CN103506194A - Preparation device and preparation method for ultrafine CL-20 - Google Patents
Preparation device and preparation method for ultrafine CL-20 Download PDFInfo
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- CN103506194A CN103506194A CN201210523625.7A CN201210523625A CN103506194A CN 103506194 A CN103506194 A CN 103506194A CN 201210523625 A CN201210523625 A CN 201210523625A CN 103506194 A CN103506194 A CN 103506194A
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Abstract
The invention provides a preparation device and a preparation method for ultrafine CL-20. The preparation device comprises a main grinding mill, a mixer and a material pump. A main ball mill comprises a grinding cavity with an agitator, and a grinding ball; the grinding ball is arranged in the grinding cavity. An agitator is arranged in the mixer, a discharge outlet and a cyclic feed inlet are formed in the mixer, the discharge outlet of the mixer is connected with a feed inlet of the main ball mill through a pipeline, a discharge outlet of the grinding cavity is connected with the cyclic feed inlet of the mixer by a pipeline, a discharge valve is arranged at a position, close to the grinding cavity, on the pipeline, and the material pump is arranged behind the discharge valve. The preparation method comprises the steps of adding the grinding ball into the grinding cavity of the main ball mill, then inputting the mixed slurry of active ingredient CL-20 and grinding liquid into the grinding cavity, circularly crushing and grinding, then discharging and performing vacuum filtration and drying, to obtain the ultrafine CL-20. The preparation device and the preparation method are simple to operate, high in safety, high in production efficiency, and capable of being widely applied to refinement of various energetic materials.
Description
Technical field
The present invention relates to a kind of refinement technology of energetic material, say further, relate to the device and method of a kind of ultra-fine CL-20 of preparation of rapid batch.
Background technology
Along with the fierceness day by day of scientific and technical development and weapon antagonism, the refinement technology of explosive is in the ascendant both at home and abroad.Because ultra-fine explosive has following advantage: detonation course approaches ideal detonation rule, potential interior can the developing of blast; Good heat conductivity, easily carries out heat conduction, and the focus that makes to explode is difficult for emerging; Be easy to carry out grain composition with large particle diameter explosive, dispersive property is good, promotes degree of packing better and more even; While being hit load, impulsive force evenly spreads in whole powder column very soon, reduces impact sensitivity.Therefore, ultra-fine explosive will play important effect in actual applications.
CL-20(hexanitro azepine different 5 is alkane hereby) be a kind of high energy density compound, density ratio HMX (HMX) is high by 8%, and explosion velocity is high by 6%, and energy density is high more than 15%.Cl-20 is energy density and the highest simple substance ammonal of explosion velocity so far, in following weaponry, has good application prospect.Ultra-fine CL-20, especially submicron order, nanoscale CL-20, except retaining the excellent properties of plain particles CL-20 high-energy-density, also there is shock sensitivity and impact sensitivity is lower, safer characteristic, this to widening the range of application of CL-20, to improve the performance of armament systems significant.
At present, ultra-fine CL-20 preparation method mainly contains solvent-nonsolvent recrystallization method, supercritical fluid recrystallization method, micro emulsion method, high-speed jet comminuting method etc., but respectively have its pluses and minuses.
Solvent-nonsolvent recrystallization method is with chemical solvent, to dissolve CL-20 to make saturated solution, then with the dilution of non-solvent inert fluid, disperses, and explosive is recrystallized with granule crystal state.The ultra-fine CL-20 of preparation, granularity is generally in micron or submicron order.Its shortcoming is that cost is high, yields poorly, and the production cycle is long; Be difficult to make explosive particle diameter ultra-fine to sub-micron, nano-scale; Solvent is required high, spent organic solvent discharge capacity is large and be difficult for reclaiming.The spent organic solvent amount that the ultra-fine CL-20 of every hectogram need to discharge is more than 1000 grams, and the granularity requirements of product is thinner, and the organic liquid waste amount of discharge is larger.
Micro emulsion method is to adopt special-purpose surfactant to improve CL-20 surface characteristics, continuous ultra-fine emulsification, in molecular scale magnitude, superelevation segmentation, becomes the good even powder CL-20 of physical property that flows under certain thermograde condition and under certain process conditions.Its shortcoming is post processing more complicated, also there is no successfully so far the report of this post processing work both at home and abroad.
High-speed jet comminuting method, thump, extruding, shearing force, strong turbulence effect and the strong high pressure sound wave effect that utilizes percussion flow to produce when extremely narrow pipeline high speed flows collision in opposite directions, make additional year mechanical function be converted into enough more fully the strength that particle is pulverized and disperseed, thereby reach the object of CL-20 granular superfine.Its shortcoming is that this just need to do very large merit to liquid because solvent is by mutually clashing into and form atomized drop; Liquid flows and needs very large pressure in pipeline high speed, and this is very high to conditional requests such as device sealing and resistance to pressures.
Ye You laboratory adopts hand grinding method to obtain the tiny CL-20 of granularity.As May L Chan(MayL Chan.New Ingredients for non-polluting propellants[J], CA93555-6001USA) HNIW is dispersed in the abrading glass vessel that distilled water and alcohol mixeding liquid body are housed and grinds 14 ~ 16 hours, obtained the HNIW of granularity in 3 μ m left and right.But the problems such as danger that this method exists milling time to grow, yield poorly, size distribution is inhomogeneous, waste liquid amount is large and hand lapping exists.
In a word, said method exists complex process in various degree, and cost is high, yields poorly, and efficiency is low, the bad control of granularity and wider distribution, and the shortcoming such as effect is not ideal enough, has limited its large-scale production and application in weapon.
Summary of the invention:
In order to solve the complex process of preparing ultra-fine CL-20 existence in prior art, cost is high, yield poorly, pollute heavy, the problems such as the bad control of granularity, the present invention designs a set of device that comprises ball mill, can realize fast the dangerous material material such as CL-20, in batches and pollution-free ultrafine pulverize, the granularity of product can realize according to the proportioning of milling time and mill ball.Provided simultaneously a kind of by mechanical lapping rapid batch and environmental protection prepare the method for CL-20.
One of object of the present invention is to provide a kind of device of preparing ultra-fine CL-20.
The preparation facilities of a kind of ultra-fine CL-20 of the present invention, comprises ball mill main frame, also includes the blender and the product pump that are connected with ball mill main frame.
Because CL-20 belongs to the high Energy Density Materials of high mechanical sensitivity, mechanical shock and clashing into is easily caused danger.Therefore,, aspect equipment design and selection, adopt and take friction force as main mechanical mill refinement grinding mode.The above ball mill main frame comprises with the grinding chamber, grinding chamber upper cover, the mill ball that stir; Grinding chamber is the uncovered cavity structure in top, and grinding chamber upper cover is anchored on grinding chamber top, and to cover its top uncovered, and sealing is set in case material spills, and is covered with charging aperture on grinding chamber, and grinding chamber bottom is provided with discharging opening, and mill ball is placed in grinding chamber;
In order to reduce to greatest extent hazards, when the ultra-fine CL-20 of preparation, adopt wet grinding to pulverize, adopting lapping liquid is abrasive media, and lapping liquid and CL-20 are uniformly mixed into CL-20 slurry in blender, and this slurry is ground in the grinding chamber of ball mill main frame; Make thus to grind middle because fricative heat and energy is by liquid transfer and consuming, thereby realize safety in production.Simultaneously, in order to realize the ultra-fine grinding of material, the holdup time of the slurry of increase CL-20 and lapping liquid configuration in grinding chamber, by pipeline, with product pump, blender is connected with the grinding chamber of ball mill main frame, slurry is circulated within a certain period of time between blender and grinding chamber, realize the circulation of material and pulverize grinding.
In described blender, be provided with stirring, on blender, be provided with discharging opening and recycle feed mouth, the charging aperture stylet covering on the grinding chamber of blender discharging opening and ball mill main frame is connected, the discharging opening of described grinding chamber is connected with the recycle feed mouth pipeline of blender, position near grinding chamber on this pipeline is provided with outlet valve, is provided with product pump afterwards on pipeline.
More specifically:
Described grinding chamber upper cover is fixed in grinding chamber top by spring clamp.Sealing between grinding chamber upper cover and grinding chamber uncovered can adopt various hermetically-sealed construction of the prior art, is preferably provided with rubber ring and seals.
The stirring of described grinding chamber comprises agitator, shaft and motor; Agitator is positioned among grinding chamber, coaxial with grinding chamber, and the bottom in agitator bottom and grinding chamber is left ，Gai gap, gap and is preferably 5 ~ 10mm; Shaft connects agitator and motor through the centre bore of grinding chamber upper cover.Agitator can adopt various agitators in prior art, in order to increase shearing force, is more preferably provided with the radially agitator of stirring rod of multilayer, many.
In order to reduce the heat producing because of mechanism in process of lapping, avoid the impact of excess Temperature on material, grinding chamber skin is provided with cooling water jecket.The skin of described grinding chamber is preferably provided with cooling water jecket, is provided with cooling water inlet and outlet on chuck.
Because CL-20 can discharge number acid when grinding refinement, therefore, grind the material of cavity and mill ball except having very strong rigidity and wear-resisting effect, also must bear stronger acid corrosion-resistant ability, can not bring extra pollution impurity to product.Therefore, device and material contact portion select purity 99.9% or above zirconium oxide abrasive ball such as grinding chamber etc. all preferably adopts the stainless steel material of wear resistant corrosion resistant, mill ball.Zirconia high abrasion, the acidproof material being well suited for as mill ball in present device.
The sphericity of mill ball is larger, and mill ball is more near the mark spherical, and sphericity is larger, when equipment grinds security higher, the granular size of the products C L-20 obtaining is got over homogeneous, size distribution is narrower.Mill ball diameter is less, and under similarity condition, the granularity of products C L-20 is less; Mill ball diameter is larger, and under similarity condition, the granularity of products C L-20 is larger.In order to improve the security of process of lapping, increase the homogeneity of products C L-20 granularity, reduce the particle size span of products C L-20, described mill ball sphericity is preferably more than 0.99; Its diameter range can require to determine according to CL-20 product granularity, is preferably 3 ~ 10mm.
Described blender is open-top receptacle or container with cover; If open-top receptacle, the pipeline outlet next from the grinding chamber discharging opening of described ball mill main frame directly inserts blender top as recycle feed mouth; If blender is lidded container, it covers and is provided with recycle feed mouth, is connected with the pipeline from grinding chamber discharging opening; The stirring of blender comprises agitator, shaft and motor; Agitator is arranged in blender, and agitator is connected with motor by shaft.
In the above discharge valve and pipeline, the conventional valve of using is all preferably ball valve; Motor used is all preferably fire-proof motor.
Described ball mill main frame is connected with remote controllers by power line and holding wire, and remote controllers comprise digital display screen, variable-frequency governor, timer, motor switch, realizes the Long-distance Control to device running operation.The safety that completes the automation of production and ensure to greatest extent operating personnel.
Two of object of the present invention is to provide the rapid batch preparation method of a kind of ultra-fine CL-20.
First preparation method of the present invention gets described mill ball to join in grinding chamber, afterwards raw material CL-20 and lapping liquid is fully mixed to get to the CL-20 slurry mixing; CL-20 slurry being input to circulates in above-mentioned grinding chamber again pulverizes and grinds, after fully pulverizing the CL-20 slurry grinding and discharging through vacuum filtration, be dried, finally obtain ultra-fine CL-20.
Particularly, preparation method of the present invention comprises the following steps:
(1) taking diameter is that the mill ball of 3 ~ 10mm joins in grinding chamber; Mill ball filling rate (refer to mill ball fill the volume filling rate of grinding chamber) has a great impact products C L-20 particle size and distribution, and filling rate hour, easily forms interstice coverage between abrading-ball, and slurry easily " short circuit " is escaped from, thereby crushing effect is poor.When filling rate is higher, grinding-crushing effect is better, but difficulty is stirred in slurry flow resistance increase in mill chamber, for CL-20, pulverizes, and most economical suitable filling rate 40 ~ 90%, is preferably 65 ~ 80%.
(2) take raw material CL-20, measure lapping liquid and add in blender, fully mix and make it to form the slurry mixing;
CL-20 sensitivity is too high, therefore this method adopts wet pulverizing to CL-20, CL-20 bubble is ground in a kind of liquid medium, increase security, only need this liquid not dissolve CL-20, lapping liquid just refers to this liquid medium, and generally conventional is water and ethanol, preferred water, comprises distilled water or deionized water etc.
CL-20 slurry concentration also has a great impact products C L-20 particle size and distribution.Slurry concentration is too low, and between abrading-ball medium, polished solid particle is few, and the probability that mill ball contacts with material is low, and its crushing effect is poor; When slurry concentration is too high, slurry viscosity increases, and material is difficult for disperseing, and product cut size is chap on the contrary; The concentration of CL-20 slurry generally can be at 20 ~ 50%wt, and preferably 35 ~ 40%wt crushing effect is best.
(3) by the CL-20 slurry mixing by pipeline and the product pump of described connection blender and grinding chamber, from blender, be input to grinding chamber, to circulate to pulverize and grind; The speed of agitator of circular grinding time and grinding is depending on reaching the effect of abundant grinding, and general milling time is 1 ~ 2h; The speed of agitator grinding is too high, dangerous increase, and rotating speed is too low, needs milling time oversize, efficiency step-down; General speed of agitator scope can be selected 5 ~ 30r/min, preferably 8 ~ 15r/min.
So-called circulation is pulverized, and refers to from mixing apparatus suspension CL-20 slurry out and enters grinding chamber, is pulverized and grinds, then discharge (being discharged to blender) by grinding chamber through filling the grinding of the mill ball stirring in the grinding chamber of mill ball and shear action; The slurry of discharging is afterwards re-entered grinding chamber by EGR again and is again pulverized, and goes round and begins again, until grind complete.
More specifically, the preparation method of ultra-fine CL-20 of the present invention, is the ultra-fine CL-20 of preparation by mechanical polishing rapid batch.This equipment is to rely on mechanical agitator (many stirring rod are housed) in grinding chamber to drive mill ball motion above, utilize between mill ball and mill ball and mill chamber inwall between extruding force and shearing force CL-20 is pulverized and grinds.CL-20 slurry enters grinding chamber from the charge door at grinding chamber top, then in each cross section of grinding chamber, be subject to the grinding of mill ball and shear force and pulverized, the CL-20 slurry of suspension is by filling the grinding chamber of mill ball, discharging opening by grinding chamber bottom is discharged to blender, slurry is re-entered grinding chamber through EGR and circulate and pulverize grinding afterwards, this process has increased the holdup time of slurry in grinding chamber, can obtain more preferably ultra-fine CL-20 powder.Because its course of work is wet pulverizing, pulverize process of lapping and carry out in grinding liquid medium, make the heat producing in friction process transmit fast and consume, prevented process of lapping heating, guaranteed process of lapping safety.Described EGR adopts common liquid circulating apparatus in prior art, for example, connect the pipeline of blender and grinding chamber and the product pump on pipeline.
(4) open discharge valve, emit the CL-20 slurry grinding in grinding chamber and carry out vacuum filtration; Then put at 40 ℃, water-bath baking oven and dry, the ultra-fine CL-20 powder that obtains being dried.The particle mean size of ultra-fine CL-20 can be at 2 ~ 20 μ m.
Above vacuum filtration can adopt various vacuum filtration equipment of the prior art to carry out, and preferred cycle ability of swimming vavuum pump carries out suction filtration and is filtered dry.Above oven dry can adopt various drying plants in prior art to carry out, and preferably baking oven adopts water-bath baking oven to dry.
Preparation method of the present invention, can pass through computer equipment remote control operation all processes, to realize automated production above.
In addition, for the sake of security, adopt method of the present invention to prepare ultra-fine CL-20 Shi， control room and carry out the omnidistance working order that monitors milling apparatus in real time by Explosionproof camera.
Equipment of the present invention is used for preparing ultra-fine CL-20, and its output is generally at 0.3 ~ 0.5 kilogram/batch, every batch of used time 1 ~ 2h, and this output and efficiency are far above conventional solvent-nonsolvent method and other method.Method of the present invention adopts equipment of the present invention, can realize rapid batch and prepare ultra-fine CL-20.Method of the present invention only needs conventional distilled water or deionized water as lapping liquid, does not therefore have the pollution of organic solvent and the toxic and side effect that may exist.Equipment of the present invention can be realized Long-distance Control and adjusting, has thoroughly avoided the potential threat that in preparation process, hazards are brought operating personnel.
Accompanying drawing explanation
Fig. 1 is the preparation system schematic diagram of ultra-fine CL-20 of the present invention.
Fig. 2 is 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 embodiment 1 resulting product.
Fig. 6 is the stereoscan photograph of the ultra-fine CL-20 of embodiment 1 resulting product.
Fig. 7 is the ultra-fine CL-20 grain size analysis figure of embodiment 2 resulting products.
Fig. 8 is the stereoscan photograph of the ultra-fine CL-20 of embodiment 2 resulting products.
Fig. 9 is the ultra-fine CL-20 grain size analysis figure of embodiment 3 resulting products.
Figure 10 is the stereoscan photograph of the ultra-fine CL-20 of embodiment 3 resulting products.
In Fig. 1: 1-motor; 2-paddle; 3-blender; 4-valve; 5-circulating pump; 6-ball mill.
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-cooling 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.
The specific embodiment:
Below in conjunction with embodiment, further illustrate the present invention.
raw material:
Hexanitro azepine different 5 is alkane: CL-20 hereby, the extraordinary Chemical Co., Ltd. in Qingyang, Liaoning.
The grain size analysis figure of Fig. 3 for adopting laser particle analyzer to obtain the granularity analysis of raw material CL-20; The granularity of the CL-20 of raw material shown in it is larger, and average grain diameter is in 150 μ m left and right.
The stereoscan photograph of Fig. 4 for adopting SEM that raw material CL-20 is taken a picture and obtained; The granularity of the CL-20 of raw material shown in it is larger, and pattern is spindle, and there are sharp-pointed corner angle at two ends.
method of testing and standard:
Grain size analysis: adopt MASTER200 type laser particle analyzer (Britain Ma Erwen Instrument Ltd.) to carry out grain size analysis to the granularity of the ultra-fine CL-20 product of the granularity of raw material CL-20 and embodiment gained, obtain grain size analysis figure.In grain size analysis figure, abscissa is particle diameter, the μ m of unit; The left longitudinal axis is volume fraction, and unit is %; The right longitudinal axis is cumulative volume mark, and unit is %.Curve 1 is size distribution curve, take left vertical as the longitudinal axis; Curve 2 is cumulative grain-size distribution curves, take the right longitudinal axis as the longitudinal axis.
The microscopic appearance of raw material CL-20 and ultra-fine CL-20 product: adopt S-4700 type SEM (HIT) to take a picture to the microscopic appearance of the ultra-fine CL-20 product of the microscopic appearance of raw material CL-20 and embodiment gained, obtain stereoscan photograph.
The preparation facilities of ultra-fine CL-20 of the present invention is specific as follows:
As shown in Figure 1, the preparation facilities of ultra-fine CL-20 of the present invention, comprises ball mill main frame 6, the blender 3 and the product pump 5 that are connected with ball mill main frame 6 pipelines.
As shown in Figure 2, ball mill main frame 6 comprises with the grinding chamber 6-6, grinding chamber upper cover 6-3, the mill ball 6-5 that stir; Grinding chamber 6-6 is the uncovered cavity structure in top, grinding chamber upper cover 6-3 utilize spring clamp to be fixed in grinding chamber 6-6 top to cover its top uncovered, grinding chamber upper cover 6-3 and grinding chamber 6-6 top cover and rubber ring are set between uncovered above it and seal; Grinding chamber upper cover 6-3 is provided with grinding chamber charging aperture 6-4, and grinding chamber 6-6 bottom is provided with grinding chamber discharging opening 6-9, and mill ball 6-5 is placed in grinding chamber 6-6.
The stirring of described grinding chamber comprises 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 7mm gap is left in the bottom in agitator bottom and grinding chamber 6-6; On agitator, be provided with radially stirring rod of multilayer, many.Grinding chamber shaft 6-2 connects agitator and grinding chamber stirring motor 6-1 through the centre bore of grinding chamber upper cover 6-3; The skin of described grinding chamber 6-6 is provided with cooling water jecket, is provided with cooling water inlet 6-8 and coolant outlet 6-7 on chuck;
The stainless steel of described grinding chamber material selection wear resistant corrosion resistant; The zirconia that described mill ball material selection purity is greater than 99.9%.Mill ball particle size range is at 3 ~ 10mm, and sphericity is 0.99.
As shown in Figure 1, in described blender 3, be provided with stirring, on blender 3, be provided with discharging opening and recycle feed mouth, grinding chamber charging aperture 6-4 stylet on the grinding chamber upper cover 6-3 of blender 3 discharging openings and ball mill main frame 6 is connected, described grinding chamber discharging opening 6-9 is connected with the recycle feed mouth pipeline of blender 3, on this pipeline, near grinding chamber 6-6 position, be provided with outlet valve 4, on pipeline, be provided with afterwards product pump 5.
Described blender 3 is open-top receptacle, and the pipeline outlet coming from the grinding chamber discharging opening 6-4 of described ball mill main frame 6 directly inserts blender 3 tops as the recycle feed mouth of blender 3; The stirring of blender 3 comprises agitator, blender shaft 2 and blender stirring motor 1; Agitator is arranged in blender 3, and agitator stirs shaft 2 by blender and is connected with blender stirring motor 1.
Described discharge valve 4 is ball valve; Motor used is fire-proof motor; In device, be stainless steel with material contact portion.
As shown in Figure 2, ball mill main frame 6 is connected with remote controllers 7, and remote controllers 7 comprise digital display screen 7-1, variable-frequency governor 7-2, timer 7-3, motor switch 7-4, realizes the Long-distance Control to device running operation.
When producing ultra-fine CL-20 product with ultra-fine CL-20 preparation facilities of the present invention, first appropriate mill ball is joined in the grinding chamber of ball mill main frame, afterwards raw material CL-20 and lapping liquid are fully mixed to get to CL-20 slurry in blender; The CL-20 slurry mixing is input in grinding chamber and is circulated and pulverize grinding by pipeline and product pump, crushing process carries out in grinding liquid medium, through the circulation of certain hour, pulverizing the CL-20 slurry grinding discharges through discharge valve, through vacuum filtration, dry, finally obtain ultra-fine CL-20 product.
Its principle is exactly the ultra-fine CL-20 of preparation by mechanical lapping rapid batch.This equipment is to rely on mechanical agitator in grinding chamber to drive mill ball motion, utilize between mill ball and mill ball and mill chamber inwall between extruding force and shearing force make CL-20 pulverize grinding.CL-20 slurry enters grinding chamber from the charge door at grinding chamber top, then in each cross section of grinding chamber, be subject to the grinding of mill ball and shear force and pulverized, the CL-20 slurry of suspension is by filling the grinding chamber of mill ball, discharging opening by grinding chamber bottom is discharged to blender, slurry is re-entered grinding chamber through the pipeline between blender and grinding chamber and product pump and circulate and pulverize grinding afterwards, this process has increased the holdup time of slurry in grinding chamber, can obtain more preferably ultra-fine CL-20 powder.Because its course of work is wet pulverizing, pulverize process of lapping and carry out in grinding liquid medium, make the heat producing in friction process transmit fast and consume, prevented process of lapping heating, guaranteed process of lapping safety.
The ultra-fine CL-20 preparation method's of the present invention specific embodiment is as follows:
(1) take 3.5kg zirconium oxide abrasive ball (zirconia purity 99.9%, sphericity 0.99) and join in grinding chamber, mill ball diameter is 4mm, and filling rate is 75%.
(2) take 350g raw material CL-20, measure 0.65L lapping liquid (distilled water) in the blender of band stirring, fully stir and make both in blender, fully be mixed into the CL-20 slurry mixing.CL-20 slurry concentration is 35%wt.
(3) by above-mentioned CL-20 slurry in blender by EGR (connect pipeline between blender and grinding chamber and product pump) be input in grinding chamber and circulate and pulverize grinding: CL-20 slurry enters grinding chamber from the charge door at grinding chamber top, pulverize grinding, then the discharging opening by grinding chamber bottom is discharged to blender, and slurry is re-entered grinding chamber through EGR again and circulate and pulverize grinding afterwards; Agitator speed is 10r/min, and it is 2h that the time of grinding is pulverized in whole circulation.
(4) open grinding chamber discharging opening valve, CL-20 in grinding chamber and lapping liquid are put into suction funnel, then with circulating water type vavuum pump suction filtration, be filtered dry, then put at 40 ℃, water-bath baking oven and dry, the ultra-fine CL-20 powder that obtains being dried.Collect the ultra-fine CL-20 powder of gained and with Particle Size Analyzer, its size distribution characterized.As shown in Figure 5, the particle mean size of products obtained therefrom CL-20 is in 2.5 μ m left and right for the results of grain size analysis of product; Narrower particle size distribution, product granularity is all below 10 μ m.As shown in Figure 6, the granular size of products obtained therefrom CL-20 is more even for the stereoscan photograph of product, and surface is round and smooth, and without obvious corner angle, pattern is similar to spheroid.
Whole preparation process ， control room is by the working order of Explosionproof camera whole process supervision in real time milling apparatus.The mixing speed of the input and output material in simultaneous grinding chamber and the mixing speed of grinding chamber, blender, the flow velocity of circulating pump etc. is all controlled automatically and is carried out by remote computer.
(1) take 3.75kg mill ball (with embodiment 1) and join in grinding chamber, mill ball diameter is 8mm, and filling rate is 80%.
(2) take 350g raw material CL-20, measure 0.65L lapping liquid (distilled water) in the blender of band stirring, fully stir and make both in blender, fully be mixed into the CL-20 slurry mixing.CL-20 slurry concentration is 35%wt.
(3) by above-mentioned CL-20 slurry in blender by EGR (connect pipeline between blender and grinding chamber and product pump) be input in grinding chamber and circulate and pulverize grinding: CL-20 slurry enters grinding chamber from the charge door at grinding chamber top, pulverize grinding, then the discharging opening by grinding chamber bottom is discharged to blender, and slurry is re-entered grinding chamber through EGR again and circulate and pulverize grinding afterwards; Agitator speed is 8r/min, and it is 1h that the time of grinding is pulverized in whole circulation.
(4) open grinding chamber discharging opening valve, CL-20 in grinding chamber and lapping liquid are put into suction funnel, then with circulating water type vavuum pump suction filtration, be filtered dry, then put at 40 ℃, water-bath baking oven and dry, the ultra-fine CL-20 powder that obtains being dried.Collect the ultra-fine CL-20 powder of gained and with Particle Size Analyzer, its size distribution characterized.As shown in Figure 7, the particle mean size of products C L-20 is in 18 μ m left and right for the results of grain size analysis of product; Narrower particle size distribution, 90% product cut size is all below 30 μ m.As shown in Figure 8, the granular size of products obtained therefrom CL-20 is more even for the stereoscan photograph of product, and surface is round and smooth, and without obvious corner angle, pattern is similar to spheroid.
Whole preparation process ， control room is by the working order of Explosionproof camera whole process supervision in real time milling apparatus.The mixing speed of the input and output material in simultaneous grinding chamber and the mixing speed of grinding chamber, blender, the flow velocity of circulating pump etc. is all controlled automatically and is carried out by remote computer.
Embodiment 3
(1) take 3.5kg mill ball (with embodiment 1) and join in grinding chamber, mill ball is by 8mm, two kinds of diameter 2:5 gradation compositions in mass ratio of 4mm, and 8mm mill ball is 1kg, and 4mm mill ball is 2.5kg; Filling rate 75%;
(2) take 400g raw material CL-20, measure 0.6L lapping liquid (distilled water) in the blender of band stirring, fully stir and make both in blender, fully be mixed into the CL-20 slurry mixing.CL-20 slurry concentration is 40%wt.
(3) by above-mentioned CL-20 slurry in blender by EGR (connect pipeline between blender and grinding chamber and product pump) be input in grinding chamber and circulate and pulverize grinding: CL-20 slurry enters grinding chamber from the charge door at grinding chamber top, pulverize grinding, then the discharging opening by grinding chamber bottom is discharged to blender, and slurry is re-entered grinding chamber through EGR again and circulate and pulverize grinding afterwards; Agitator speed is 14r/min, and it is 2h that the time of grinding is pulverized in whole circulation.
(4) open grinding chamber discharging opening valve, CL-20 in grinding chamber and lapping liquid are put into suction funnel, then with circulating water type vavuum pump suction filtration, be filtered dry, then put at 40 ℃, water-bath baking oven and dry, the ultra-fine CL-20 powder that obtains being dried.Collect the ultra-fine CL-20 powder of gained and with Particle Size Analyzer, its size distribution characterized.The results of grain size analysis of product as shown in Figure 9; The particle mean size of products C L-20 is in 3.5 μ m left and right; Narrower particle size distribution, product cut size is all below 10 μ m.As shown in figure 10, the granular size of products obtained therefrom CL-20 is more even for the stereoscan photograph of product, and surface is round and smooth, and without obvious corner angle, pattern is similar to spheroid.
Whole preparation process ， control room is by the working order of Explosionproof camera whole process supervision in real time milling apparatus.The mixing speed of the input and output material in simultaneous grinding chamber and the mixing speed of grinding chamber, blender, the flow velocity of circulating pump etc. is all controlled automatically and is carried out by remote computer.
Claims (10)
1. a preparation facilities of ultra-fine CL-20, comprises ball mill main frame, it is characterized in that:
Be provided with the blender and the product pump that are connected with ball mill main frame;
Described ball mill main frame comprises with the grinding chamber, grinding chamber upper cover, the mill ball that stir; Grinding chamber is the uncovered cavity structure in top, and grinding chamber upper cover is anchored on grinding chamber top, and to cover its top uncovered and sealing is set, and is covered with charging aperture on grinding chamber, and grinding chamber bottom is provided with discharging opening, and mill ball is placed in grinding chamber;
In described blender, be provided with stirring, on blender, be provided with discharging opening and recycle feed mouth, the feeding hole pipeline covering on the grinding chamber of blender discharging opening and ball mill main frame is connected, the discharging opening of described grinding chamber is connected with the recycle feed mouth pipeline of blender, position near grinding chamber on this pipeline is provided with outlet valve, is provided with product pump afterwards on pipeline.
2. preparation facilities according to claim 1, is characterized in that:
The stirring of described grinding chamber comprises agitator, shaft and motor; Described agitator is positioned among grinding chamber, coaxial with grinding chamber, and gap is left in the bottom in agitator bottom and grinding chamber; Shaft connects agitator and motor through the centre bore of grinding chamber upper cover.
3. preparation facilities according to claim 2, is characterized in that:
The gap of the bottom in described agitator bottom and grinding chamber is 5 ~ 10mm.
4. preparation facilities according to claim 1, is characterized in that:
The skin of described grinding chamber is provided with cooling water jecket, is provided with cooling water inlet and outlet on chuck;
Described grinding chamber upper cover is fixed in grinding chamber top by spring clamp; Between grinding chamber upper cover and grinding chamber uncovered straight, being provided with rubber ring seals;
The stainless steel of described grinding chamber material selection wear resistant corrosion resistant; Described mill ball material selection zirconia.
5. according to the preparation facilities described in claims 1, it is characterized in that:
Described blender is open-top receptacle or container with cover; If open-top receptacle, the pipeline outlet next from the grinding chamber discharging opening of described ball mill main frame directly inserts blender top as recycle feed mouth; If blender is lidded container, it covers and is provided with recycle feed mouth, is connected with the pipeline from grinding chamber discharging opening; The stirring of blender comprises agitator, shaft and motor; Agitator is arranged in blender, and agitator is connected with motor by shaft.
6. according to the preparation facilities one of claims 1 ~ 5 Suo Shu, it is characterized 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 characterized in that:
The stirring of the grinding chamber of described ball mill main frame comprises agitator, shaft and motor; Agitator is positioned among grinding chamber, coaxial with grinding chamber, and the gap of 5 ~ 10mm is left in the bottom in agitator bottom and grinding chamber; Shaft connects agitator and motor through the centre bore of grinding chamber upper cover; The skin of described grinding chamber is provided with cooling water jecket, is provided with cooling water inlet and outlet on chuck; Described grinding chamber upper cover is fixed in grinding chamber top by spring clamp, and the uncovered rubber ring that is directly provided with of grinding chamber upper cover and grinding chamber seals;
The stainless steel of described grinding chamber material selection wear resistant corrosion resistant; The zirconia of described mill ball material selection high abrasion, acidproof, high-purity, high ball form quotient;
Described blender is open-top receptacle or container with cover; If open-top receptacle directly inserts blender top from the next pipeline outlet of the grinding chamber discharging opening of described ball mill main frame; If blender is lidded container, it covers and is provided with recycle feed mouth, is connected with the pipeline from grinding chamber discharging opening; The stirring of blender comprises agitator, shaft and motor; Agitator is arranged in blender, and agitator is connected with motor by shaft;
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; In device, be stainless steel with material contact portion;
Described ball mill main frame is connected with remote controllers, and remote controllers comprise digital display screen, variable-frequency governor, timer, motor switch, realizes the Long-distance Control to device running operation.
8. a ultra-fine CL-20 preparation method who adopts one of claim 1 ~ 7 described ultra-fine CL-20 preparation facilities, comprise: first get described mill ball and join in described ball mill main frame grinding chamber, afterwards raw material CL-20 and lapping liquid are fully mixed to get to the CL-20 slurry mixing; CL-20 slurry being input to circulates in above-mentioned grinding chamber again pulverizes and grinds, after fully pulverizing the CL-20 slurry grinding and discharging through vacuum filtration, be dried, finally obtain described ultra-fine CL-20.
9. preparation method according to claim 8, is characterized in that comprising the following steps:
(1) taking diameter is that the mill ball of 3 ~ 10mm joins in described ball mill main frame grinding chamber, and mill ball filling rate is 40 ~ 90%, is preferably 65 ~ 80%;
(2) take raw material CL-20, with lapping liquid, add in described blender, it is 20 ~ 50%wt that abundant mixing makes it to form the concentration mixing, preferably the slurry of 35 ~ 40%wt; Described lapping liquid is water or ethanol;
(3) above gained CL-20 slurry is input to described grinding chamber and circulates and pulverize grinding from described blender;
(4) after circulation is pulverized and ground, open discharge valve, emit the CL-20 slurry grinding in grinding chamber and carry out vacuum filtration, dry the ultra-fine CL-20 powder that obtains being dried.
10. preparation method according to claim 9, is characterized in that:
It is 1 ~ 2h that the time of grinding is pulverized in described step (3) circulation; In described grinding chamber, agitator speed is 5 ~ 30r/min, preferably 8 ~ 15r/min.
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| CN105413556A (en) * | 2014-09-15 | 2016-03-23 | 广东雪莱特光电科技股份有限公司 | Alumina dispersion apparatus |
| 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 |
| CN107088458A (en) * | 2017-04-20 | 2017-08-25 | 南京晓庄学院 | A kind of molecular biology experiment sample mill and its application method |
| CN108686526A (en) * | 2018-07-05 | 2018-10-23 | 马鞍山市思迪包装材料科技有限公司 | A kind of flow-type combination board processing solid-liquid mixing device |
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| 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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