CN115322062A - Novel initiating explosive and preparation method thereof - Google Patents

Novel initiating explosive and preparation method thereof Download PDF

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Publication number
CN115322062A
CN115322062A CN202211037779.5A CN202211037779A CN115322062A CN 115322062 A CN115322062 A CN 115322062A CN 202211037779 A CN202211037779 A CN 202211037779A CN 115322062 A CN115322062 A CN 115322062A
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tank
suction filtration
ethanol
temperature
drying
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杨昌德
乔秀泉
于双泉
刘刚
刘国华
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Shandong Taishan Explosive Materials Co ltd
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Shandong Taishan Explosive Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B33/00Compositions 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
    • C06B33/08Compositions 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
    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B21/00Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • C06B21/0008Compounding the ingredient
    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B21/00Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • C06B21/0033Shaping the mixture

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Drilling And Exploitation, And Mining Machines And Methods (AREA)

Abstract

The invention discloses a novel initiating explosive, which belongs to the technical field of blasting equipment and comprises the following materials: 3.4-3.6 parts of minium, 2-2.4 parts of silicon and 80-100 parts of SY initiating explosive, and by preparing a certain amount of SY initiating explosive and adding silicon and minium with a certain proportion and fineness, because the silicon and the minium with a certain proportion and fineness are combustion agents, the flame sensitivity of the powder can be greatly improved, and the detonation growth period is easy to shorten; because silicon and the minium that add are thinner, can cladding SY initiating explosive, therefore solved the easy moisture absorption's of SY initiating explosive characteristics, improved its free flowing performance simultaneously, because silicon and minium avoid the direct contact of SY initiating explosive and other article to the cladding of SY initiating explosive, therefore can not produce the corruption to other materials, the result of use is better.

Description

Novel initiating explosive and preparation method thereof
Technical Field
The invention relates to the technical field of blasting equipment, in particular to a novel initiating explosive and a preparation method thereof.
Background
Triethylene diamine perchlorate ethylenediamine perchlorate eutectic initiating explosive is a eutectic initiating explosive, and the initiating explosive has the defects of high stability, high temperature resistance, easy moisture absorption, poor free-running property and difficult explosive charging; the flame sensitivity is low, so that the detonation growth period is long, and the single initiating explosive is not suitable to be used; the initiating explosive has high acidity, is easy to corrode substances in contact with the initiating explosive, and has poor using effect, so a novel initiating explosive and a preparation method thereof are needed.
Disclosure of Invention
The invention aims to provide a novel initiating explosive and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a novel initiating explosive comprises the following materials:
3.4 to 3.6 parts of minium, 2 to 2.4 parts of silicon and 80 to 100 parts of SY initiating explosive.
Preferably, the lead and silicon have a particle size of 2.5 μm.
The invention also provides a novel method for preparing the initiating explosive, which comprises the following steps:
s1, preparing SY initiating explosive:
step 1: SY raw material preparation, 1.08kg of ethylenediamine, 2.016kg of triethylenediamine, perchloric acid: not less than 72.0%, ethanol: content is not less than 95%, deionized water: the conductivity is 0.1-1us/cm;
and 2, step: preparing SY base solution, namely slowly pouring 2.016kg of metered triethylene diamine and 1.08kg of ethylene diamine into a chemical combination tank along the edge of the chemical combination tank, starting heating and stirring equipment in the chemical combination tank to start stirring at a stirring speed of 75-250r/min, starting a heating device of the chemical combination tank, heating to 50 ℃, closing the heating device, observing that the triethylene diamine is completely dissolved, and controlling the temperature to be 50 ℃ for later use;
and 3, step 3: SY chemical combination and crystallization, a charging manual control valve of a perchloric acid tank is opened, 10.08kg of perchloric acid liquid is set in charging quantity, 10.08kg of perchloric acid is metered into the chemical combination tank, the charging speed is controlled to be 15 +/-1 minutes, the flow speed value of a flow meter is controlled to be 26 +/-2, liquid adding is stopped when the charging quantity reaches the set quantity, deionized water is injected into the chemical combination tank when the liquid medicine reaction temperature exceeds 80 ℃, deionized water is properly injected into the chemical combination tank for cooling, chloric acid adding is stopped when the deionized water adding cooling measure is invalid, a chemical combination tank cooling device is immediately started to start cooling treatment, chloric acid adding is continued after the temperature is effectively controlled, the chemical combination tank cooling device is started for cooling, circulating cooling water is added into an interlayer in the chemical combination tank in the continuous stirring process, SY crystallization is started when the liquid medicine temperature is reduced to about 50 ℃, the SY crystallization is continued to be cooled to 9 ℃, the temperature is confirmed to be qualified through a machine, cooling is stopped after the temperature is reduced, cooling of the chemical combination tank is qualified, and the SY is finished;
and 4, step 4: SY suction filtration and dehydration are carried out, stirring equipment is closed after SY crystallization is finished, an operator opens an explosion-proof door and enters an operation room to check the state of SY products in a combination tank, and emptying is carried out after visual inspection is qualified;
before discharging, checking that no impurities exist in the leaching tank, accurately checking and checking the liquid level measurement of the mother liquid tank, the liquid level measurement of the recovered ethanol tank and the temperature measurement of the mother liquid tank, and ensuring that a ventilation fan, a mother liquid leaching diaphragm valve, an ethanol leaching diaphragm valve and a manual valve of the leaching tank are safe and reliable, the liquid level of the ethanol tank is normal, the vacuum pressure is-0.08 mpa, and the temperature in the chemical combination tank does not exceed 10 ℃;
an operator washes a suction filtration tank clean, and spreads clean white cotton cloth without holes and defects on a filter screen of the suction filtration tank layer by layer, wherein the number of the white cotton cloth is not less than two, and the edge of the filter cloth is completely arranged outside the opening of the suction filtration tank;
in the discharging process, starting stirring equipment in the chemical combination tank, keeping the stirring speed at 45r/min, and putting the materials in the chemical combination tank into a suction filtration tank;
and (3) mother liquor suction filtration: after the discharge of the chemical combination tank is finished, closing the stirring equipment, closing the discharge program, starting a suction filtration program, opening the suction filtration tank for suction filtration, and suction-filtering the mother liquor in the chemical combination tank into a mother liquor tank through a suction filtration manual valve, wherein the suction filtration time is not less than 10min, after the suction filtration is finished, closing the suction filtration program, closing the suction filtration manual valve of the suction filtration tank, and finishing the suction filtration of the mother liquor;
ethanol dehydration: opening an ethanol tank discharging manual valve, starting a discharging program, placing the ethanol tank discharging manual valve above a medicament in a suction filtration tank through an ethanol discharging hose, opening the ethanol discharging manual valve above the suction filtration tank, placing ethanol into the suction filtration tank, simultaneously stirring SY materials by using a wood tool to fully mix the SY materials with the ethanol, closing the ethanol discharging manual valve after the SY materials are completely soaked by the ethanol, starting a recovery program, opening the suction filtration tank suction filtration manual valve, starting to pump the ethanol into the ethanol recovery tank, closing the suction filtration tank suction filtration manual valve after the suction filtration time is 10min, injecting the ethanol into the suction filtration tank again, carrying out the process for three times, grinding the medicament surface by using a wood shovel during each suction filtration to prevent air permeability from influencing the suction filtration effect, stopping the suction filtration program after the last suction filtration time is not less than 15min, closing the suction filtration tank suction filtration manual valve, a vacuum pump and the vacuum pump, and finishing ethanol dehydration;
and 5: SY is dispersed in a tray, a wet SY material is poured onto a tray machine medicine tray, a drying tray is placed on an electronic balance, balance weight display is reset to zero, a medicine dispersing comb is operated to scrape the SY material on the tray machine onto the drying tray, a monitor is used for observing that about 534g +/-10 g of medicine on the balance is achieved, and medicine scraping is stopped according to 400g of dry product;
after the medicine is taken off, the medicine tray is conveyed to a SY drying room;
and 6: SY drying, wherein the medicine tray is manually placed in a drying room, the dryer is automatically closed, heating and vacuumizing are carried out according to process setting parameters, the temperature and the vacuum degree reach set values, heating and vacuumizing are stopped, automatic timing is carried out, the process setting time is reached, automatic emptying is carried out, the dryer is automatically opened, and the manual material taking is carried out to finish a drying process;
placing the medicines on a heating plate of a vacuum dryer disc by disc in a drying chamber in the order from top to bottom, firstly placing the medicines from the middle to the two sides, enabling the distance between the drying discs and the inner wall of the dryer to be not less than 100mm, checking that the temperature before pumping is not lower than 30 ℃, enabling the temperatures of the heating plates to be consistent, leaving the drying chamber, tightly closing an iron door, tightly closing an air release switch, tightly closing an explosion-proof door of the drying chamber, and carrying out automatic drying treatment;
vacuum pumping treatment is carried out through a vacuum pump in the drying process;
drying for a specified time, completely closing the vacuum pump and the air extraction switch, opening the evacuation valve, slowly introducing air for 5min, then opening another air inlet valve for about 10min, opening the cover of the dryer when the vacuum degree in the tank reaches below 0.020Mpa, cooling the medicine to below 40 ℃, discharging, taking out the medicine tray from the dryer from bottom to top, two sides and the middle at each time when discharging; boxing the sampling disc according to the requirement of the medicine screening process, and carrying out sampling treatment in batches;
s2, mixing the initiating explosive, placing the SY initiating explosive after sampling verification, the red lead and the silicon into the mixer, forming the coating of the red lead and the silicon on the SY initiating explosive after mixing, and completing the preparation of the novel initiating explosive
Preferably, in the step 2 of S1, the initial stirring speed of the stirring device is 70-85r/min, and the stirring speed after feeding is 200-250r/min.
Preferably, in the step 2 of S1, deionized water should be used for no mother liquor in the first production, deionized water is not used for the subsequent production as long as the mother liquor in the mother liquor tank exceeds 9.6kg, a mother liquor tank discharging manual valve or a deionized water tank discharging manual valve is opened, the feeding amount of the mother liquor or the deionized water is set to 9.6kg according to the production control program, and the feeding is automatically stopped by the process when the feeding amount reaches a set value.
Preferably, in the step 3 of S1, the perchloric acid content is not lower than 72.0 percent, no visible impurities exist, the dripping time is controlled to be 14-16 minutes, the temperature during combination is not higher than 80 ℃, the stirring speed is 230-250r/min, and the temperature during discharging is not higher than 10 ℃.
Preferably, in the step 4 of S1, the ethanol dehydration times are not less than 3, each suction filtration time is 10-20min, and the storage temperature of the mother liquor is 15-30 ℃.
Preferably, in step S1 and step 5, the air pressure of the tray separator is 0.4MPa to 0.5MPa, and in step S1 and step 6, the drying temperature of the vacuum dryer is: not higher than 55 ℃, vacuum degree: -0.05Mpa to-0.08 Mpa, compressed air pressure: 0.6-0.8 Mpa, dry dose: less than or equal to 5Kg per tank; vacuum drying time: not less than 40min, drying moisture: not more than 0.05%.
Preferably, in the S2, the mixer is a gravity-free sealed mixer, and the mixing time is 10-15min.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, by preparing quantitative SY initiating explosive and adding silicon and lead with a certain proportion and fineness, the flame sensitivity of the SY initiating explosive can be greatly improved and the detonation growth period is easy to shorten as the silicon and lead with a certain proportion and fineness are combustion agents; because the added silicon and the red lead are thinner and can coat the SY initiating explosive, the characteristic that the SY initiating explosive is easy to absorb moisture is solved, and meanwhile, the flowing and dispersing performance of the SY initiating explosive is improved.
Drawings
FIG. 1 is a schematic flow chart of the raw material metering of the present invention;
FIG. 2 is a schematic diagram of a preparation process in the present invention;
FIG. 3 is a comparative illustration of the force and severity of a detonation in accordance with the present invention;
FIG. 4 is a comparison of impact sensitivity test data for the present invention;
fig. 5 is a comparative data plot of moisture encapsulation in accordance with the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Referring to fig. 1-5, the present invention provides a technical solution:
a novel primary explosive comprises the following materials:
3.4-3.6 parts of minium, 2-2.4 parts of silicon and 80-100 parts of SY initiating explosive.
Specifically, the particle size of the red lead and the silicon is 2.5 mu m.
The invention also provides a novel method for preparing the initiating explosive, which comprises the following steps:
s1, SY initiating explosive preparation:
step 1: SY raw material preparation, 1.08kg of ethylenediamine, 2.016kg of triethylenediamine, perchloric acid: not less than 72.0%, ethanol: content is not less than 95%, deionized water: the conductivity is 0.1-1us/cm;
step 2: preparing SY base solution, namely slowly pouring 2.016kg of metered triethylene diamine and 1.08kg of ethylene diamine into a chemical combination tank along the edge of the chemical combination tank, starting heating and stirring equipment inside the chemical combination tank to start stirring at a stirring speed of 75-250r/min, starting a heating device of the chemical combination tank, heating to 50 ℃, closing the heating device, observing that the triethylene diamine is completely dissolved, and controlling the temperature to be 50 ℃ for later use;
and step 3: SY is combined and crystallized, a charging manual control valve of a perchloric acid tank is opened, the charging quantity of perchloric acid charging liquid is set to be 10.08kg, 10.08kg of perchloric acid is metered into the combination tank, the charging speed is controlled to be 15 +/-1 minutes, the flow speed value of a flow meter is controlled to be 26 +/-2, the charging liquid is stopped when the charging quantity reaches the set quantity, deionized water is injected into the combination tank when the reaction temperature of liquid medicine exceeds 80 ℃, the deionized water is properly injected into the combination tank for cooling, the perchloric acid is stopped when the deionized water charging temperature reduction measure is invalid, a temperature reduction device of the combination tank is immediately started, the temperature reduction treatment is started, the perchloric acid is continued after the temperature is effectively controlled, the charging liquid of the combination tank is finished, a cooling device of the combination tank is started for cooling, circulating cooling water is added into an interlayer in the combination tank in the process of continuing stirring, SY starts crystallization when the temperature of the liquid medicine is reduced to about 50 ℃, the SY is continued to be cooled to be qualified after the temperature is reduced by a machine, the cooling of the combination tank is stopped after the liquid is qualified, and the crystal is finished;
and 4, step 4: SY suction filtration and dehydration are carried out, stirring equipment is closed after SY crystallization is finished, an operator opens an explosion-proof door and enters an operation room to check the state of SY products in a combination tank, and emptying is carried out after visual inspection is qualified;
before discharging, checking that no impurities exist in the leaching tank, accurately checking and checking the liquid level measurement of the mother liquid tank, the liquid level measurement of the recovered ethanol tank and the temperature measurement of the mother liquid tank, and ensuring that a ventilation fan, a mother liquid leaching diaphragm valve, an ethanol leaching diaphragm valve and a manual valve of the leaching tank are safe and reliable, the liquid level of the ethanol tank is normal, the vacuum pressure is-0.08 mpa, and the temperature in the chemical combination tank does not exceed 10 ℃;
an operator washes a suction filtration tank clean, and spreads clean white cotton cloth without holes and defects on a filter screen of the suction filtration tank layer by layer, wherein the number of the white cotton cloth is not less than two, and the edge of the filter cloth is completely arranged outside the opening of the suction filtration tank;
in the discharging process, starting stirring equipment in the chemical combination tank, keeping the stirring speed at 45r/min, and putting the materials in the chemical combination tank into a suction filtration tank;
and (3) mother liquor suction filtration: after the discharge of the chemical combination tank is finished, closing the stirring equipment, closing the discharge program, starting the suction filtration program, opening the suction filtration tank for suction filtration, suction-filtering the mother liquor in the chemical combination tank into the mother liquor tank through a suction filtration manual valve, wherein the suction filtration time is not less than 10min, closing the suction filtration program after the suction filtration is finished, closing the suction filtration manual valve of the suction filtration tank, and finishing the suction filtration of the mother liquor;
ethanol dehydration: opening an ethanol tank discharging manual valve, starting a discharging program, placing the ethanol tank discharging manual valve above a medicament in a suction filtration tank through an ethanol discharging hose, opening the ethanol discharging manual valve above the suction filtration tank, placing ethanol into the suction filtration tank, simultaneously stirring SY materials by using a wood tool to fully mix the SY materials with the ethanol, closing the ethanol discharging manual valve after the SY materials are completely soaked by the ethanol, starting a recovery program, opening the suction filtration tank suction filtration manual valve, starting to pump the ethanol into the ethanol recovery tank, closing the suction filtration tank suction filtration manual valve after the suction filtration time is 10min, injecting the ethanol into the suction filtration tank again, carrying out the process for three times, grinding the medicament surface by using a wood shovel during each suction filtration to prevent air permeability from influencing the suction filtration effect, stopping the suction filtration program after the last suction filtration time is not less than 15min, closing the suction filtration tank suction filtration manual valve, a vacuum pump and the vacuum pump, and finishing ethanol dehydration;
and 5: SY is divided and dispersed, a wet SY material is poured on a medicine tray of a dividing machine, a drying tray is taken and placed on an electronic balance, the weight display of the balance is reset to zero, a medicine dispersing comb is operated to scrape the SY material on the dividing machine onto the drying tray, a monitor is used for observing that the medicine on the balance reaches about 534g +/-10 g, and medicine scraping is stopped according to 400g of dry products;
after the medicine is taken out, the medicine tray is conveyed to a SY drying room;
and 6: SY drying, wherein the medicine tray is manually placed in a drying room, the dryer is automatically closed, heating and vacuumizing are carried out according to process setting parameters, the temperature and the vacuum degree reach set values, heating and vacuumizing are stopped, automatic timing is carried out, the process setting time is reached, automatic emptying is carried out, the dryer is automatically opened, and the manual material taking is carried out to finish a drying process;
placing the medicines on a heating plate of a vacuum dryer one by one in a drying chamber from top to bottom in the placing sequence, placing the medicines from the middle to the two sides, keeping the distance between the drying plate and the inner wall of the dryer to be not less than 100mm, checking that the temperature before pumping is not lower than 30 ℃, keeping the temperature of each heating plate consistent, leaving the drying chamber, tightly closing an iron door, tightly closing an air release switch, tightly closing an explosion-proof door of the drying chamber, and carrying out automatic drying treatment;
vacuum pumping treatment is carried out through a vacuum pump in the drying process;
drying for a specified time, completely closing the vacuum pump and the air extraction switch, opening the evacuation valve, slowly introducing air for 5min, then opening another air inlet valve for about 10min, opening the cover of the dryer when the vacuum degree in the tank reaches below 0.020Mpa, cooling the medicine to below 40 ℃, discharging, taking out the medicine tray from the dryer from bottom to top, two sides and the middle at each time when discharging; boxing the sampling disc according to the requirement of the medicine screening process, and sampling in batches;
s2, mixing the initiating explosive, placing the SY initiating explosive after sampling verification, the red lead and the silicon into the mixer, and forming the coating of the red lead and the silicon on the SY initiating explosive after mixing to complete the preparation of the novel initiating explosive.
Specifically, in the step 2 of S1, the initial stirring speed of the stirring equipment is 70-85r/min, and the stirring speed after feeding is 200-250r/min.
Specifically, in the step 2 of S1, deionized water is not used in the first production when no mother liquor is used, deionized water is not used in the subsequent production as long as the mother liquor in the mother liquor tank exceeds 9.6kg, a mother liquor tank discharging manual valve or a deionized water tank discharging manual valve is opened, the feeding quantity of the mother liquor or the deionized water is set to be 9.6kg according to a production control program, and the feeding is automatically stopped in the process when the feeding quantity reaches a set value.
Specifically, in the step 3 of S1, the perchloric acid content is not lower than 72.0%, no visible impurity exists, the dripping time is controlled to be 14-16 minutes, the temperature is not higher than 80 ℃ during combination, the stirring speed is 230-250r/min, and the temperature is not higher than 10 ℃ during discharging.
Specifically, in the step S1 and step 3, the temperature of the combination tank is controlled within 80 ℃, and the heating should be stopped immediately when the temperature of the combination tank rises sharply or other abnormal conditions are found.
Specifically, in the step 4 of S1, the ethanol dehydration times are not less than 3, each suction filtration time is 10-20min, and the storage temperature of the mother liquor is 15-30 ℃.
Specifically, in step S1 and step 5, the air pressure of the tray separator is 0.4MPa to 0.5MPa, and in step S1 and step 6, the drying temperature of the vacuum dryer is: not higher than 55 ℃, vacuum: -0.05Mpa to-0.08 Mpa, compressed air pressure: 0.6-0.8 Mpa, dry dose: less than or equal to 5Kg per tank; and (3) vacuum drying time: not less than 40min, drying moisture: not more than 0.05%.
Specifically, in S2, the mixer is a gravity-free sealed mixer, and the mixing time is 10-15min.
According to the technical scheme, the working steps of the scheme are summarized and carded: according to the invention, by preparing quantitative SY initiating explosive and adding silicon and lead with a certain proportion and fineness, the flame sensitivity of the SY initiating explosive can be greatly improved and the detonation growth period is easy to shorten as the silicon and lead with a certain proportion and fineness are combustion agents; because the added silicon and the red lead are thinner and can coat the SY initiating explosive, the characteristic that the SY initiating explosive is easy to absorb moisture is solved, and meanwhile, the flowing and dispersing performance of the SY initiating explosive is improved.
As shown in fig. 5, experimental case one:
hygroscopicity comparison, the hygroscopicity comparison of SY drug with those coated with minium silicon, the environment for placing the drug: in the vessel, the temperature is 30.5 ℃ and the humidity is 100 percent.
As shown in fig. 3, test case two:
SY is compared with the power of TNT, PDX and PETN explosives, and the explosive power of each explosive are compared.
As shown in fig. 4, experimental case three:
1. the impact sensitivity test was carried out on the explosive agents such as LTNR, LDNP, sodium salt, GTX.GTG, etc., 25 doses were tested per sample, and the dose per dose was 20mg, using an ascending and descending method. The lifting method can concentrate most of the tested information near 50% of explosion points by using less test times, can obtain accurate results by using only 20 to 30 samples, and is simple and convenient to operate. Lifting method test procedure: let ho denote the level of the initial trial (zero level), d denote equal spacing of the drop height, and the value of d should be chosen to approximate the standard deviation. The test is first carried out at ho, if the sample explodes, it is indicated by "1", and the next test should be carried out at ho-d with the falling height: if the test is carried out at ho and the test specimen is not explosive, it is indicated by "0", and the next test should be carried out with an increased drop height at ha + d, and so on. The test level is hodd.ho +2d.ho soil 3d.
2. And (3) performing friction sensitivity test on each sample by using a friction sensitivity instrument. For initiating explosive such as initiating explosive and the like, a 60-degree swing angle and a pressure of 0.88MPa are generally selected for operation, the swing angle and the pressure can float along with the phenomenon in the test, and finally, the ignition probability under a certain swing angle pressure is taken to evaluate the sensitivity of a sample. In the test, if the medicament explodes, burns, emits light, smokes or changes color, the medicament is considered to be ignited.
The parts not involved in the present invention are the same as or can be implemented by the prior art. Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. The novel primary explosive is characterized by comprising the following materials:
3.4 to 3.6 parts of minium, 2 to 2.4 parts of silicon and 80 to 100 parts of SY initiating explosive.
2. A novel primary explosive according to claim 1, wherein: the lead and the silicon have the particle size of 2.5 mu m.
3. The novel method for preparing the primary explosive according to claim 1, wherein: the method comprises the following steps:
s1, SY initiating explosive preparation:
step 1: SY raw material preparation, 1.08kg of ethylenediamine, 2.016kg of triethylenediamine, perchloric acid: not less than 72.0%, ethanol: content is not less than 95%, deionized water: the conductivity is 0.1-1us/cm;
and 2, step: preparing SY base solution, namely slowly pouring 2.016kg of metered triethylene diamine and 1.08kg of ethylene diamine into a chemical combination tank along the edge of the chemical combination tank, starting heating and stirring equipment inside the chemical combination tank to start stirring at a stirring speed of 75-250r/min, starting a heating device of the chemical combination tank, heating to 50 ℃, closing the heating device, observing that the triethylene diamine is completely dissolved, and controlling the temperature to be 50 ℃ for later use;
and step 3: SY is combined and crystallized, a charging manual control valve of a perchloric acid tank is opened, the charging quantity of perchloric acid charging liquid is set to be 10.08kg, 10.08kg of perchloric acid is metered into the combination tank, the charging speed is controlled to be 15 +/-1 minutes, the flow speed value of a flow meter is controlled to be 26 +/-2, the charging liquid is stopped when the charging quantity reaches the set quantity, deionized water is injected into the combination tank when the reaction temperature of liquid medicine exceeds 80 ℃, the deionized water is properly injected into the combination tank for cooling, the perchloric acid is stopped when the deionized water charging temperature reduction measure is invalid, a temperature reduction device of the combination tank is immediately started, the temperature reduction treatment is started, the perchloric acid is continued after the temperature is effectively controlled, the charging liquid of the combination tank is finished, a cooling device of the combination tank is started for cooling, circulating cooling water is added into an interlayer in the combination tank in the process of continuing stirring, SY starts crystallization when the temperature of the liquid medicine is reduced to about 50 ℃, the SY is continued to be cooled to be qualified after the temperature is reduced by a machine, the cooling of the combination tank is stopped after the liquid is qualified, and the crystal is finished;
and 4, step 4: SY suction filtration and dehydration, SY crystallization, stirring equipment closing, an operator opening an explosion door, entering an operation room, checking the state of SY products in a combination tank, and preparing for emptying after visual inspection is qualified;
before discharging, checking that no impurities exist in the filtration tank, accurately checking and checking the liquid level measurement of the mother liquid tank, the liquid level measurement of the recovered ethanol tank and the temperature measurement of the mother liquid tank, wherein a ventilation fan, a mother liquid filtration diaphragm valve, an ethanol filtration diaphragm valve and a manual control valve of the filtration tank are safe and reliable, the liquid level of the ethanol tank is normal, the vacuum pressure is-0.08 mpa, and the temperature in the chemical combination tank is not more than 10 ℃;
an operator washes a suction filtration tank clean, and spreads clean white cotton cloth without holes and defects on a filter screen of the suction filtration tank layer by layer, wherein the number of the white cotton cloth is not less than two, and the edge of the filter cloth is completely arranged outside the opening of the suction filtration tank;
in the discharging process, starting stirring equipment in the chemical combination tank, keeping the stirring speed at 45r/min, and putting the materials in the chemical combination tank into a suction filtration tank;
and (3) mother liquor suction filtration: after the discharge of the chemical combination tank is finished, closing the stirring equipment, closing the discharge program, starting the suction filtration program, opening the suction filtration tank for suction filtration, suction-filtering the mother liquor in the chemical combination tank into the mother liquor tank through a suction filtration manual valve, wherein the suction filtration time is not less than 10min, closing the suction filtration program after the suction filtration is finished, closing the suction filtration manual valve of the suction filtration tank, and finishing the suction filtration of the mother liquor;
ethanol dehydration: opening an ethanol tank discharging manual valve, starting a discharging program, placing the ethanol tank discharging manual valve above a medicament in a suction filtration tank through an ethanol discharging hose, opening the ethanol discharging manual valve above the suction filtration tank, placing ethanol into the suction filtration tank, simultaneously stirring SY materials by using a wood tool to fully mix the SY materials with the ethanol, closing the ethanol discharging manual valve after the SY materials are completely soaked by the ethanol, starting a recovery program, opening the suction filtration tank suction filtration manual valve, starting to pump the ethanol into the ethanol recovery tank, closing the suction filtration tank suction filtration manual valve after the suction filtration time is 10min, injecting the ethanol into the suction filtration tank again, carrying out the process for three times, grinding the medicament surface by using a wood shovel during each suction filtration to prevent air permeability from influencing the suction filtration effect, stopping the suction filtration program after the last suction filtration time is not less than 15min, closing the suction filtration tank suction filtration manual valve, a vacuum pump and the vacuum pump, and finishing ethanol dehydration;
and 5: SY is divided and dispersed, a wet SY material is poured on a medicine tray of a dividing machine, a drying tray is taken and placed on an electronic balance, the weight display of the balance is reset to zero, a medicine dispersing comb is operated to scrape the SY material on the dividing machine onto the drying tray, a monitor is used for observing that the medicine on the balance reaches about 534g +/-10 g, and medicine scraping is stopped according to 400g of dry products;
after the medicine is taken off, the medicine tray is conveyed to a SY drying room;
step 6: SY drying, wherein the medicine tray is manually placed in a drying room, the dryer is automatically closed, heating and vacuumizing are carried out according to process setting parameters, the temperature and the vacuum degree reach set values, heating and vacuumizing are stopped, automatic timing is carried out, the process setting time is reached, automatic emptying is carried out, the dryer is automatically opened, and the manual material taking is carried out to finish a drying process;
placing the medicines on a heating plate of a vacuum dryer disc by disc in a drying chamber in the order from top to bottom, firstly placing the medicines from the middle to the two sides, enabling the distance between the drying discs and the inner wall of the dryer to be not less than 100mm, checking that the temperature before pumping is not lower than 30 ℃, enabling the temperatures of the heating plates to be consistent, leaving the drying chamber, tightly closing an iron door, tightly closing an air release switch, tightly closing an explosion-proof door of the drying chamber, and carrying out automatic drying treatment;
vacuum pumping treatment is carried out through a vacuum pump in the drying process;
drying for a set time, completely closing the vacuum pump and the air extraction switch, opening the evacuation valve, slowly introducing air for 5min, then opening another air inlet valve for about 10min, opening the cover of the dryer when the vacuum degree in the tank reaches below 0.020MPa, cooling the medicine to below 40 ℃, discharging, taking out the medicine tray from the bottom to the top, two sides and the middle of the dryer at each time when discharging; boxing the sampling disc according to the requirement of the medicine screening process, and carrying out sampling treatment in batches;
s2, mixing the initiating explosive, placing SY initiating explosive after sampling verification, red lead and silicon into a mixer, forming coating of the red lead and the silicon on the SY initiating explosive after mixing, and completing preparation of the novel initiating explosive.
4. The novel method for preparing the primary explosive according to claim 1, wherein: in the step 2 of S1, the initial stirring speed of the stirring equipment is 70-85r/min, and the stirring speed after feeding is 200-250r/min.
5. The novel method for preparing the primary explosive according to claim 1, wherein: in the step 2 of S1, deionized water is not used for mother liquor in the first production, deionized water is not used for subsequent production as long as mother liquor in a mother liquor tank exceeds 9.6kg, a mother liquor tank discharging manual valve or a deionized water tank discharging manual valve is opened, the feeding quantity of the mother liquor or the deionized water is set to be 9.6kg according to a production control program in the control program, and the feeding of the mother liquor or the deionized water is automatically stopped by the control program when the feeding quantity reaches a set numerical value.
6. The novel method for preparing the primary explosive according to claim 1, wherein: in the step 3 of S1, the perchloric acid content is not lower than 72.0 percent, no visible impurities exist, the dripping time is controlled to be 14-16 minutes, the temperature during combination is not higher than 80 ℃, the stirring speed is 230-250r/min, and the temperature during discharging is not higher than 10 ℃.
7. The novel method for preparing the primary explosive according to claim 1, wherein: in the step S1 and the step 3, the temperature of the chemical combination tank is controlled within 80 ℃, and the heating is stopped immediately when the chemical combination tank is found to be suddenly increased or other abnormal conditions occur.
8. The novel method for preparing the initiating explosive according to claim 1, wherein the method comprises the following steps: in the step 4 of S1, the ethanol dehydration times are not less than 3, the suction filtration time is 10-20min each time, and the storage temperature of the mother liquor is 15-30 ℃.
9. The novel method for preparing the initiating explosive according to claim 1, wherein the method comprises the following steps: in the step 5 of S1, the air pressure of the disc separator is 0.4MPa-0.5MPa, and in the step 6 of S1, the drying temperature of the vacuum dryer is as follows: not higher than 55 ℃, vacuum degree: -0.05Mpa to-0.08 Mpa, compressed air pressure: 0.6 Mpa-0.8 Mpa, and the dry drug quantity: less than or equal to 5Kg per tank; and (3) vacuum drying time: not less than 40min, drying moisture: not more than 0.05%.
10. The novel method for preparing the primary explosive according to claim 1, wherein: in the S2, the mixer is a gravity-free sealed mixer, and the mixing time is 10-15min.
CN202211037779.5A 2022-08-27 2022-08-27 Novel initiating explosive and preparation method thereof Pending CN115322062A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1474157A (en) * 2002-08-06 2004-02-11 武汉安全环保研究院 Simplified detonating element for no-initiator detonator
CN101570459A (en) * 2008-04-30 2009-11-04 南京理工大学 Ethylenediamine perchlorate.triethylene diamine perchlorate eutectic initiating explosive and preparation method thereof
CN202793187U (en) * 2011-08-24 2013-03-13 安徽理工大学 Non-primary explosive detonator
CN104211548A (en) * 2014-07-02 2014-12-17 北京理工大学 Continuous automatic production technology and production line of primary explosive pyrotechnic medicine
WO2021147960A1 (en) * 2020-01-22 2021-07-29 中山大学 Compounds and preparation method therefor and use thereof as energetic materials
CN113929641A (en) * 2020-07-14 2022-01-14 西安固能新材料科技有限公司 Serial ethylenediamine ternary crystalline compounds, preparation method thereof and application thereof as energetic materials

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1474157A (en) * 2002-08-06 2004-02-11 武汉安全环保研究院 Simplified detonating element for no-initiator detonator
CN101570459A (en) * 2008-04-30 2009-11-04 南京理工大学 Ethylenediamine perchlorate.triethylene diamine perchlorate eutectic initiating explosive and preparation method thereof
CN202793187U (en) * 2011-08-24 2013-03-13 安徽理工大学 Non-primary explosive detonator
CN104211548A (en) * 2014-07-02 2014-12-17 北京理工大学 Continuous automatic production technology and production line of primary explosive pyrotechnic medicine
WO2021147960A1 (en) * 2020-01-22 2021-07-29 中山大学 Compounds and preparation method therefor and use thereof as energetic materials
CN113929641A (en) * 2020-07-14 2022-01-14 西安固能新材料科技有限公司 Serial ethylenediamine ternary crystalline compounds, preparation method thereof and application thereof as energetic materials

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