Uniformly mixing the nitrified bamboo cellulose with other raw materials to obtain a mixture, slowly dripping the adhesive A obtained in the step (2), granulating, and sieving with a 100-mesh sieve after finishing.
Adding the starch glue obtained in the step (2) according to a differential method, and granulating. The starch glue in the step (2) is always placed on an electronic balance, and the adding amount of the starch is 130g according to the formula, and the amount of the starch glue to be added is as follows:when the electronic balance shows +> And (3) finishing the addition of the starch glue. After the granulation process is finished, selecting a 100-mesh sieve particle size.
Step (3): uniformly mixing the mixture particles obtained in the step (2) with 240g of expanded perlite, placing the mixture particles in a shady and ventilated place, and airing the mixture particles until the humidity is 3%, thereby obtaining the drop-explosion type firecracker medicament;
weighing 5g of firecracker breaking sample from the firecracker breaking agent crude product, charging, testing, falling to a height higher than 120cm, and displaying the result: the flame retardant type smoke-free flame retardant plastic has the advantages of no smoke, no pungent smell and no dangerousness during the firing, simple and quick processing technology, no dangerousness during the processing, excellent raw material and product stability, good working state and no phenomenon of advanced or delayed explosion.
While the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (5)
1. The utility model provides a fall and explode formula firecracker medicament which characterized in that: the formula is as follows: fine sand, nitrifying bamboo cellulose, a stabilizer, potassium benzoate, melamine and a substance A, wherein the mass ratio of the fine sand to the nitrifying bamboo cellulose is (25-40): (10-16): (7-10): (10-16): (12-20): (8-15);
the substance A is one of starch, phenolic resin, rosin, lactose or white latex;
the preparation method of the nitrified bamboo cellulose comprises the following steps:
step (1): placing the bamboo fiber or bamboo fiber product in a drying oven, wherein the temperature of the oven is controlled to be lower than 100 ℃ until the moisture content of the bamboo fiber or bamboo fiber product is less than 7%;
step (2): preparing a mixed acid solution from concentrated sulfuric acid with the concentration of 60-95% and concentrated nitric acid with the concentration of 70-92%; the mass ratio of the concentrated sulfuric acid to the concentrated nitric acid is as follows: (2.2-3.5): 1.0-2.0);
step (3): adding the bamboo fiber or bamboo fiber product dried in the step (1) into the mixed acid solution in the step (2); controlling the reaction temperature to be lower than 60 ℃, controlling the feeding speed to be 30-180 g/min, controlling the stirring speed to be 60-1200 r/min, taking out after reacting for 5-45 min, and cleaning with cold water to obtain the nitrified bamboo cellulose; the mass ratio of the bamboo fiber or bamboo fiber product to the concentrated nitric acid in the mixed acid solution is (2-20) (6-80);
step (4): putting the nitrified bamboo cellulose obtained in the step (3) into a container, and pouring sodium carbonate solution with the concentration not higher than 18mol/L or sodium bicarbonate solution with the concentration not higher than 25mol/L into the container until the solution is neutral;
step (5): taking out the nitrified bamboo cellulose in the step (4), placing the nitrified bamboo cellulose in a wall breaking machine filled with distilled water or ethanol, preparing the nitrified bamboo cellulose into powder, filtering, drying the powder, and storing the powder in a polyethylene tank or jar; adding distilled water or ethanol into a polyethylene tank or jar; the distilled water content is not less than 11%; the ethanol content is not less than 25%.
2. The utility model provides a fall and explode formula firecracker medicament which characterized in that: the formula is as follows: the weight ratio of the expanded perlite to the nitrogenated bamboo cellulose to the stabilizer to the stearic acid to the melamine to the substance A is (20-28): (12-15): (15-18): (12-18): (15-20): (10-16);
the substance A is one of starch, phenolic resin, rosin, lactose or white latex;
the preparation method of the nitrified bamboo cellulose comprises the following steps:
step (1): placing the bamboo fiber or bamboo fiber product in a drying oven, wherein the temperature of the oven is controlled to be lower than 100 ℃ until the moisture content of the bamboo fiber or bamboo fiber product is less than 7%;
step (2): preparing a mixed acid solution from concentrated sulfuric acid with the concentration of 60-95% and concentrated nitric acid with the concentration of 70-92%; the mass ratio of the concentrated sulfuric acid to the concentrated nitric acid is as follows: (2.2-3.5): 1.0-2.0);
step (3): adding the bamboo fiber or bamboo fiber product dried in the step (1) into the mixed acid solution in the step (2); controlling the reaction temperature to be lower than 60 ℃, controlling the feeding speed to be 30-180 g/min, controlling the stirring speed to be 60-1200 r/min, taking out after reacting for 5-45 min, and cleaning with cold water to obtain the nitrified bamboo cellulose; the mass ratio of the bamboo fiber or bamboo fiber product to the concentrated nitric acid in the mixed acid solution is (2-20) (6-80);
step (4): putting the nitrified bamboo cellulose obtained in the step (3) into a container, and pouring sodium carbonate solution with the concentration not higher than 18mol/L or sodium bicarbonate solution with the concentration not higher than 25mol/L into the container until the solution is neutral;
step (5): taking out the nitrified bamboo cellulose in the step (4), placing the nitrified bamboo cellulose in a wall breaking machine filled with distilled water or ethanol, preparing the nitrified bamboo cellulose into powder, filtering, drying the powder, and storing the powder in a polyethylene tank or jar; adding distilled water or ethanol into a polyethylene tank or jar; the distilled water content is not less than 11%; the ethanol content is not less than 25%.
3. The medicament of claim 1 or 2, wherein: the stabilizer is one of sodium carbonate and sodium bicarbonate.
4. The medicament of claim 1 or 2, wherein: the bamboo fiber product is bamboo fiber paper or bamboo fiber yarn.
5. A method of preparing the medicament of claim 1, wherein: the preparation method comprises the following specific preparation steps:
step (1): selecting fine sand with the grain diameter of 15-100 meshes;
step (2): weighing a substance A, and preparing to obtain an A adhesive with the mass percentage concentration of 2% -42%;
step (3): weighing other raw materials except fine sand according to a formula; firstly, placing the nitrocellulose in a wall breaking machine containing 2/3 distilled water or ethanol, beating the nitrocellulose into cotton floc, filtering to obtain the nitrocellulose, and regulating the humidity of the nitrocellulose to be not less than 10% by using distilled water or ethanol; uniformly mixing the nitrified bamboo cellulose with other raw materials to obtain a mixture, slowly dripping the adhesive A obtained in the step (2), granulating, and sieving with a 15-150-mesh sieve after finishing;
the glue A in the step (3) has viscosity, and in actual use, the glue head dropper and the container wall have loss; for the accurate formula, the quantity of the adhesive A is more in actual preparation, the adhesive A is added by adopting a differential method, the dripping termination is determined according to the adhesive A allowance, and the adhesive A allowance is determined by the following formula:
M dosage of A glue =M Total amount of A glue -M Adhesive margin A ;
Wherein m is A In order to break the dosage of the substance A in the explosion formula, a percent is the mass percentage concentration of the colloid A obtained in the step (2), M Total amount of A glue The weighing is obtained in the step (2), and the weighing is known;
step (4): and (3) uniformly mixing the mixture particles obtained in the step (3) with the fine sand obtained in the step (1), placing the mixture particles in a shady and cool ventilation place, and airing until the humidity is lower than 5%, thereby obtaining the drop-explosion type firecracker medicament.
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