CN113860975A - Safety mixed ignition powder for detonator and preparation method and application thereof - Google Patents
Safety mixed ignition powder for detonator and preparation method and application thereof Download PDFInfo
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- CN113860975A CN113860975A CN202111265138.0A CN202111265138A CN113860975A CN 113860975 A CN113860975 A CN 113860975A CN 202111265138 A CN202111265138 A CN 202111265138A CN 113860975 A CN113860975 A CN 113860975A
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- lead
- potassium perchlorate
- trinitrophloroglucinol
- ignition powder
- detonator
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B29/00—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate
- C06B29/02—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate of an alkali metal
- C06B29/16—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate of an alkali metal with a nitrated organic compound
- C06B29/18—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate of an alkali metal with a nitrated organic compound the compound being nitrated toluene or a nitrated phenol
-
- 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
- C06B23/001—Fillers, gelling and thickening agents (e.g. fibres), absorbents for nitroglycerine
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06C—DETONATING OR PRIMING DEVICES; FUSES; CHEMICAL LIGHTERS; PYROPHORIC COMPOSITIONS
- C06C7/00—Non-electric detonators; Blasting caps; Primers
Abstract
The invention provides a safe mixed ignition powder for a detonator, and a preparation method and application thereof, and belongs to the field of detonator charging. The methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer is a water-soluble polymer, has good bonding performance, can be bonded into particles with good free-running property and high apparent density when the bonding agent amount is 1.0-1.5 wt%, and can fully ensure the initiation performance of the ignition charge due to the small addition amount of the bonding agent; and because of adding the adhesive, the sensitivity of the ignition powder is reduced; the trinitrophloroglucinol lead has good flame sensitivity, but the explosion change acceleration is small, and a certain amount of combustion agent-lead benzoate and oxidant-potassium perchlorate are introduced into the formula so as to make up the defect of initiation of the trinitrophloroglucinol lead in the formula, thereby ensuring that the ignition powder is safe to use and reliable in initiation.
Description
Technical Field
The invention relates to the technical field of detonator charging, in particular to a safe mixed ignition powder for a detonator, and a preparation method and application thereof.
Background
The ignition charge is a core material of a detonating device, directly influences the performance and quality of the detonator, and influences the production safety and economic benefit of enterprises. Because the ignition charge is the necessary raw material with highest sensitivity and highest risk in the technical field of civil blasting equipment, the safety problem in the ignition charge production and detonator filling process is one of the most concerned core problems of enterprises. The preparation of the domestic ignition powder generally adopts a paste sieving method to carry out artificial granulation, selects shellac as a bonding agent, and has the addition amount of 2.5-4 wt%, and the preparation of the ignition powder has the problems of high sensitivity and poor initiation effect.
Disclosure of Invention
In view of the above, the present invention aims to provide a safe mixed ignition powder for detonators, and a preparation method and an application thereof. The safety mixed ignition powder for the detonator provided by the invention has low sensitivity and good detonation effect.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a safe mixed ignition powder for a detonator, which comprises the following components in percentage by weight: 29.5-29.7 wt% of trinitrophloroglucinol lead, 19.7-19.8 wt% of lead benzoate, 49.3-49.5 wt% of potassium perchlorate and 1.0-1.5 wt% of a methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer.
Preferably, the mass ratio of the trinitrophloroglucinol lead to the lead benzoate to the potassium perchlorate is 3:2: 5.
Preferably, the mass ratio of the trinitrophloroglucinol lead to the benzoic acid lead, the potassium perchlorate to the methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer is 4.5:3:7.5: 0.316-0.471.
The invention also provides a preparation method of the safety mixed ignition powder for the detonator, which comprises the following steps:
mixing trinitrophloroglucinol lead, lead benzoate, potassium perchlorate and water to obtain dispersion liquid;
preheating the dispersion to obtain a preheated dispersion;
adding potassium perchlorate into the preheated dispersion liquid to obtain suspension;
mixing the suspension with a methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer to obtain a mixed solution;
mixing the mixed solution with a demulsifier to perform demulsification to obtain a demulsified solution;
dripping an organic solvent into the demulsified solution, granulating and drying to obtain granules;
and passivating the granules to obtain the safety mixed ignition powder for the detonator.
Preferably, the mass ratio of the total mass of the trinitrophloroglucinol lead, the lead benzoate and the potassium perchlorate to the water is 1: (2.5-3).
Preferably, the temperature of the preheating is 50 ± 2 ℃.
Preferably, the total mass of trinitrophloroglucinol lead, lead benzoate and potassium perchlorate is 15kg, and the water-material ratio is (2.5-3): 1, calculating, wherein the mass of the supplementary potassium perchlorate is 1.91-2.30 kg.
Preferably, the particle size of the granules is 0.85-1 mm.
Preferably, the passivation comprises distillation, organic solvent washing, filtration and drying, which are carried out in sequence.
The invention also provides the application of the safety mixed ignition powder for the detonator in the technical scheme in the preparation of the detonator.
The invention provides a safe mixed ignition powder for a detonator, which comprises the following components in percentage by weight: 29.5-29.7 wt% of trinitrophloroglucinol lead, 19.7-19.8 wt% of lead benzoate, 49.3-49.5 wt% of potassium perchlorate and 1.0-1.5 wt% of a methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer. The invention takes the methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer as the adhesive, the methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer is a water-soluble polymer, the adhesive property is good, the adhesive amount is 1.0-1.5 wt%, and the particles with good free-running property and high loose packing density can be bonded; and because of adding the adhesive, the sensitivity of the ignition powder is reduced; the trinitrophloroglucinol lead has good flame sensitivity, but the explosion change acceleration is small, and a certain amount of combustion agent-lead benzoate and oxidant-potassium perchlorate are introduced into the formula so as to make up the defect of initiation of the trinitrophloroglucinol lead in the formula, thereby ensuring that the ignition powder is safe to use and reliable in initiation.
Furthermore, the invention takes the methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer as the adhesive, thereby avoiding the problem that the shellac needs a large amount of solvent to be dissolved and the solvent is volatilized into the atmosphere to cause certain harm to the environment.
The invention also provides a preparation method of the safety mixed ignition powder for the detonator, which comprises the following steps: mixing trinitrophloroglucinol lead, lead benzoate, potassium perchlorate and water to obtain dispersion liquid; preheating the dispersion to obtain a preheated dispersion; adding potassium perchlorate into the preheated dispersion liquid to obtain suspension; mixing the suspension with a methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer to obtain a mixed solution; mixing the mixed solution with a demulsifier to perform demulsification to obtain a demulsified solution; dripping an organic solvent into the demulsified solution and drying to obtain granules; and passivating the granules to obtain the safety mixed ignition powder for the detonator. The invention adopts the 'water suspension preparation process', is safe, reliable, simple and feasible, and is suitable for large-scale production.
Detailed Description
The invention provides a safe mixed ignition powder for a detonator, which comprises the following components in percentage by weight: 29.5-29.7 wt% of trinitrophloroglucinol lead, 19.7-19.8 wt% of lead benzoate, 49.3-49.5 wt% of potassium perchlorate and 1.0-1.5 wt% of a methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer.
In the present invention, unless otherwise specified, the raw materials used are all commercial products available in the art, and specifically, for example, the quaternary copolymer of methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate is available from Shanxi North chemical industry Co., Ltd, model number KY8, and the monomers for synthesizing the quaternary copolymer of methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate include methyl methacrylate, methacrylic acid, acrylic acid and butyl acrylate.
In the invention, the mass ratio of the trinitrophloroglucinol lead, the lead benzoate and the potassium perchlorate is preferably 3:2: 5.
In the invention, the mass ratio of the trinitrophloroglucinol lead, the lead benzoate, the potassium perchlorate and the methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer is preferably 4.5:3:7.5: 0.316-0.471, more preferably 4.5:3:7.5: 0.348-0.412, and most preferably 4.5:3:7.5: 0.380.
In the invention, the solid content of the methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer is preferably 48-49%.
The invention also provides a preparation method of the safety mixed ignition powder for the detonator, which comprises the following steps:
mixing trinitrophloroglucinol lead, lead benzoate, potassium perchlorate and water to obtain dispersion liquid;
preheating the dispersion to obtain a preheated dispersion;
adding potassium perchlorate into the preheated dispersion liquid to obtain suspension;
mixing the suspension with a methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer to obtain a mixed solution;
mixing the mixed solution with a demulsifier to perform demulsification to obtain a demulsified solution;
dripping an organic solvent into the demulsified solution, granulating and drying to obtain granules;
and passivating the granules to obtain the safety mixed ignition powder for the detonator.
The invention mixes trinitrophloroglucinol lead, lead benzoate, potassium perchlorate and water to obtain dispersion.
In the present invention, the mass ratio of the total mass of the trinitrophloroglucinol lead, the lead benzoate and the potassium perchlorate to water is preferably 1: (2.5-3).
The mixing method is not particularly limited in the present invention, and the technical scheme of mixing materials well known to those skilled in the art can be adopted.
In the invention, the mixing is preferably stirring, the stirring is preferably stirring by using a four-blade propeller type, and the stirring speed is preferably 40 +/-5 Hz; the stirring function is to fully and uniformly mix trinitrophloroglucinol lead, lead benzoate and potassium perchlorate in water to obtain dispersion liquid. Because the potassium perchlorate is dissolved in water, after the dispersion liquid is obtained, a certain amount of potassium perchlorate must be supplemented, so that the content of the potassium perchlorate in the safe mixed ignition powder for the detonator is ensured, and the ignition powder can be fully combusted.
After the dispersion liquid is obtained, the invention preheats the dispersion liquid to obtain the preheated dispersion liquid.
In the invention, the preheating temperature is preferably 50 +/-2 ℃, and the rate of heating to the preheating temperature is preferably 1-2 ℃/min; the preheating is preferably performed by heating. In the invention, the preheating has the function of controlling the amount of potassium perchlorate supplemented, and also aims to reach the temperature of demulsification process by adding a demulsifier at the later stage.
After the preheated dispersion liquid is obtained, potassium perchlorate is supplemented into the preheated dispersion liquid to obtain suspension, and the potassium perchlorate can be dissolved in water, so that the potassium perchlorate is supplemented to supplement the amount of the potassium perchlorate dissolved in the water in a mixture of trinitrophloroglucinol lead, lead benzoate and potassium perchlorate at a certain temperature, and the aim of ensuring the mixture ratio of each component in the mixture of the trinitrophloroglucinol lead, the lead benzoate and the potassium perchlorate to be unchanged is achieved.
In the invention, the total mass of trinitrophloroglucinol lead, lead benzoate and potassium perchlorate is 15kg, and the water-material ratio is (2.5-3): 1, the mass of the supplementary potassium perchlorate is preferably 1.91-2.30 kg.
After the potassium perchlorate is supplemented, the method also comprises a mixing step, wherein the mixing is preferably mechanically stirred for 20-30 min.
After the suspension is obtained, the suspension is mixed with the quadripolymer of methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate to obtain a mixed solution.
In the present invention, the mixing is preferably carried out in a granulator.
After the mixed solution is obtained, the mixed solution is mixed with a demulsifier to perform demulsification, so as to obtain a demulsified solution.
In the invention, the mass concentration of the demulsifier is preferably 15-20%, and the dosage of the demulsifier is preferably 3-6% of the total mass of the mixture of trinitrophloroglucinol lead, lead benzoate and potassium perchlorate.
In the invention, the demulsifier is preferably CaCl2Or anhydrous Na2SO4。
In the demulsification process, the adhesive methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate is separated out on the crystal surface of the explosive, is fully contacted with the mixture of trinitrophloroglucinol lead, lead phthalate and potassium perchlorate, and is bonded into particles, so that the finally obtained product has uniform particle size, and the safety of the explosive pressing or charging process is improved.
After the demulsified solution is obtained, the organic solvent is sequentially dripped into the demulsified solution, and granules are obtained after granulation and drying.
In the present invention, the organic solvent is preferably butyl acetate or ethyl acetate.
In the invention, the dripping speed is preferably 4-6 mL/min. In the invention, under the dropping speed, the particles formed at each position in the mixed solution system are uniformly polymerized and grown at a consistent speed, so that the adding process is closely matched with the diffusion process of the organic solvent, and the growth rate of the particles is uniform to the maximum extent. In the invention, the organic solvent bonds the mixture of trinitrophloroglucinol lead, lead benzoate and potassium perchlorate and the quadripolymer of methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate to form a small ball, and gradually dissolves the adhesive to finish the coating process, the adding speed of the organic solvent is high, and the granularity of the particles is larger.
The present invention preferably controls the rate of addition of the organic solvent by sampling to observe the size of the particle size.
In the present invention, the granulation is preferably carried out in a granulator.
In the present invention, the particle size of the pellets is preferably 0.85 to 1 mm.
After the granular materials are obtained, the granular materials are passivated to obtain the safe mixed ignition powder for the detonator.
In the present invention, the passivation preferably includes distillation, organic solvent washing, filtration and drying, which are sequentially performed.
In the invention, the distillation is preferably vacuum distillation, the temperature of the vacuum distillation is preferably 50 ℃, the vacuum degree of the vacuum distillation is preferably 0.01-0.02 MPa, and the distillation is used for removing the organic solvent.
In the present invention, the organic solvent used for the organic solvent washing is preferably absolute ethanol.
In the invention, the mass ratio of the absolute ethyl alcohol to the material to be washed is preferably 1: 1.
in the present invention, the filtration is preferably wet filtration. The anhydrous ethanol is selected because the trinitrophloroglucinol lead, the lead benzoate and the potassium perchlorate are not dissolved in the anhydrous ethanol, so that the effective components of the safe mixed ignition powder for the detonator can be effectively ensured, and the service performance of the booster powder is met; the wet filtration is to remove part of large particles and fine particles which can not meet the use requirement of the product, and to obtain qualified products meeting the requirement; and secondly, the safety risk caused by high mechanical sensitivity of the ignition powder is avoided.
In the invention, the drying is preferably water bath drying, the temperature of the water bath drying is preferably 50-60 ℃, and the time is preferably 4-6 h.
The invention also provides the application of the safety mixed ignition powder for the detonator in the technical scheme in the preparation of the detonator, and the specific mode of the application is not particularly limited, and the mode known by the technical personnel in the field can be adopted.
In order to further illustrate the present invention, the safety mixed ignition charge for detonators provided by the present invention, the preparation method and the application thereof will be described in detail with reference to examples, which should not be construed as limiting the scope of the present invention.
Example 1
(1) Putting a mixture of 4.5kg of trinitrophloroglucinol lead, 3.0kg of lead benzoate and 7.5kg of potassium perchlorate into 37.5kg of water to prepare a dispersion liquid;
(2) starting a water circulation heating system, and heating the dispersion liquid of the mixture of trinitrophloroglucinol lead, lead benzoate and potassium perchlorate to 50 ℃;
(3) adding 1.92Kg of potassium perchlorate solid into 50 ℃ dispersion of a mixture of trinitrophloroglucinol lead, lead phthalate and potassium perchlorate, and fully stirring for 30min to obtain suspension;
(4) adding 0.316kg (solid content is 48%) of methyl methacrylate-isooctyl acrylate adhesive into the suspension to obtain a mixed solution system 1;
(5) adding a demulsifier of 4kg of anhydrous sodium sulfate (15 wt%) solution into the obtained mixed solution system 1 under the condition that the temperature is kept at 50 ℃, and obtaining a mixed solution system 2 after the aqueous solution is clarified;
(6) opening a vacuum system, adding ethyl acetate into the obtained mixed solution system 2 at a speed of 6mL/min for granulation under the conditions that the temperature is kept at 50 ℃ and the vacuum degree is 0.02MPa, and controlling the adding amount of the ethyl acetate by sampling and observing the granularity of orange granules, wherein the more the ethyl acetate is added, the larger the granularity of the orange granules is;
(7) when the granularity of the orange granules reaches 1.00-0.85 mm (18-80 meshes), stopping adding the ethyl acetate, and distilling and removing the ethyl acetate to obtain a suspension system;
(8) when the particles are hard, the ethyl acetate is distilled, the suspension system is poured into absolute ethyl alcohol, then a standard sieve with the particle size of 1.00mm and 0.85mm is adopted for wet screening, and a screen object with the particle size of 1.00 mm-0.85 mm is reserved, so that the novel semi-finished product of the safety mixed ignition powder for the detonator is obtained;
(9) drying the ignition powder obtained by filtering by adopting water bath drying, controlling the water bath drying temperature at 50 ℃ and the water bath drying time at 6h to obtain a novel safety mixed ignition powder for the detonator;
(10) the obtained explosive is detected according to the industrial electric detonator GB8031-2005, the requirement of the national standard No. 8 industrial electric detonator on a lead plate with the explosion penetration thickness of 5mm can be met, the perforation diameter is 11.2mm, and the technical requirement is met.
Example 2:
(1) putting a mixture of 4.5kg of trinitrophloroglucinol lead, 3.0kg of lead benzoate and 7.5kg of potassium perchlorate into 39kg of water to prepare a dispersion liquid;
(2) starting a water circulation heating system, and heating the dispersion liquid of the mixture of trinitrophloroglucinol lead, lead benzoate and potassium perchlorate to 50 ℃;
(3) adding 1.99Kg of potassium perchlorate solid into a dispersion of a mixture of trinitrophloroglucinol lead, lead phthalate and potassium perchlorate at 50 ℃, and fully stirring for 29 min;
(4) adding 0.348kg (solid content is 48%) of methyl methacrylate-isooctyl acrylate adhesive into the suspension to obtain a mixed solution system 1;
(5) adding a demulsifier of 4.5kg of anhydrous sodium sulfate (15 wt%) solution into the obtained mixed solution system 1 under the condition that the temperature is kept at 50 ℃, and obtaining a mixed solution system 2 after the aqueous solution is clarified;
(6) opening a vacuum system, adding ethyl acetate into the obtained mixed solution system 2 at a rate of 5mL/min for granulation under the conditions that the temperature is kept at 50 ℃ and the vacuum degree is 0.015MPa, and controlling the addition amount of the ethyl acetate by sampling and observing the granularity of orange granules, wherein the more the addition amount of the ethyl acetate is, the larger the granularity of the orange granules is;
(7) when the granularity of the orange granules reaches 1.00-0.85 mm (18-80 meshes), stopping adding the ethyl acetate, and distilling and removing the ethyl acetate to obtain a suspension system;
(8) when the particles are hard, the ethyl acetate is distilled, the suspension system is poured into absolute ethyl alcohol, then a standard sieve with the particle size of 1.00mm and 0.85mm is adopted for wet screening, and a screen object with the particle size of 1.00 mm-0.85 mm is reserved, so that the novel semi-finished product of the safety mixed ignition powder for the detonator is obtained;
(9) drying the ignition powder obtained by filtering by adopting water bath drying, wherein the water bath drying temperature is controlled at 60 ℃, and the water bath drying time is 4 hours, so as to obtain a novel safety mixed ignition powder for the detonator;
(10) the obtained explosive is detected according to the industrial electric detonator GB8031-2005, the requirement of the national standard No. 8 industrial electric detonator on a lead plate with the explosion penetration thickness of 5mm can be met, the perforation diameter is 12.6mm, and the technical requirement is met.
Example 3:
(1) putting a mixture of 4.5kg of trinitrophloroglucinol lead, 3.0kg of lead benzoate and 7.5kg of potassium perchlorate into 40.5kg of water to prepare a dispersion liquid;
(2) starting a water circulation heating system, and heating the dispersion liquid of the mixture of trinitrophloroglucinol lead, lead benzoate and potassium perchlorate to 50 ℃;
(3) adding 2.07Kg of potassium perchlorate solid into a dispersion of a mixture of trinitrophloroglucinol lead, lead phthalate and potassium perchlorate at 50 ℃, and fully stirring for 28 min;
(4) adding 0.380kg (solid content is 48%) of methyl methacrylate-isooctyl acrylate adhesive into the suspension to obtain a mixed solution system 1;
(5) adding a demulsifier of 5kg of anhydrous sodium sulfate (15 wt%) solution into the obtained mixed solution system 1 under the condition that the temperature is kept at 50 ℃, and obtaining a mixed solution system after the aqueous solution is clarified;
(6) opening a vacuum system, adding ethyl acetate into the obtained mixed solution system at a rate of 4mL/min for granulation under the conditions that the temperature is kept at 50 ℃ and the vacuum degree is 0.020MPa, and controlling the adding amount of the ethyl acetate by sampling and observing the granularity of orange granules, wherein the more the ethyl acetate is added, the larger the granularity of the orange granules is;
(7) when the granularity of the orange granules reaches 1.00-0.85 mm (18-80 meshes), stopping adding the ethyl acetate, and distilling and removing the ethyl acetate to obtain a suspension system;
(8) when the particles are hard, the ethyl acetate is distilled, the suspension system is poured into absolute ethyl alcohol, then a standard sieve with the particle size of 1.00mm and 0.85mm is adopted for wet screening, and a screen object with the particle size of 1.00 mm-0.85 mm is reserved, so that the novel semi-finished product of the safety mixed ignition powder for the detonator is obtained;
(9) drying the ignition powder obtained by filtering by adopting water bath drying, wherein the water bath drying temperature is controlled at 60 ℃, and the water bath drying time is 6 hours, so as to obtain a novel safety mixed ignition powder for the detonator;
(10) the obtained explosive is detected according to the industrial electric detonator GB8031-2005, the requirement of the national standard No. 8 industrial electric detonator on a lead plate with the explosion penetration thickness of 5mm can be met, the perforation diameter is 12.5mm, and the technical requirement is met.
Example 4:
(1) putting a mixture of 4.5kg of trinitrophloroglucinol lead, 3.0kg of lead benzoate and 7.5kg of potassium perchlorate into 42kg of water to prepare suspension;
(2) starting a water circulation heating system, and heating the suspension of the mixture of trinitrophloroglucinol lead, lead benzoate and potassium perchlorate to 50 ℃;
(3) adding 2.14Kg of potassium perchlorate solid into the suspension of the mixture of trinitrophloroglucinol lead, lead phthalate and potassium perchlorate at 50 ℃, and fully stirring for 25 min;
(4) adding 0.412kg (solid content is 48%) of methyl methacrylate-isooctyl acrylate adhesive into the suspension to obtain a mixed solution system 1;
(5) adding a demulsifier of 5.5kg of anhydrous sodium sulfate (15 wt%) solution into the obtained mixed solution system 1 under the condition that the temperature is kept at 50 ℃, and obtaining a mixed solution system 2 after the aqueous solution is clarified;
(6) opening a vacuum system, adding ethyl acetate into the obtained mixed solution system 2 at a rate of 4.5mL/min for granulation under the conditions that the temperature is kept at 50 ℃ and the vacuum degree is 0.015MPa, and controlling the addition amount of the ethyl acetate by sampling and observing the granularity of orange particles, wherein the more the addition amount of the ethyl acetate is, the larger the granularity of the orange particles is;
(7) when the granularity of the orange granules reaches 1.00-0.85 mm (18-80 meshes), stopping adding the ethyl acetate, and distilling and removing the ethyl acetate to obtain a suspension system;
(8) when the particles are hard, the ethyl acetate is distilled, the suspension system is poured into absolute ethyl alcohol, then a standard sieve with the particle size of 1.00mm and 0.85mm is adopted for wet screening, and a screen object with the particle size of 1.00 mm-0.85 mm is reserved, so that the novel semi-finished product of the safety mixed ignition powder for the detonator is obtained;
(9) drying the ignition powder obtained by filtering by adopting water bath drying, controlling the water bath drying temperature at 50 ℃ and the water bath drying time at 6h to obtain a novel safety mixed ignition powder for the detonator;
(10) the obtained explosive is detected according to the industrial electric detonator GB8031-2005, the requirement of the national standard No. 8 industrial electric detonator on a lead plate with the explosion penetration thickness of 5mm can be met, the perforation diameter is 12.2mm, and the technical requirement is met.
Example 5:
(1) putting a mixture of 4.5kg of trinitrophloroglucinol lead, 3.0kg of lead benzoate and 7.5kg of potassium perchlorate into 45kg of water to prepare a dispersion liquid;
(2) starting a water circulation heating system, and heating the dispersion liquid of the mixture of trinitrophloroglucinol lead, lead benzoate and potassium perchlorate to 50 ℃;
(3) adding 2.30Kg of potassium perchlorate solid into a dispersion of a mixture of trinitrophloroglucinol lead, lead phthalate and potassium perchlorate at 50 ℃, and fully stirring for 20 min;
(4) adding 0.471kg (solid content is 48%) of methyl methacrylate-isooctyl acrylate adhesive into the suspension to obtain a mixed solution system 1;
(5) adding a demulsifier of 6kg of anhydrous sodium sulfate (15 wt%) solution into the obtained mixed solution system 1 under the condition that the temperature is kept at 50 ℃, and obtaining a mixed solution system 2 after the aqueous solution is clarified;
(6) opening a vacuum system, adding ethyl acetate into the obtained mixed solution system 2 at a rate of 4mL/min for granulation under the conditions that the temperature is kept at 50 ℃ and the vacuum degree is 0.010MPa, and controlling the addition amount of the ethyl acetate by sampling and observing the granularity of orange granules, wherein the more the addition amount of the ethyl acetate is, the larger the granularity of the orange granules is;
(7) when the granularity of the orange granules reaches 1.00-0.85 mm (18-80 meshes), stopping adding the ethyl acetate, and distilling and removing the ethyl acetate to obtain a suspension system;
(8) when the particles are hard, the ethyl acetate is distilled, the suspension system is poured into absolute ethyl alcohol, then a standard sieve with the particle size of 1.00mm and 0.85mm is adopted for wet screening, and a screen object with the particle size of 1.00 mm-0.85 mm is reserved, so that the novel semi-finished product of the safety mixed ignition powder for the detonator is obtained;
(9) drying the ignition powder obtained by filtering by adopting water bath drying, wherein the water bath drying temperature is controlled at 50 ℃, and the water bath drying time is 4 hours, so as to obtain a novel safety mixed ignition powder for the detonator;
(10) the obtained explosive is detected according to the industrial electric detonator GB8031-2005, the requirement of the national standard No. 8 industrial electric detonator on a lead plate with the explosion penetration thickness of 5mm can be met, the perforation diameter is 12.0mm, and the technical requirement is met.
The test results of the safety mixed ignition powder for the detonator in the invention in the embodiment 5 of the invention according to GB8031-2005 Industrial electric detonator are shown in the table 1, and the table 1 is the comparison result of the sensitivity performance of the explosive obtained in the embodiment 5 of the invention and the sensitivity performance of the common ignition powder. As can be seen from table 1, the "safe mixed ignition powder" for the detonator provided in embodiment 5 of the present invention has a greatly reduced sensitivity compared to the conventional ignition powder, and the safety performance is greatly improved. The binder in the embodiment 5 is added in the largest amount, and the degradation performance is the largest, namely the performance tested in the embodiment 5 can meet the requirement of initiation, and other embodiments have no problem.
Table 1 results of sensitivity performance test of the ignition powder obtained in examples 1 to 5 of the present invention and the conventional ignition powder
From the above embodiments, the safety mixed ignition powder for detonators or the safety mixed ignition powder for detonators prepared by the preparation method provided by the invention has the characteristics of reliable action, safe use, small static electricity, good free-running property and uniform particle size, is beneficial to mechanical charging of the booster for detonators, and is completely exploded by assembling No. 8 industrial electric detonators and performing a 5mm lead plate perforation test
All are qualified, and the produced detonator meets the national standard requirement.
Ultimate ignition charge test an 8# industrial electric detonator was assembled under the same assembly conditions as those tested in table 1, and an ultimate ignition charge test of the safety mixed ignition charge for detonators and DDNP of example 5 of the present invention was carried out, with the test results as in table 2. As can be seen from Table 2, the limit ignition charge of the DDNP is 0.20g which is better than that of the DDNP under the same assembly condition, while the limit ignition charge of the DDNP is 0.15g which can meet the requirement of detonation.
TABLE 2 Limit dose test
| Ignition powder | Minimum charge g | Test conditions |
| Example 5 | 0.15 | 40 full explosion |
| DDNP | 0.20 | 40 full explosion |
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (10)
1. A safety mixed ignition powder for a detonator is characterized by comprising the following components in percentage by weight: 29.5-29.7 wt% of trinitrophloroglucinol lead, 19.7-19.8 wt% of lead benzoate, 49.3-49.5 wt% of potassium perchlorate and 1.0-1.5 wt% of a methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer.
2. The safety mixed ignition powder for detonators according to claim 1, wherein the mass ratio of trinitrophloroglucinol lead, lead benzoate and potassium perchlorate is 3:2: 5.
3. The safety mixed ignition powder for the detonator according to claim 1, wherein the mass ratio of trinitrophloroglucinol lead, lead benzoate, potassium perchlorate and the quaternary copolymer of methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate is 4.5:3:7.5: 0.316-0.471.
4. A method for preparing a safe mixed ignition powder for detonators according to any one of claims 1 to 3, which comprises the steps of:
mixing trinitrophloroglucinol lead, lead benzoate, potassium perchlorate and water to obtain dispersion liquid;
preheating the dispersion to obtain a preheated dispersion;
adding potassium perchlorate into the preheated dispersion liquid to obtain suspension;
mixing the suspension with a methyl methacrylate-methacrylic acid-acrylic acid-butyl acrylate quadripolymer to obtain a mixed solution;
mixing the mixed solution with a demulsifier to perform demulsification to obtain a demulsified solution;
dripping an organic solvent into the demulsified solution, granulating and drying to obtain granules;
and passivating the granules to obtain the safety mixed ignition powder for the detonator.
5. The preparation method according to claim 4, wherein the mass ratio of the total mass of the trinitrophloroglucinol lead, the lead benzoate and the potassium perchlorate to water is 1: (2.5-3).
6. The method of claim 4, wherein the temperature of the preheating is 50 ± 2 ℃.
7. The preparation method according to claim 4 or 5, characterized in that the total mass of the trinitrophloroglucinol lead, the lead benzoate and the potassium perchlorate is 15kg, and the water-material ratio is (2.5-3): 1, calculating, wherein the mass of the supplementary potassium perchlorate is 1.91-2.30 kg.
8. The method according to claim 4, wherein the pellet has a particle size of 0.85 to 1 mm.
9. The method according to claim 4, wherein the passivation comprises distillation, organic solvent washing, filtration and drying in this order.
10. Use of the safe mixed-ignition powder for detonators according to any one of claims 1 to 3 in the preparation of detonators.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115594555A (en) * | 2022-09-23 | 2023-01-13 | 西安庆华民用爆破器材股份有限公司（Cn） | Environment-friendly high-temperature-resistant ignition agent |
| CN115819160A (en) * | 2022-11-25 | 2023-03-21 | 山西北化关铝化工有限公司 | Explosive for detonator assembly and preparation method thereof |
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