CN103172478A - Preparation method of ZPP (Zinc Protoporphyrin) insensitive ignition explosive - Google Patents

Abstract

The invention discloses a preparation method of a ZPP (Zinc Protoporphyrin) insensitive ignition explosive, and belongs to the preparation field of initiating explosive medicaments. The preparation method comprises the following steps of: refining zirconium powder and potassium perchlorate; enabling the average particle diameter of the zirconium powder and the potassium perchlorate to be respectively less than 3mu m and 20mu m; evenly mixing the zirconium powder and the potassium perchlorate manually or mechanically; mixing the zirconium powder and the potassium perchlorate with a prepared nitrocotton acetone solution; volatilizing the acetone in a stirring manner; and collecting semi-dry medicament particles of 18 to 60 meshes and drying, thereby obtaining the ZPP insensitive ignition explosive as a finished product in the shape of a gray solid granule. The prepared ZPP insensitive ignition explosive is accurate in medicament content, can be stored for a long time and used at any time, and is suitable for the pressing charging of the medicaments in various shapes and density changes.

Description

The preparation method of ZPP insensitiveness priming charge

Technical field

The invention belongs to priming system medicament preparation field, relate generally to a kind of insensitiveness priming charge preparation method, relate in particular to a kind of insensitiveness priming charge preparation method who can be used for the insensitiveness electrical igniter.

Background technology

ZPP insensitiveness priming charge (Zirconium potassium-perchlorate is called for short ZPP) is comprised of zirconium powder, potassium perchlorate and tackiness agent, is a kind of priming charge of insensitiveness.The insensitiveness priming charge refers to sample in electric spark workpiece, and applying minimum current 1A corresponding power is the direct current of 1W, and conduction time, minimum 5min, misfired, and reliably gets angry when the Firing test of regulation.ZPP insensitiveness priming charge meets the requirement of 1A1W5min fully, is mainly used in lighting a fire or the ignition control of explosive train, is widely used in the seed element in military and civilian field.ZPP insensitiveness priming charge is to static, radio frequency, thunder and lightning insensitiveness, available heat bridge silk or laser ignition, thereby it is high to have reliability, and long storage performance is good, and heat output is high, the characteristic that combustion time is short.

European patent EP 1803698 has been reported formula of ZPP insensitiveness priming charge and preparation method thereof and loading method.In this patent, ZPP insensitiveness priming charge consists of zirconium, potassium perchlorate, nitro-cotton and solvent acetic acid isopentyl ester, nitro-cotton content is 0.1%～0.5% of zirconium powder and potassium perchlorate gross weight, Isoamyl Acetate FCC content is 12.5%～14.0% of zirconium powder and potassium perchlorate gross weight, zirconium powder and potassium perchlorate two component concentrations are respectively zirconium powder 50%～70%,potassium perchlorate 30%～50%.The preparation method is that tackiness agent is dissolved in solvent, mixes with reductive agent, oxygenant respectively, forms a kind of liquid of viscosity, use during use in syringe decanting point firearm cavity volume, 60 ℃ of dryings of whole lighter for ignition, the volatilization of solvent acetic acid isopentyl ester forms ZPP insensitiveness priming charge solid chemicals.The advantage of this method is to eliminate accumulation of static electricity, and shortcoming is now to do existing use, can not prolonged preservation, and also the method for injection powder charge is not suitable with the press loading technology of various variable density.This patent does not relate to raw-material specification and state yet.

Summary of the invention

The technical problem that will solve of the present invention is that the deficiency for existing in existing ZPP insensitiveness priming charge preparation and use provides a kind of ZPP insensitiveness priming charge preparation method.

For solving the problems of the technologies described above, ZPP insensitiveness priming charge preparation method provided by the invention comprises following processing step:

The first step is used the ball mill grinding zirconium powder, and its concrete technology parameter and operation are:

1.1 500g ball milling pearl, 30g zirconium powder and 70ml deionized water are poured in the ball grinder of ball mill, the ball milling pearl is the zirconium white ball of φ 2mm, the rotating speed of ball mill is set to 250r/min, each milling time is set to 30min, grind altogether 10 times, the interval heat radiation time of adjacent twice grinding is 15min;

1.2 the mixture in ball grinder is poured in thing standard 40 mesh sieves, is separated with the ball milling pearl will be with the water zirconium powder;

1.3 discharge port and the filter flask of funnel are tightly connected, put into two Medium speed filter papers in the bottom of funnel and will be with the water zirconium powder to pour funnel into, open the vacuum-pump power supply that is connected with filter flask the material in funnel is carried out suction filtration, until the discharge port of funnel no longer leaks, half wet zirconium powder in funnel is put on the plate that is covered with template, shakeouts with glass stick partly wet zirconium powder and thickness and be no more than 1cm;

1.4 give insulation after water-bath baking oven for heating to 60 ℃, the plate that is covered with half wet zirconium powder is put into the water-bath baking oven and dry 4h at the temperature of 60 ℃ ± 2 ℃, after the 20min that at room temperature dries in the air, bottling is stand-by;

Second step grinds potassium perchlorate with mixing machine, and its concrete technology parameter and operation are:

2.1 the mill ball of 500g, the ethanolic soln of 500ml and the pure potassium perchlorate of 500g are joined respectively in the mixed medicinal cupping of mixing machine, mill ball is agate ball or Stainless Steel Ball or wooden shot, the rotating speed of mixing machine is set to 36r/min, milling time is 6h, then will mix mixture in pencil and pour in the plate that is covered with template and to shakeout 1cm thick;

2.2 give insulation after water-bath baking oven for heating to 60 ℃, the plate that fills mixture is put into the water-bath baking oven and dry 12h at the temperature of 60 ℃ ± 2 ℃, then naturally cooling at room temperature;

2.3 cooled mixture is poured in 18 mesh standard sieves, potassium perchlorate is separated with mill ball, then potassium perchlorate is poured in 200 mesh standard sieves, collect in vial the potassium perchlorate under 200 mesh sieves stand-by;

In the 3rd step, weigh zirconium powder after grinding and potassium perchlorate with electronic balance according to ratio requirement and with both abundant mixings;

In the 4th step, weigh nitro-cotton with electronic balance according to ratio requirement, and be poured in flask, add the pure acetone solvent in flask according to ratio requirement, cover grinding port plug to flask after jiggling flask, more than standing 24h, form the nitro-cotton acetone liquid of transparent glue;

The 5th step, described powdery ZPP insensitiveness priming charge is carried out granulation, namely the ZPP insensitiveness igniting medicinal powder that is mixed and nitro-cotton acetone liquid mixing and stirring, after the acetone volatilization forms leather hard ZPP insensitiveness priming charge, sieve with 20 eye mesh screens, the 10min that dries in the air after medicament shakeouts of sieving crosses 18 orders and 60 mesh sieves more successively, to collect the pharmacy particle between 18 orders～60 orders;

The 6th step, the pharmacy particle of collecting is put into shakeout at porcelain dish and thickness less than 1cm, give insulation after water-bath baking oven for heating to 60 ℃, porcelain dish is put into the water-bath baking oven and dry 12h at the temperature of 60 ℃ ± 2 ℃, then take out the porcelain dish that fills pharmacy particle from the water-bath baking oven, at room temperature after naturally cooling 20min, particulate state ZPP insensitiveness priming charge is packed.

Beneficial effect of the present invention is embodied in the following aspects.

(1) due in ZPP insensitiveness priming charge, have a significant impact as the globule size of the reductive agent zirconium powder combustionproperty to priming charge, granularity is thinner, contact area between solid particulate is larger, reacts faster, and combustion accuracy is also just higher, for this reason, the present invention refine to mean particle size less than 3 μ m by mechanical milling tech with thick zirconium powder, thereby, provide technical support to the inner quality that improves ZPP insensitiveness ignition powder.

(2) the present invention is for making potassium perchlorate section by standard 200 mesh sieves, adopted the three-dimensional gravity mixing machine to carry out refinement to potassium perchlorate, this process for refining can carry out the batch refinement to potassium perchlorate, thereby the ZPP medicament that can make different batches adopts the potassium perchlorate with batch refinement, thereby has improved the consistence of ZPP insensitiveness priming charge burning.

(3) the present invention is carrying out medicament when mixing to refinement zirconium powder and potassium perchlorate, medicament for different stage weight provides three kinds of mixed processes, be a kind of manual mixing method and two kinds of mechanical mixings, the manual mixing method is adapted to low dose and easily and fast; It is the purpose of medicament mixing that the middle dosage of hectogram level adopts mixing machine and the long time running by mixing machine to reach, and the mode that the heavy dose of feather weight adopts mixing machine to add agate ball and roll and rub by increase reaches the purpose that a large amount of medicaments are mixed.Thereby the present invention can adapt to the mixing of various pharmaceutical quantities.

(4) the present invention mixes the ZPP medicinal powder that mixes and makes acetone volatilization by stirring with the nitro-cotton acetone soln of configuration, collect under the leather hard of ZPP between 18 orders～60 orders pharmacy particle and with these particles as final ZPP finished product.This granular medicament is compared with existing liquid preparation, and its advantage is in long-term storage or transhipment, can not destroy the homogeneity of two kinds of compositions; Can use at any time, be easy to claim the medicine operation, and adapt to the press loading of different shape and variable density.

Description of drawings

Fig. 1 is the testing graininess distribution plan of refinement zirconium powder.

Fig. 2 is the DSC curve of ZPP insensitiveness priming charge.

Embodiment

The invention will be further described below in conjunction with accompanying drawing and preferred embodiment:

The first step is carried out mechanical mill to zirconium (Zr) powder, and its concrete technology parameter and operation are:

1.1 adopt Japanese planetary ball mill PL-1200 type, this owner will be comprised of mechanical part and control section.Mechanical part has ball grinder (φ 130 * 80mm) and the fastening piece composition of three symmetrical rotations mainly by the rotating disk of diameter 60cm on rotating disk.Ball grinder is the UFO-like tank body of capacity 500ml, is divided into cavity volume part and sealing cover, and the ball milling pearl is the zirconium white ball of φ 2mm.500g ball milling pearl, 30g zirconium powder and 70ml deionized water are poured in the ball grinder of ball mill, and the batching of three ball grinders is identical, loads onto round rubber sealed strip and the sealing cover that closes at the cavity volume face of ball grinder, with spanner with screw tightening.Three ball grinders are put into the ball mill fixed position, install fastening piece by operational requirement, buckle well outer protective cover.Connect the 308v power supply, open the ball mill power switch, the rotating speed of ball mill is set to 250r/min, and each milling time is set to 30min, grinds altogether 10 times, and the interval heat radiation time of adjacent twice grinding is 15min.

1.2 after ball milling is completed, unload the goods from the airplane by the installation reverse order, open after waiting the ball grinder naturally cooling, content is poured in the 500ml glass cylinder, with the 50ml deionized water, ball grinder is rinsed well.Mixture in glass cylinder is poured in the sieve at the 40 Stainless Steel Bands sieves ends, and is rinsed glass cylinder with 20ml water, with rock gently sieve and with the zirconium pearl in the wash bottle flushing sieve of dress 50ml water until wash clean, thereby will be with the water zirconium powder to separate with the ball milling pearl.

1.3 the discharge port of Bush's funnel of φ 9cm and the filter flask of 1L are tightly connected, middle sealing-ring sealing with φ 4.Put into two in the bottom surface of funnel with the water-moistened φ 9cm of 5ml Medium speed filter paper, flatten with the wet filter paper of handgrip, couple together with the hose of φ 6 suction filtration mouth and SHZ-D (III) the circulating water type vacuum pump with filter flask.And will be with the water zirconium powder to pour in funnel, open vacuum-pump power supply the material in funnel is carried out suction filtration, until the discharge port of funnel no longer leaks.Close vacuum-pump power supply, funnel is unloaded down from filter flask, press from both sides out partly wet zirconium powder with tweezers, half wet zirconium powder is put on the Stainless Steel Disc or porcelain dish that is covered with template, shakeout with glass stick partly wet zirconium powder and thickness and be no more than 1cm;

1.4 with five rings, the Chongqing WGP120 of test apparatus company limited type water-bath baking oven for heating to 60 ℃, open the plate that oven door will be covered with half wet zirconium powder and put into the water-bath baking oven, dry 4h after closing oven door at the temperature of 60 ℃ ± 2 ℃, pour in the cone-shaped glass bottle of 100ml after at room temperature the refinement zirconium powder of drying being dried in theair 20 minutes, cover ground glass stopper, labelled, record the medicament lot number, time, weight.

Fig. 1 has provided and has adopted the Ma Erwen laser particle analyzer to the test result of refinement zirconium powder sample granularity, and result shows that the median size of refinement zirconium powder is 1.91 μ m.According to GJB3425-1998 blasting agent and thermobattery zirconium powder standard, the zirconium activity of measuring the refinement zirconium powder is 90.74%.

Second step grinds potassium perchlorate (KClO with mixing machine₄), its concrete technology parameter and operation are:

2.1 mixing machine is selected SH-2600 three-dimensional gravity mixing machine, the stainless steel cylindrical tank that its mixed medicinal cupping is φ 13 * 19cm, mill ball are agate ball or Stainless Steel Ball or the wooden shot of all size, adopt φ 6mm agate ball in this example.The ethanolic soln of 500g agate ball ball, 500ml and the pure potassium perchlorate of 500g are joined respectively in the mixed medicinal cupping of mixing machine, shake gently mixed medicinal cupping and make the potassium perchlorate complete wetting, cover and to mix medicinal cupping after circular spill lid and transfer in the fixed card slot of mixing machine, install fixed support and tight a bolt, making mixed medicinal cupping fix and seal.Open the power switch of mixing machine controller, the rotating speed of mixing machine is set to 36r/min, and milling time is 6h, after mixing machine shuts down, cuts off the electricity supply and unloads mixed medicinal cupping.Pour into the mixture in mixed pencil in the plate that is covered with the A3 template and to shakeout 1cm thick, clean grinding pot with 20ml ethanol.

2.2 with five rings, the Chongqing WGP120 of test apparatus company limited type water-bath baking oven for heating to 60 ℃, open oven door the plate that the potassium perchlorate mixture will be housed is put into the water-bath baking oven, dry 12h after closing upper chamber door at the temperature of 60 ℃ ± 2 ℃, take out plate from baking oven, then naturally cooling mixture at room temperature.

Add in 18 mesh standard sieves that sieve the end 2.3 cooled mixture is poured into down, shake gently sieve potassium perchlorate is sieved fully, the agate ball in sieve is put into the glass beaker of 500ml, rinse well with tap water, naturally dry; Potassium perchlorate under sieve is poured in 200 mesh standard sieves again, gently scraped with bamboo clappers, the potassium perchlorate under 200 mesh sieves is collected in the vial of 500ml, cover ground glass stopper, labelled, record the medicament lot number, the time, weight, and at room temperature preserve.

In the 3rd step, weigh zirconium powder after grinding and potassium perchlorate with electronic balance according to ratio requirement and with both abundant mixings.If choose positive oxygen balance formula, i.e. 2Zr+KClO₄→ KCl+2ZrO₂, obtaining two constituent mass per-cents under zero oxygen balance is Zr: KClO₄=56.8: 43.2.For ZPP insensitiveness electricity gunpowder can fully be burnt, oxygen level must be sufficient, and for this reason, this preferred embodiment heightens 1.5% with the content of potassium perchlorate, and namely the formula of choosing of zirconium powder and potassium perchlorate is: Zr: KClO₄=55.3: 44.7.

If the total mass of zirconium powder and potassium perchlorate is during less than 20g, adopt the manual mixing method that it is mixed, if the total mass of zirconium powder and potassium perchlorate is in 20g～1000g scope, adopt the first mechanical mixing that it is mixed, if the total mass of zirconium powder and potassium perchlorate greater than 1000g, adopts the second mechanical mixing that it is mixed:

3.1 the operation of manual mixing method is:

With Zr powder and KClO₄Be poured on an A4 template, mention paper on one side, make medicament along with paper rolls, palikinesia from different directions, used time 33min estimates more evenly, and this is preliminary mixing.Pour on 200 mesh sieve the band sieve end after tentatively mixing into, with the band offace 5 * 5cm, the wood shovel is gently scraped, make medicament sieve fully, sieve end medicament is rolled over to mix to the A4 paper again pour into again on 200 mesh sieves, so operate 5 times, form even Dark grey medicinal powder.

3.2 the operation of the first mechanical mixing is:

With Zr powder and KClO₄Be poured in the cylindrical stainless steel cask ofφ 5 * 15cm, surrounding also seals with the bolted of φ 6mm, then drum is placed on three rod ball mills, plug in, the rotating speed of three rod ball mills is arranged on 16r/min, and mixing time is 16h, forms even Dark grey medicinal powder.

3.3 the operation of the second mechanical mixing is:

Just Zr powder and KClO₄Be poured in the cylindrical stainless steel cask of φ 13 * 25cm, then add the agate ball 500g of φ 6, surrounding bolted and the sealing of φ 6mm, again drum is placed on three rod ball mills, plug in, the rotating speed of three rod ball mills is arranged on 16r/min, and mixing time is 16h; By sieving, agate ball is separated after mixing, screen underflow is even Dark grey medicinal powder.

In the 4th step, weigh nitro-cotton with electronic balance according to ratio requirement and be poured in the triangle ground flask of 500ml.In this example, the content of nitro-cotton is 4% of zirconium powder and potassium perchlorate total mass, and the complete formula of ZPP insensitiveness electricity gunpowder is: Zr: KClO₄: nitro-cotton=53.17: 42.98: 3.85.The ratio of then joining 26ml pure acetone solvent in the 1g nitro-cotton joins the pure acetone solvent in flask, covers grinding port plug to flask after jiggling flask, more than standing 24h, forms the nitro-cotton acetone liquid of transparent glue.

5.1 manual granulation

The 100gZPP insensitiveness igniting medicinal powder that is mixed is poured in the 250ml glass cylinder, added 100ml nitro-cotton acetone liquid, fully stir with φ 6mm * 40cm glass stick, acetone volatilizees along with whipping process, until become leather hard ZPP insensitiveness priming charge.Because of acetone volatile, easy firing, pungent is therefore acetone volatilization operation will be carried out in stink cupboard.Leather hard ZPP insensitiveness priming charge is poured onband sieve 20 eye mesh screens at the end, a little firmly medicament was scraped screen cloth with the wood shovel, sieve at the end medicament spread out, dried in theair 10 minutes, pour into 18 orders, middle 60 orders, beneath be to sieve in the sieve at the end, jog sieves.Collect the particle between 18～60 orders.To and collect less than 60 purpose pharmacy particles greater than 18 orders, then add a small amount of acetone, stir, repeat the granulation of sieving, collect the pharmacy particle between 18 orders～60 orders.

5.2 mechanical pelleting

To pour in kneader over the ZPP insensitiveness igniting medicinal powder that 200g is mixed, and add needed nitro-cotton acetone soln, plug plugs in; press power knob; electric machine rotation until shut down after forming leather hard ZPP insensitiveness priming charge, is put into leather hard ZPP insensitiveness priming charge on swing tablets press 20 eye mesh screens; switch on power; press power knob, the teflon rod of φ 10cm is vacillated now to the left, now to the right and is rolled, and medicament all passes through; after drying in theair 20 minutes, collect the pharmacy particle between 18～60 orders.

the 6th step, the pharmacy particle of collecting is put into shakeout at porcelain dish and thickness less than 1cm, with after five rings, the Chongqing WGP120 of test apparatus company limited type water-bath baking oven for heating to 60 ℃, open oven door, the porcelain dish that is placed with ZPP insensitiveness priming charge is moved in the water-bath baking oven, dry 12h after closing oven door at the temperature of 60 ℃, then take out the porcelain dish that fills pharmacy particle from the water-bath baking oven, at room temperature after naturally cooling 20min, the ZPP insensitiveness priming charge of drying by the weighing of weighing step in the weighing room, and the papery medicine box of 14 * 9 * 7cm that packs into, the box face indicates lot identification mark, quality, date etc.Afterwards, ZPP insensitiveness priming charge is left in moisture eliminator.

The ZPP insensitiveness priming charge that adopts the preparation of preferred embodiment of the present invention technique has been carried out following test:

1.DSC thermal analysis, analytical results show, its exothermic peak is at 508.15 ℃ (referring to Fig. 2).

2. press quick-fried heat and gas specific volume that GJB5891.29-2006, GJB5891.30-2006 measure ZPP insensitiveness priming charge, result is:, its quick-fried calorific value is: 6063J/g; The gas specific volume value is: 51.1mL/g.

3. measure the impact sensitivity of ZPP insensitiveness priming charge according to GJB5891.22-2006, test conditions is: 2000g drops hammer, the 20mg dose is pressed in igniter cap, tests several 30.Test-results is: 50% igniting sensitivity: 32.9cm, standard deviation: 2.7cm.

4. measure the friction sensitivity of ZPP insensitiveness priming charge according to GJB5891.24-2006, test conditions is: 80 ° of gauge pressure 3.43MPa of pendulum pivot angle, dose 20mg, test several 50.Test-results is: average sparking rate: 24%.

5. measure the flame sensitivity of ZPP insensitiveness priming charge according to GJB5891.25-2006, test conditions is: dose 20mg, test several 50.Test-results: 50% igniting sensitivity: 23.9cm, standard deviation: 2.1cm.

6. measure the electrostatic sensitivity of ZPP insensitiveness priming charge according to GJB5891.27-2006, test conditions is: electrode gap: 1.0mm; Electric capacity: 0.033 μ f; Resistance: 100K Ω; Dose: 25mg.Test-results is: positive pole: 50% ignition voltage: 1.69KV, 50% firing energy: 0.047J; Negative pole: 50% ignition voltage: 1.71KV, 50% firing energy: 0.048J.

Claims (3)

1. the preparation method of a ZPP insensitiveness priming charge, is characterized in that, the method comprises following processing step:

The first step is used the ball mill grinding zirconium powder, and its concrete technology parameter and operation are:

1.1 500g ball milling pearl, 30g zirconium powder and 70ml deionized water are poured in the ball grinder of ball mill, the ball milling pearl is the zirconium white ball of φ 2mm, the rotating speed of ball mill is set to 250r/min, each milling time is set to 30min, grind altogether 10 times, the interval heat radiation time of adjacent twice grinding is 15min;

1.2 the mixture in ball grinder is poured in thing standard 40 mesh sieves, is separated with the ball milling pearl will be with the water zirconium powder;

1.3 discharge port and the filter flask of funnel are tightly connected, put into two Medium speed filter papers in the bottom of funnel and will be with the water zirconium powder to pour funnel into, open the vacuum-pump power supply that is connected with filter flask the material in funnel is carried out suction filtration, until the discharge port of funnel no longer leaks, half wet zirconium powder in funnel is put on the plate that is covered with template, shakeouts with glass stick partly wet zirconium powder and thickness and be no more than 1cm;

1.4 give insulation after water-bath baking oven for heating to 60 ℃, the plate that is covered with half wet zirconium powder is put into the water-bath baking oven and dry 4h at the temperature of 60 ℃ ± 2 ℃, after the 20min that at room temperature dries in the air, bottling is stand-by;

Second step grinds potassium perchlorate with mixing machine, and its concrete technology parameter and operation are:

2.1 the mill ball of 500g, the ethanolic soln of 500ml and the pure potassium perchlorate of 500g are joined respectively in the mixed medicinal cupping of mixing machine, mill ball is agate ball or Stainless Steel Ball or wooden shot, the rotating speed of mixing machine is set to 36r/min, milling time is 6h, then will mix mixture in pencil and pour in the plate that is covered with template and to shakeout 1cm thick;

2.2 give insulation after water-bath baking oven for heating to 60 ℃, the plate that fills mixture is put into the water-bath baking oven and dry 12h at the temperature of 60 ℃ ± 2 ℃, then naturally cooling at room temperature;

2.3 cooled mixture is poured in 18 mesh standard sieves, potassium perchlorate is separated with mill ball, then potassium perchlorate is poured in 200 mesh standard sieves, collect in vial the potassium perchlorate under 200 mesh sieves stand-by;

In the 3rd step, weigh zirconium powder after grinding and potassium perchlorate with electronic balance according to ratio requirement and with both abundant mixings;

In the 4th step, weigh nitro-cotton with electronic balance according to ratio requirement, and be poured in flask, add the pure acetone solvent in flask according to ratio requirement, cover grinding port plug to flask after jiggling flask, more than standing 24h, form the nitro-cotton acetone liquid of transparent glue;

The 5th step, described powdery ZPP insensitiveness priming charge is carried out granulation, namely the ZPP insensitiveness igniting medicinal powder that is mixed and nitro-cotton acetone liquid mixing and stirring, after the acetone volatilization forms leather hard ZPP insensitiveness priming charge, sieve with 20 eye mesh screens, the 10min that dries in the air after medicament shakeouts of sieving crosses 18 orders and 60 mesh sieves more successively, to collect the pharmacy particle between 18 orders～60 orders;

The 6th step, the pharmacy particle of collecting is put into shakeout at porcelain dish and thickness less than 1cm, give insulation after water-bath baking oven for heating to 60 ℃, porcelain dish is put into the water-bath baking oven and dry 12h at the temperature of 60 ℃ ± 2 ℃, then take out the porcelain dish that fills pharmacy particle from the water-bath baking oven, at room temperature after naturally cooling 20min, particulate state ZPP insensitiveness priming charge is packed.

2. the preparation method of ZPP insensitiveness priming charge according to claim 1, it is characterized in that, when the zirconium powder after described grinding and potassium perchlorate are mixed, the device proportioning is: zirconium powder: potassium perchlorate=55.3: 44.7, when the described nitro-cotton acetone liquid of configuration, the content of described nitro-cotton is 4% of zirconium powder and potassium perchlorate total mass, and the 1g nitro-cotton need to be joined the pure acetone solvent of 26ml.

3. the preparation method of ZPP insensitiveness priming charge according to claim 1, it is characterized in that, when the zirconium powder after described grinding and potassium perchlorate are mixed, if both total masses during less than 20g, adopt the manual mixing method, if both total masses are in 20g～1000g scope, adopt the first mechanical mixing, if both total masses greater than 1000g, adopt the second mechanical mixing

The operation of described manual mixing method is: zirconium powder and potassium perchlorate are poured on a template, mentioning from different directions paper makes medicament along with paper rolls on one side, used time amounts to 3min, again confection is poured on 200 mesh sieve, gently scrape with wood shovel and make confection sieve fully, form even Dark grey medicinal powder;

The operation of described the first mechanical mixing is: zirconium powder and potassium perchlorate are poured in the charging basket of three rod ball mills, and the rotating speed of three rod ball mills is arranged on 16r/min, and mixing time is 16h, forms even Dark grey medicinal powder;

The operation of described the second mechanical mixing is: zirconium powder, potassium perchlorate and agate ball are poured in the charging basket of three rod ball mills, the rotating speed of three rod ball mills is arranged on 16r/min, mixing time is 16h, by sieving, agate ball is separated, and screen underflow is even Dark grey medicinal powder.

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