CN103506194B - The preparation facilities of a kind of ultra-fine CL-20 and preparation method - Google Patents
The preparation facilities of a kind of ultra-fine CL-20 and preparation method Download PDFInfo
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- CN103506194B CN103506194B CN201210523625.7A CN201210523625A CN103506194B CN 103506194 B CN103506194 B CN 103506194B CN 201210523625 A CN201210523625 A CN 201210523625A CN 103506194 B CN103506194 B CN 103506194B
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Abstract
The present invention provides a kind of ultra-fine CL-20 preparation facilities and preparation method.Including grinder main frame, blender and product pump.Main ball mill includes grinding chamber, the mill ball that band stirs；Mill ball is placed in grinding chamber.Stirring it is provided with in blender, discharging opening and recycle feed mouth it is provided with on blender, blender discharging opening is connected with the feeding hole pipeline of main ball mill, grinding chamber discharging opening is connected with the recycle feed mouth pipeline of blender, on this pipeline, the position near grinding chamber is provided with outlet valve, is provided with product pump afterwards.Take mill ball and join in described main ball mill grinding chamber, be input to the mixed slurry of raw material CL-20 and lapping liquid in above-mentioned grinding chamber afterwards be circulated attrition grinding, discharge afterwards and be dried through vacuum filtration, obtain described ultra-fine CL-20.This preparation facilities and method are simple to operate, and safety is high, and production efficiency is high, can be widely applied to the refinement of various energetic material.
Description
Technical field
The present invention relates to the refinement technology of a kind of energetic material, say further, relate to a kind of rapid batch
The device and method preparing ultra-fine CL-20.
Background technology
Development and fierceness, the refinement technology Fang Xing of domestic and international explosive day by day of weapon countermine along with science and technology
Do not end.Because ultra-fine explosive have several advantages that detonation course close to ideal detonation rule, blast
Potential interior can develop；Good heat conductivity, easily carries out conduction of heat, makes blast focus be difficult to be emerged；
Being prone to carry out grain composition with big particle diameter explosive, dispersive property is good, promotes degree of packing more preferably and evenly；
During the load that is hit, impulsive force quickly evenly spreads in whole powder column, reduces impact sensitivity.Therefore, super
Thin explosive will play an important role in actual applications.
CL-20 (hexanitro azepine different 5 hereby alkane) is a kind of high energy density compound, and density compares HMX
(HMX) high by 8%, explosion velocity is high by 6%, and energy density is high by more than 15%.Cl-20 be so far energy density and
The simple substance ammonal that explosion velocity is the highest, has good application prospect in following weaponry.Ultra-fine CL-20,
Especially submicron order, nanoscale CL-20, except the superiority retaining plain particles CL-20 high-energy-density
Outside energy, also having shock sensitivity and impact sensitivity is lower, safer characteristic, this is to widening CL-20's
Range of application, improve armament systems performance significant.
At present, ultra-fine CL-20 preparation method mainly has solvent-nonsolvent recrystallization method, shooting flow body weight to tie
Crystallization, micro emulsion method, high-speed jet comminuting method etc., but it is respectively arranged with its pluses and minuses.
Solvent-nonsolvent recrystallization method chemical solvent dissolves CL-20 makes saturated solution, then with non-molten
The dilution dispersion of agent inert fluid, makes explosive be recrystallized with granule crystal state.The ultra-fine CL-20 of preparation,
Granularity is typically in micron or submicron order.Its shortcoming is that cost is high, yields poorly, and the production cycle is long；It is difficult to
Make explosive particle diameter ultra-fine to submicron, nano-scale；High to solvent requirement, spent organic solvent discharge capacity big and
It is not easily recycled.The spent organic solvent amount that every ultra-fine CL-20 of hectogram needs discharge is more than 1000 grams, product
Granularity requirements is the thinnest, and the organic waste liquid measure of discharge is the biggest.
Micro emulsion method is to use special surfactant to improve CL-20 surface character, continuous ultra-fine emulsifying,
Superelevation segmentation in molecular scale magnitude, makes under certain temperature gradient conditions and under certain process conditions
It becomes the even powder body CL-20 that flowing physical property is good.Its shortcoming is that post processing is more complicated, state so far
Inside and outside the most successfully this post processing work report.
High-speed jet comminuting method, is to utilize percussion flow to produce when the narrowest pipeline high speed flows collision in opposite directions
Thump, extruding, shearing force, strong turbulence effect and strong high pressure acoustic wave action so that additional load mechanical power
Can more fully hereinafter be converted into granule to pulverize and scattered strength, thus reach the mesh of CL-20 granular superfine
's.Its shortcoming is owing to solvent forms atomized drop by mutually clashing into, and this is accomplished by doing liquid the biggest
Merit；Liquid flow at high speed in the duct needs the biggest pressure, and this is to conditions such as device sealing and resistance to pressures
Require the highest.
Also have and use hand grinding method to obtain the CL-20 that granularity is tiny at laboratory.Such as May L Chan (May
L Chan.New Ingredients for non-polluting propellants [J], CA93555-6001 USA) will
HNIW is dispersed in equipped with grinding 14～16 in the abrading glass vessel of distilled water and alcohol mixeding liquid body little
Time, obtain granularity HNIW about 3 μm.But this method exist milling time length, yield poorly,
The problems such as the danger that particle size distribution is uneven, waste liquid amount is big and hand lapping exists.
In a word, said method also exists complex process in various degree, and cost is high, yields poorly, and efficiency is low, grain
Spend bad control and wider distribution, the shortcomings such as effect is not ideal enough, limit it and give birth on a large scale in weapon
Produce and application.
Summary of the invention:
In order to solve to prepare the complex process that ultra-fine CL-20 exists in prior art, cost is high, yields poorly,
Polluting the problems such as heavy, the bad control of granularity, the present invention designs a set of device including ball mill, can be to CL-20
Realizing quickly Deng dangerous materials material, pulverize with pollution-free ultrafine in batches, the granularity of product can be according to milling time
Realize with the proportioning of mill ball.Thered is provided out a kind of to be made by mechanical lapping rapid batch and environmental protection simultaneously
The method of standby CL-20.
An object of the present invention is to provide a kind of device preparing ultra-fine CL-20.
The preparation facilities of a kind of ultra-fine CL-20 of the present invention, including main ball mill, also includes and ball milling
Machine host be connected blender and product pump.
It is susceptible to owing to CL-20 belongs to the high Energy Density Materials of high mechanical sensitivity, mechanical shock and shock
Dangerous.Therefore, in terms of equipment design and type selecting, use the mechanical mill refinement based on friction force
Grinding mode.The above main ball mill includes the grinding chamber with stirring, grinding chamber upper cover, mill ball；
Grinding chamber is the uncovered cavity structure in top, grinding chamber upper cover be anchored on above grinding chamber cover above it uncovered,
And arrange sealing in case material spills, grinding chamber is covered with grinding chamber charging aperture, is provided with bottom grinding chamber and grinds
Mill chamber discharging opening, mill ball is placed in grinding chamber；
In order to reduce risk factor to greatest extent, wet grinding is used to pulverize when preparing ultra-fine CL-20,
I.e. using lapping liquid is abrasive media, and lapping liquid and CL-20 are uniformly mixed in blender CL-20 slurry
Material, grinds this slurry in the grinding chamber of main ball mill；Thus make to grind and middle produce because of friction
Raw heat and energy by liquid transfer and consume, thus realize safety in production.Meanwhile, in order to realize
The superfine grinding of material, the slurry that increase CL-20 and lapping liquid the configure holdup time in grinding chamber, logical
Cross pipeline to be connected with the grinding chamber of main ball mill by blender with product pump, make slurry exist within a certain period of time
Circulate between blender and grinding chamber, it is achieved the circulation attrition grinding of material.
It is provided with stirring in described blender, blender is provided with discharging opening and recycle feed mouth, blender
Discharging opening be connected with the grinding chamber feeding hole pipeline covered on the grinding chamber of main ball mill, described grinding chamber
Discharging opening is connected with the recycle feed mouth pipeline of blender, near the position of grinding chamber on this recycle feed mouth pipeline
Install and be equipped with outlet valve, be provided with product pump on recycle feed mouth pipeline afterwards.
More specifically:
Described grinding chamber upper cover is fixed in above grinding chamber by spring clamp.Grinding chamber upper cover and grinding chamber spacious
Sealing between Kou can use various sealing structure of the prior art, is preferably provided with rubber ring and seals.
The stirring of described grinding chamber includes agitator, grinding chamber shaft and motor；Agitator is positioned at grinding chamber
Among, coaxial with grinding chamber, and the bottom in agitator bottom and grinding chamber leaves gap, and this gap is excellent
Elect 5～10mm as；Grinding chamber shaft connects agitator and motor through the centre bore of grinding chamber upper cover.Stirring
Device can use various agitators in prior art, in order to increase shearing force, be more preferably provided with multilamellar, many
The radially agitator of stirring rod.
In order to reduce the heat produced in process of lapping because of mechanism, it is to avoid the too high impact on material of temperature,
Grinding chamber outer layer is provided with cooling water jecket.The outer layer of described grinding chamber is preferably provided with cooling water jecket, chuck
On be provided with cooling water inlet and outlet.
Owing to CL-20 can discharge number acid when grinding refinement, therefore, grind cavity and the material of mill ball
Matter is in addition to having the strongest rigidity and wear-resisting effect, it is necessary to bear stronger acid corrosion-resistant ability, it is impossible to give
Product brings extra pollution impurity.Therefore, device is the most preferably adopted with material contact portion such as grinding chamber etc.
With the stainless steel material of wear resistant corrosion resistant, mill ball then select purity 99.9% or above zirconium oxide abrasive
Ball.Zirconium oxide high abrasion, acidproof it is well suited as the material of mill ball in present device.
The sphericity of mill ball is the biggest, and mill ball is spherical closer to standard, and sphericity is the biggest, and equipment grinds
During mill, safety is the highest, and the granular size of products C L-20 obtained is the most homogeneous, and particle size distribution is the narrowest.Grind
Bulb diameter is the least, and under similarity condition, the granularity of products C L-20 is the least；Mill ball diameter is the biggest, same to batten
Under part, the granularity of products C L-20 is the biggest.In order to be able to improve the safety of process of lapping, increase products C L-20
The homogeneity of granularity, reduces the particle size span of products C L-20, described mill ball sphericity preferably more than 0.99；
Depending on its diameter range can require according to CL-20 product granularity, preferably 3～10mm.
Described blender is open-top receptacle or container with cover；If open-top receptacle, from described ball mill
The pipeline outlet that the grinding chamber discharging opening of main frame comes is inserted directly into above blender as recycle feed mouth；If
Blender is lidded container, and it covers and is provided with recycle feed mouth, and the pipeline phase from grinding chamber discharging opening
Connect；The stirring of blender includes agitator, stirring paddle and motor；Agitator is arranged in blender, stirs
Mix device to be connected with motor by stirring paddle.
In the above discharge valve and pipeline, the conventional valve used is both preferably ball valve；Motor used is equal
It is preferably fire-proof motor.
Described main ball mill is connected by power line and holding wire has remote controllers, remote controllers to include
Digital display screen, variable-frequency governor, timer, motor switch, it is achieved the long-range control to device running operation.
Complete the automatization produced and the safety ensureing operator to greatest extent.
The two of the purpose of the present invention are to provide the rapid batch preparation method of a kind of ultra-fine CL-20.
The preparation method is that first taking described mill ball joins in grinding chamber, afterwards by raw material CL-20
The CL-20 slurry being uniformly mixed it is sufficiently mixed with lapping liquid；Again CL-20 slurry is input to above-mentioned grinding
Mill chamber is circulated attrition grinding, through abundant attrition grinding CL-20 slurry discharge after through vacuum filtration,
It is dried, finally gives ultra-fine CL-20.
Specifically, the preparation method of the present invention comprises the following steps:
(1) weigh the mill ball of a diameter of 3～10mm to join in grinding chamber；Mill ball filling rate (refers to grind
Abrading-ball fills the volume filling rate of grinding chamber) products C L-20 size and distribution are had a great impact,
When filling rate is less, being easily formed interstice coverage between abrading-ball, slurry easily " short-circuit " is escaped from, thus crushing effect is poor.
When filling rate is higher, grinding-crushing effect is preferable, but slurry flow resistance in mill chamber increases, stirring difficulty,
CL-20 is pulverized, most economical suitable filling rate 40～90%, preferably 65～80%.
(2) weigh raw material CL-20, measure lapping liquid and add in blender, be sufficiently mixed and be allowed to form mixing
Uniform slurry；
CL-20 sensitivity is the highest, and therefore this method uses waterproof pulverization to CL-20, i.e. CL-20 is steeped one
Plant in liquid medium and be ground, increase safety, it is only necessary to this liquid does not dissolves CL-20, grinds
Mill liquid refers to this liquid medium, and general conventional is water and ethanol, preferably water, including distilled water or go
Ionized water etc..
Products C L-20 size and distribution are also had a great impact by CL-20 slurry concentration.Slurry concentration
The lowest, the solid particle being ground between abrading-ball medium is few, and the probability that mill ball contacts with material is low, and it is pulverized
Weak effect；When slurry concentration is the highest, slurry viscosity increases, and material is difficult to dispersion, and product cut size becomes on the contrary
Slightly；The concentration of CL-20 slurry typically can 20～50%wt, preferably 35～40%wt crushing effect best.
(3) by the CL-20 slurry of mix homogeneously by described connection blender and the pipeline of grinding chamber and material
Pump, is input to grinding chamber be circulated attrition grinding from blender；Circular grinding time and the stirring of grinding
Rotating speed is depending on reaching the effect being fully ground, and general milling time is 1～2h；The speed of agitator ground is the highest,
Dangerous increase, rotating speed is the lowest, needs milling time oversize, efficiency step-down；General speed of agitator scope can
Select 5～30r/min, preferably 8～15r/min.
So-called circulation is pulverized, and refers to enter grinding chamber from mixing apparatus suspension CL-20 slurry out,
The grinding of mill ball and the shear action that stirred in filling the grinding chamber of mill ball and crushed grinding,
(being discharged to blender) is discharged again by grinding chamber；The slurry discharged afterwards is re-entered into further through circulating device
Grinding chamber is pulverized again, goes round and begins again, until grinding complete.
More specifically, the preparation method of the ultra-fine CL-20 of the present invention, is quickly to be criticized by mechanical polishing
That measures prepares ultra-fine CL-20.This equipment is dependent on mechanical agitator in grinding chamber (being fitted with many stirring rod)
Drive mill ball moves, and utilizes between mill ball and the extruding force between mill ball and mill chamber inwall and shearing force
Make CL-20 pulverize and grind.The CL-20 slurry grinding chamber charging aperture from grinding chamber top enters grinding chamber,
Then crushed by grinding and the shear force of mill ball in each cross section of grinding chamber, suspension
CL-20 slurry, by filling the grinding chamber of mill ball, is discharged to mixing by the grinding chamber discharging opening bottom grinding chamber
Device, disposed slurry be circulated attrition grinding through circulating device by being re-entered into grinding chamber, this process increase
Add the slurry holdup time in grinding chamber, the most ultra-fine CL-20 powder body can have been obtained.Due to it
Work process is waterproof pulverization, and attrition grinding process is carried out in grinding liquid medium, makes to produce in friction process
Raw heat quickly transmits and consumes, it is therefore prevented that process of lapping generates heat, it is ensured that process of lapping safety.
Described circulating device uses common liquid circulating apparatus in prior art, such as, connect blender and grinding chamber
Pipeline and pipeline on product pump.
(4) open discharge valve, release ground CL-20 slurry in grinding chamber and carry out vacuum filtration；So
After put at 40 DEG C of water-bath baking oven dry, obtain the ultra-fine CL-20 powder being dried.Ultra-fine CL-20's is average
Granularity can be in 2～20 μm.
Above vacuum filtration can use various vacuum filtration equipment of the prior art to carry out, preferred cycle ability of swimming
Vacuum pump carries out sucking filtration and is filtered dry.Above drying can use various drying plants in prior art to carry out, preferably
Baking oven uses water-bath baking oven to dry.
The preparation method of the above present invention, can pass through computer equipment remote control operation all processes, with reality
Existing automated production.
Additionally, for the sake of security, when using the method for the present invention to prepare ultra-fine CL-20, lead at control room
Cross Explosionproof camera and carry out the most omnidistance working order monitoring milling apparatus.
The equipment of the present invention is used for preparing ultra-fine CL-20, its yield typically 0.3～0.5 kilogram/batch, every batch
Secondary used time 1～2h, this yield and efficiency are far above conventional solvent-nonsolvent method and other method.The present invention's
Method uses the equipment of the present invention, can realize rapid batch and prepare ultra-fine CL-20.The method of the present invention only needs
As lapping liquid, the most there is not the pollution of organic solvent and there may be in conventional distilled water or deionized water
Toxic and side effects.The equipment of the present invention can realize remotely controlling and regulating, and thoroughly avoids in preparation process and endangers
The potential threat that operator are brought by danger factor.
Accompanying drawing explanation
Fig. 1 is the preparation system schematic diagram of the ultra-fine CL-20 of the present invention.
Fig. 2 is the ball mill structural representation of the present invention.
Fig. 3 is the grain size analysis figure of raw material CL-20.
Fig. 4 is the stereoscan photograph of raw material CL-20.
Fig. 5 is the ultra-fine CL-20 grain size analysis figure of the product obtained by embodiment 1.
Fig. 6 is the stereoscan photograph of the ultra-fine CL-20 of the product obtained by embodiment 1.
Fig. 7 is the ultra-fine CL-20 grain size analysis figure of the product obtained by embodiment 2.
Fig. 8 is the stereoscan photograph of the ultra-fine CL-20 of the product obtained by embodiment 2.
Fig. 9 is the ultra-fine CL-20 grain size analysis figure of the product obtained by embodiment 3.
Figure 10 is the stereoscan photograph of the ultra-fine CL-20 of the product obtained by embodiment 3.
In Fig. 1: 1 motor；2 stirring paddles；3 blenders；4 valves；5 circulating pumps；6 balls
Grinding machine.
In Fig. 2: 6-1 grinding chamber stirring motor；6-2 grinding chamber shaft；6-3 grinding chamber upper cover；
6-4 grinding chamber charging aperture；6-5 mill ball；6-6 grinding chamber；6-7 coolant outlet；6-8 cools down
Water inlet；6-9 grinding chamber discharging opening；7 remote controllers；7-1 digital display screen；7-2 variable-frequency governor；
7-3 timer；7-4 motor switch.
Detailed description of the invention:
Below in conjunction with embodiment, further illustrate the present invention.
Raw material:
Hexanitro azepine different 5 hereby alkane: CL-20, Qingyang, Liaoning special type Chemical Co., Ltd..
Fig. 3 is to use laser particle analyzer that the granularity of raw material CL-20 is analyzed the grain size analysis figure obtained；
The granularity of raw material CL-20 shown in it is relatively big, and mean diameter is about 150 μm.
Fig. 4 is the stereoscan photograph using scanning electron microscope to obtain raw material CL-20 photograph；Wherein
The granularity of shown raw material CL-20 is relatively big, and pattern is spindle, and there are sharp-pointed corner angle at two ends.
Method of testing and standard:
Grain size analysis: use MASTER200 type laser particle analyzer (Malvern Instr Ltd. of Britain)
The granularity of the granularity of raw material CL-20 and the ultra-fine CL-20 product of embodiment gained is carried out grain size analysis,
To grain size analysis figure.In grain size analysis figure, abscissa is particle diameter, unit μm；The left longitudinal axis is volume fraction,
Unit is %；The right longitudinal axis is cumulative volume mark, and unit is %.Curve 1 is size distribution curve, with the left side
The longitudinal axis is the longitudinal axis；Curve 2 is cumulative grain-size distribution curve, with the right longitudinal axis as the longitudinal axis.
Raw material CL-20 and the microscopic appearance of ultra-fine CL-20 product: use S-4700 type scanning electron microscope
(HIT) is to the ultra-fine CL-20 product of the microscopic appearance of raw material CL-20 and embodiment gained
Microscopic appearance is taken a picture, and obtains stereoscan photograph.
The preparation facilities of the ultra-fine CL-20 of the present invention is specific as follows:
As it is shown in figure 1, the preparation facilities of the ultra-fine CL-20 of the present invention, including main ball mill 6, with ball milling
Machine host 6 pipeline be connected blender 3 and product pump 5.
As in figure 2 it is shown, main ball mill 6 include with stirring grinding chamber 6-6, grinding chamber upper cover 6-3,
Mill ball 6-5；Grinding chamber 6-6 is the cavity structure that top is uncovered, and grinding chamber upper cover 6-3 utilizes spring clamp
It is fixed in and covers above it uncovered above grinding chamber 6-6, above grinding chamber upper cover 6-3 and grinding chamber 6-6, cover it
Arrange rubber ring between top is uncovered to seal；Grinding chamber upper cover 6-3 is provided with grinding chamber charging aperture 6-4, grinds
Being provided with grinding chamber discharging opening 6-9 bottom mill chamber 6-6, mill ball 6-5 is placed in grinding chamber 6-6.
The stirring of described grinding chamber includes agitator, grinding chamber shaft 6-2 and grinding chamber stirring motor 6-1；
Agitator is positioned among grinding chamber 6-6, coaxial with grinding chamber, and in agitator bottom and grinding chamber 6-6
7mm gap is left in bottom；Multilamellar, many radial direction stirring rod it are provided with on agitator.Grinding chamber shaft 6-2
Centre bore through grinding chamber upper cover 6-3 connects agitator and grinding chamber stirring motor 6-1；Described grinding chamber 6-6
Outer layer be provided with cooling water jecket, chuck is provided with cooling water inlet 6-8 and coolant outlet 6-7；
The rustless steel of described grinding chamber material selection wear resistant corrosion resistant；Described mill ball material selection purity is more than
The zirconium oxide of 99.9%.Mill ball particle size range is 3～10mm, and sphericity is 0.99.
As it is shown in figure 1, be provided with stirring in described blender 3, blender 3 be provided with discharging opening and follow
Ring charging aperture, blender 3 discharging opening and the grinding chamber charging aperture on the grinding chamber upper cover 6-3 of main ball mill 6
6-4 stylet is connected, and described grinding chamber discharging opening 6-9 is connected with the recycle feed mouth pipeline of blender 3, should
On pipeline, the position of grinding chamber 6-6 is provided with outlet valve 4, rear line on be provided with product pump 5.
Described blender 3 is open-top receptacle, the pipe come from the grinding chamber discharging opening 6-9 of described main ball mill 6
Line outlet is inserted directly into above blender 3 as the recycle feed mouth of blender 3；The stirring bag of blender 3
Include agitator, blender stirring paddle 2 and blender stirring motor 1；Agitator is arranged in blender 3, stirs
Mix device to be connected with blender stirring motor 1 by blender stirring paddle 2.
Described discharge valve 4 is ball valve；Motor used is fire-proof motor；With material contact portion in device
It is rustless steel.
Remote controllers 7, remote controllers 7 are had to include digital display screen as in figure 2 it is shown, main ball mill 6 connects
7-1, variable-frequency governor 7-2, timer 7-3, motor switch 7-4, it is achieved long-range to device running operation
Control.
When the ultra-fine CL-20 preparation facilities using the present invention produces ultra-fine CL-20 product, first will be suitable
The mill ball of amount joins in the grinding chamber of main ball mill, raw material CL-20 and lapping liquid is being mixed afterwards
It is sufficiently mixed in device and obtains CL-20 slurry；The CL-20 slurry of mix homogeneously is defeated by pipeline and product pump
Entering and be circulated attrition grinding in grinding chamber, crushing process is carried out in grinding liquid medium, through a timing
Between circulation attrition grinding CL-20 slurry through discharge valve discharge, through vacuum filtration, be dried, finally
Obtain ultra-fine CL-20 product.
What its principle was through mechanical lapping rapid batch prepares ultra-fine CL-20.This equipment is dependent on grinding chamber
Middle mechanical agitator drives mill ball motion, utilizes between mill ball and squeezing between mill ball and mill chamber inwall
Pressure and shearing force make CL-20 attrition grinding.CL-20 slurry enters from the grinding chamber charging aperture at grinding chamber top
Enter grinding chamber, then crushed by grinding and the shear force of mill ball in each cross section of grinding chamber,
The CL-20 slurry of suspension is by filling the grinding chamber of mill ball, by the grinding chamber discharging opening bottom grinding chamber
Be discharged to blender, disposed slurry pipeline between blender and grinding chamber and product pump be re-entered into
Grinding chamber is circulated attrition grinding, and this process adds the slurry holdup time in grinding chamber, can obtain
To the most ultra-fine CL-20 powder body.Owing to its work process is waterproof pulverization, attrition grinding process is being ground
Mill liquid medium is carried out, makes the heat produced in friction process quickly transmit and consume, it is therefore prevented that to grind
Honed journey is generated heat, it is ensured that process of lapping safety.
The detailed description of the invention of the ultra-fine CL-20 preparation method of the present invention is as follows:
Embodiment 1
(1) weigh 3.5kg zirconium oxide abrasive ball (zirconium oxide purity 99.9%, sphericity 0.99) to join
In grinding chamber, a diameter of 4mm of mill ball, filling rate is 75%.
(2) weigh 350g raw material CL-20, measure the mixing that 0.65L lapping liquid (distilled water) stirs in band
In device, it is sufficiently stirred for making both be sufficiently mixed into the CL-20 slurry of mix homogeneously in blender.CL-20
Slurry concentration is 35%wt.
(3) by above-mentioned CL-20 slurry in blender by circulating device (connect blender and grinding chamber it
Between pipeline and product pump thereon) be input in grinding chamber be circulated attrition grinding: CL-20 slurry is from grinding
The grinding chamber charging aperture at mill chamber top enters grinding chamber, carries out attrition grinding, then by grinding bottom grinding chamber
Mill chamber discharging opening is discharged to blender, disposed slurry followed by being re-entered into grinding chamber through circulating device again
Ring attrition grinding；Agitator speed is 10r/min, and the time of whole circulation attrition grinding is 2h.
(4) open grinding chamber discharging opening valve, CL-20 in grinding chamber and lapping liquid put into suction funnel,
Then it is filtered dry with circulating water type vacuum pump sucking filtration, is then placed at 40 DEG C of water-bath baking oven drying, obtains being dried
Ultra-fine CL-20 powder.Collect gained ultra-fine CL-20 powder and with Particle Size Analyzer, its particle size distribution carried out
Characterize.The results of grain size analysis of product is as it is shown in figure 5, the particle mean size of products obtained therefrom CL-20 is in 2.5 μm
Left and right；Narrower particle size distribution, product granularity is all below 10 μm.The stereoscan photograph of product such as Fig. 6
Shown in, the granular size ratio of products obtained therefrom CL-20 is more uniform, and surface is round and smooth, and without obvious corner angle, pattern is near
Like spheroid.
Whole preparation process, at control room by the Explosionproof camera omnidistance operating feelings monitoring milling apparatus in real time
Condition.The input and output material in simultaneous grinding chamber and the mixing speed of grinding chamber, the mixing speed of blender, circulating pump
Flow velocitys etc. all control automatically to carry out by remote computer.
Embodiment 2
(1) weigh 3.75kg mill ball (with embodiment 1) and join in grinding chamber, a diameter of 8mm of mill ball,
Filling rate is 80%.
(2) weigh 350g raw material CL-20, measure the mixing that 0.65L lapping liquid (distilled water) stirs in band
In device, it is sufficiently stirred for making both be sufficiently mixed into the CL-20 slurry of mix homogeneously in blender.CL-20
Slurry concentration is 35%wt.
(3) by above-mentioned CL-20 slurry in blender by circulating device (connect blender and grinding chamber it
Between pipeline and product pump thereon) be input in grinding chamber be circulated attrition grinding: CL-20 slurry is from grinding
The grinding chamber charging aperture at mill chamber top enters grinding chamber, carries out attrition grinding, then by grinding bottom grinding chamber
Mill chamber discharging opening is discharged to blender, disposed slurry followed by being re-entered into grinding chamber through circulating device again
Ring attrition grinding；Agitator speed is 8r/min, and the time of whole circulation attrition grinding is 1h.
(4) open grinding chamber discharging opening valve, CL-20 in grinding chamber and lapping liquid put into suction funnel,
Then it is filtered dry with circulating water type vacuum pump sucking filtration, is then placed at 40 DEG C of water-bath baking oven drying, obtains being dried
Ultra-fine CL-20 powder.Collect gained ultra-fine CL-20 powder and with Particle Size Analyzer, its particle size distribution carried out
Characterize.The results of grain size analysis of product is as it is shown in fig. 7, the particle mean size of products C L-20 is about 18 μm；
Narrower particle size distribution, 90% product cut size is all below 30 μm.The stereoscan photograph of product as shown in Figure 8,
The granular size ratio of products obtained therefrom CL-20 is more uniform, and surface is round and smooth, without obvious corner angle, pattern approximate spheres.
Whole preparation process, at control room by the Explosionproof camera omnidistance operating feelings monitoring milling apparatus in real time
Condition.The input and output material in simultaneous grinding chamber and the mixing speed of grinding chamber, the mixing speed of blender, circulating pump
Flow velocitys etc. all control automatically to carry out by remote computer.
Embodiment 3
(1) weigh 3.5kg mill ball (with embodiment 1) and join in grinding chamber, mill ball by 8mm,
4mm two kinds of diameters gradation composition of 2:5 in mass ratio, i.e. 8mm mill ball is that 1kg, 4mm mill ball is
2.5kg；Filling rate 75%；
(2) weigh 400g raw material CL-20, measure the mixing that 0.6L lapping liquid (distilled water) stirs in band
In device, it is sufficiently stirred for making both be sufficiently mixed into the CL-20 slurry of mix homogeneously in blender.CL-20
Slurry concentration is 40%wt.
(3) by above-mentioned CL-20 slurry in blender by circulating device (connect blender and grinding chamber it
Between pipeline and product pump thereon) be input in grinding chamber be circulated attrition grinding: CL-20 slurry is from grinding
The grinding chamber charging aperture at mill chamber top enters grinding chamber, carries out attrition grinding, then by grinding bottom grinding chamber
Mill chamber discharging opening is discharged to blender, disposed slurry followed by being re-entered into grinding chamber through circulating device again
Ring attrition grinding；Agitator speed is 14r/min, and the time of whole circulation attrition grinding is 2h.
(4) open grinding chamber discharging opening valve, CL-20 in grinding chamber and lapping liquid put into suction funnel,
Then it is filtered dry with circulating water type vacuum pump sucking filtration, is then placed at 40 DEG C of water-bath baking oven drying, obtains being dried
Ultra-fine CL-20 powder.Collect gained ultra-fine CL-20 powder and with Particle Size Analyzer, its particle size distribution carried out
Characterize.The results of grain size analysis of product is as shown in Figure 9；The particle mean size of products C L-20 is about 3.5 μm；
Narrower particle size distribution, product cut size is all below 10 μm.The stereoscan photograph of product as shown in Figure 10,
The granular size ratio of products obtained therefrom CL-20 is more uniform, and surface is round and smooth, without obvious corner angle, pattern approximate spheres.
Whole preparation process, at control room by the Explosionproof camera omnidistance operating feelings monitoring milling apparatus in real time
Condition.The input and output material in simultaneous grinding chamber and the mixing speed of grinding chamber, the mixing speed of blender, circulating pump
Flow velocitys etc. all control automatically to carry out by remote computer.
Claims (12)
1. a preparation facilities of ultra-fine CL-20, including main ball mill, it is characterised in that:
It is provided with the blender and product pump being connected with main ball mill；
Described main ball mill includes the grinding chamber with stirring, grinding chamber upper cover, mill ball；Grinding chamber is
The cavity structure that top is uncovered, grinding chamber upper cover is anchored on above grinding chamber and covers uncovered above it and arrange close
Envelope, grinding chamber is covered with grinding chamber charging aperture, is provided with grinding chamber discharging opening bottom grinding chamber, and mill ball is put
In grinding chamber, mill ball filling rate is 65～80%；Described mill ball material selection zirconium oxide；
It is provided with stirring in described blender, blender is provided with discharging opening and recycle feed mouth, blender
Discharging opening be connected with the grinding chamber feeding hole pipeline covered on the grinding chamber of main ball mill, described grinding chamber
Discharging opening is connected with the recycle feed mouth pipeline of blender, near the position of grinding chamber on this recycle feed mouth pipeline
Install and be equipped with outlet valve, be provided with product pump on recycle feed mouth pipeline afterwards.
Preparation facilities the most according to claim 1, it is characterised in that:
The stirring of described grinding chamber includes agitator, grinding chamber shaft and motor；Described agitator is positioned at and grinds
Among mill chamber, coaxial with grinding chamber, and the bottom in agitator bottom and grinding chamber leaves gap；Grind
Chamber shaft connects agitator and motor through the centre bore of grinding chamber upper cover.
Preparation facilities the most according to claim 2, it is characterised in that:
Described agitator bottom is 5～10mm with the gap of the bottom in grinding chamber.
Preparation facilities the most according to claim 1, it is characterised in that:
The outer layer of described grinding chamber is provided with cooling water jecket, and chuck is provided with cooling water inlet and outlet；
Described grinding chamber upper cover is fixed in above grinding chamber by spring clamp；Grinding chamber upper cover and grinding chamber spacious
It is provided with rubber ring between Kou to seal；
The rustless steel of described grinding chamber material selection wear resistant corrosion resistant.
5. according to the preparation facilities described in claims 1, it is characterised in that:
Described blender is open-top receptacle or container with cover；If open-top receptacle, from described ball mill
The pipeline outlet that the grinding chamber discharging opening of main frame comes is inserted directly into above blender as recycle feed mouth；If
Blender is lidded container, and it covers and is provided with recycle feed mouth, and the pipeline phase from grinding chamber discharging opening
Connect；The stirring of blender includes agitator, stirring paddle and motor；Agitator is arranged in blender, stirs
Mix device to be connected with motor by stirring paddle.
6. according to the preparation facilities one of claims 1～5 Suo Shu, it is characterised in that:
Described mill ball sphericity is more than 0.99；Its diameter range is 3～10mm.
7. according to the preparation facilities described in claims 1, it is characterised in that:
The stirring of the grinding chamber of described main ball mill includes agitator, grinding chamber shaft and motor；Stirring
Device is positioned among grinding chamber, coaxial with grinding chamber, and agitator bottom is left with the bottom in grinding chamber
The gap of 5～10mm；Grinding chamber shaft connects agitator and motor through the centre bore of grinding chamber upper cover；Institute
The outer layer stating grinding chamber is provided with cooling water jecket, and chuck is provided with cooling water inlet and outlet；Described grinding
Chamber upper cover is fixed in above grinding chamber by spring clamp, and grinding chamber upper cover and the uncovered of grinding chamber are provided directly with
Rubber ring seals；
The rustless steel of described grinding chamber material selection wear resistant corrosion resistant；
Described blender is open-top receptacle or container with cover；If open-top receptacle, from described ball mill
The pipeline outlet that the grinding chamber discharging opening of main frame comes is inserted directly into above blender；If blender is appearance with cover
Device, it covers and is provided with recycle feed mouth, is connected with the pipeline from grinding chamber discharging opening；Blender
Stirring includes agitator, stirring paddle and motor；Agitator is arranged in blender, agitator by stirring paddle with
Motor connects；
Described mill ball sphericity is more than 0.99；Its diameter range is 3～10mm；
Described discharge valve is ball valve；Motor used is fire-proof motor；
Described main ball mill connect have remote controllers, remote controllers include digital display screen, variable-frequency governor,
Timer, motor switch, it is achieved the long-range control to preparation facilities running operation.
8. the ultra-fine CL-20 preparation side using the described ultra-fine CL-20 preparation facilities of one of claim 1～7
Method, including: first take described mill ball and join in described main ball mill grinding chamber, afterwards by raw material CL-20
The CL-20 slurry being uniformly mixed it is sufficiently mixed with lapping liquid；Again CL-20 slurry is input to above-mentioned grinding
Mill chamber is circulated attrition grinding, through abundant attrition grinding CL-20 slurry discharge after through vacuum filtration,
It is dried, finally gives described ultra-fine CL-20.
Preparation method the most according to claim 8, it is characterised in that comprise the following steps:
(1) weigh mill ball to join in described main ball mill grinding chamber；
(2) weigh raw material CL-20, add in described blender with lapping liquid, be sufficiently mixed to be allowed to be formed and mix
Close the slurry that uniform concentration is 20～50%wt；Described lapping liquid is water or ethanol；
(3) it is input to described grinding chamber be circulated powder from described blender by CL-20 slurry obtained as above
Breakdown mill；
(4), after circulation attrition grinding, open discharge valve, release CL-20 ground in grinding chamber
Slurry carries out vacuum filtration, dries, obtains the ultra-fine CL-20 powder being dried.
Preparation method the most according to claim 9, it is characterised in that:
Described step (2) weighs raw material CL-20, adds in described blender with lapping liquid, is sufficiently mixed and makes
The slurry that concentration is 35～40%wt of formation mix homogeneously.
11. preparation methoies according to claim 9, it is characterised in that:
The time of described step (3) circulation attrition grinding is 1～2h；In described grinding chamber, agitator speed is
5～30r/min.
12. preparation methoies according to claim 11, it is characterised in that:
Described in described step (3), in grinding chamber, agitator speed is 8～15r/min.
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| CN106553117A (en) * | 2016-10-17 | 2017-04-05 | 北京理工大学 | A kind of method that mechanical lapping prepares 20 crystal of spherical super fine ε CL |
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| CN112403619B (en) * | 2020-10-28 | 2022-01-07 | 南京新康达磁业股份有限公司 | Mechanical ball milling device for preparing ferrite material and ball milling method thereof |
| CN114632460A (en) * | 2022-03-09 | 2022-06-17 | 宜兴市星光宝亿化工有限公司 | Stirring device for grey water scale inhibition and dispersion agent and using method thereof |
| CN115490695B (en) * | 2022-09-05 | 2024-02-20 | 雅邦绿色过程与新材料研究院南京有限公司 | CL-20 intermediate production process optimization method based on liquid continuous phase impinging stream |
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