CN102219232A - Efficient compact spherical agglomerated particle of superfine boron powder and preparation method thereof - Google Patents
Efficient compact spherical agglomerated particle of superfine boron powder and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-efficiency compact spherical agglomerated particle of superfine boron powder and a preparation method thereof, wherein the superfine boron powder is subjected to vacuum drying treatment at 70-90 ℃, added into a ball milling tank, added with a binder, a diluent, a functional assistant and a grinding ball in proportion, subjected to roller ball milling for 3-30 hours to prepare slurry, and subjected to spray drying granulation to prepare a fine spherical agglomerated particle of 25-80 mu m; the fine particles are directly introduced into a centrifugal granulator to serve as mother nuclei after thermal curing treatment, and grow gradually into compact spherical large agglomerated particles under the multiple actions of centrifugation, impact force and the like through continuous slurry spraying and powder supply. The prepared boron powder agglomerate has controllable particle size and high structural strength, and can well improve the addition amount and the combustion efficiency of boron powder fuel for explosives and propellants by proper particle size distribution and addition of functional components in the agglomerate.
Description
Technical field
The present invention relates to efficient dense spherical agglomerating particles of a kind of ultra-fine boron powder and preparation method thereof, belong to fiery explosive and propelling agent and use the compound granulation of boron powder fuel field.
Background technology
Boron has high volume calorific value and quality calorific value, is that present unique can making solid reaches the propelling energy more than the 10kNS/kg towards engine/motor specific impulse.The preparation of using undressed boron powder to carry out the boracic fuel-rich propellant mainly faces following several problem: 1, material such as the boric acid on boron powder surface and propelling agent system binding agent hydroxy-terminated polybutadienes (HTPB) reaction causes processing performance to worsen; 2, boron powder footpath is too small, and specific surface area is big, and addition is limited; The surface formed oxide film when 3, boron burnt, and hindered further burning, and combustionproperty is poor.Boron-propellant has been carried out big quantity research both at home and abroad for many years, the result shows boron particles is reunited, can reduce the specific surface value, increase addition, form coating film obstruct boric acid simultaneously on reunion boron powder surface and directly contact, can add short combustion composition in addition in the aggregation procedure and improve combustionproperty with HTPB.As seen the reunion to boron is the effective way that addresses the above problem.
Main spray-drying process, centrifugal granulation, kneading comminution granulation and the extruder grain method of adopting of the reunion boron powder preparation of domestic and foreign literature report, but the shortcoming that the particle density of spray drying method for preparation is low, there are the little and sphericity difference of granulometric range in centrifugal granulation nuclei of origin difficulty, the particle of mediating comminution granulation and the preparation of extruder grain method, and general preparation efficiency is low, reunion boron powder that can't the efficient production dense spherical.
Publication number for the CN101734680A(application number is: Chinese patent application 200910273247) relates to the method for utilizing the spray drying method for preparation spherical amorphous boron powder.Agglomerating particles sphericity, particles dispersed and the flowing property of the preparation of this method are good, can make the coating of powder and the step of reuniting realizes, and particle can keep original proterties, and can realize mass production, suitable industrial application.But the reunion boron powder that this method is produced adopts water and polyoxyethylene glycol as bonding system, and the boron powder that causes reuniting contains can weak effect, and density and granule strength are low, are not suitable for directly adding in the propelling agent system.
Publication number is 200910022197.8 for the CN101531556A(application number) Chinese patent application relate to and a kind of the boron powder adopted the kneader process for granulating.Publication number is 201010131010 for the CN101805238A(application number) Chinese patent application relate to employing with the premix of boron powder after the preparation method that sieves of extruding.Adopt the sieve particle density of preparation of kneader granulation and extruding higher, but only be fit to do larger particles and size range is little, Zhi Bei particulate matter homogeneity is relatively poor simultaneously.The particle of preparation is not the sphere of stricti jurise, and particle is difficult for disperseing.Therefore grain size distribution can't be realized, space and poly-boron powder inner material and inhomogeneous can be occurred piling up.
Summary of the invention
The present invention is intended to comprehensive centrifugal granulating and spray-dired advantage, utilize spray drying method for preparation fine grain size reunion boron powder particles, the small-particle of preparing serves as the centrifugal granulating parent nucleus, solve the problem that centrifugal granulation is difficult to nuclei of origin, utilize the compound prilling process of mist projection granulating-centrifugal granulator to prepare the poly-particle of ultra-fine boron powder ball.Adopt the parent nucleus of spraying drying preparation, the particle rounding, the production efficiency height is fit to mass production; In centrifugal granulator, introduce the parent nucleus of spraying drying preparation, can effectively solve ultrafine powder is difficult to nuclei of origin in centrifugal granulator problem, solved the loss of wafting in a large number of boron powder, the problem that production efficiency is low.The reunion boron powder particles intensity height that employing a process for preparing, the sphericity height, particle diameter is controlled, and the preparation efficiency height.
By mist projection granulating-centrifugal granulator recombining process, efficient production controlled, the spherical roundness of 50～500 μ m particle diameters good, structural strength is high, density is greater than 1.8g/cm
3, the function ingredients adjustable ratio ultra-fine boron powder dense spherical coacervate, a difficult problem such as preparation efficiency is low when effectively having avoided routine techniques at the granulation of boron powder class superthin light powder, density is low, nuclei of origin is difficult and granularity is wayward.
Above-mentioned purpose of the present invention realizes that by a kind of preparation method of efficient dense spherical agglomerating particles of ultra-fine boron powder this method comprises the steps:
(1) vacuum drying: ultra-fine boron powder is carried out 70～90 ℃ of vacuum dryings handle, the treatment time is 1～6 hour;
(2) spraying drying prepares parent nucleus: boron powder, binding agent, organic thinner and functional agent after the described processing of step (1) are added in the ball grinding cylinder, the mass ratio of boron powder, binding agent, thinner and functional agent is 100:6～20:100～300:1～15, prepare slip by 3～30 hours roller ball mills, adopt the spray-drying process method to prepare the tiny spherical agglomerated particle of 25～80 μ m;
(3) centrifugal granulating: above-mentioned fine particle is directly served as parent nucleus in the introducing centrifugal granulator after thermofixation is handled,, grow up into the big agglomerating particles of dense spherical gradually by centrifugal granulating;
(4) solidification treatment: the resulting big agglomerating particles of step (3) placed be cured processing in the vacuum drying oven, solidification value is more than 70 ℃, and be 2～4 days set time.
Preferably, the preparation method of the efficient dense spherical agglomerating particles of described ultra-fine boron powder is characterized in that: the described ultra-fine boron powder of step (1) is the amorphous boron powder of particle diameter at 0.1～10 μ m.
Preferably, the preparation method of the efficient dense spherical agglomerating particles of described ultra-fine boron powder is characterized in that: the described binding agent of step (2) is polyurethane prepolymer class binding agent or polyvinyl alcohol; Thinner is ethyl acetate, ethanol, acetone or deionized water; Functional agent is cyanate solidifying agent, silane or Borate Ester as Coupling.
Preferably, the preparation method of the efficient dense spherical agglomerating particles of described ultra-fine boron powder is characterized in that: the described spray drying process of step (2) is centrifugal, pressure type or pneumatic spray drying method.
Preferably, the preparation method of the efficient dense spherical agglomerating particles of described ultra-fine boron powder is characterized in that: the used parent nucleus of the described centrifugal granulating of step (3) is the prepared tiny spherical agglomerated particle of 25～80 μ m of step (2).
Preferably, the preparation method of the efficient dense spherical agglomerating particles of described ultra-fine boron powder is characterized in that: the big reunion grain diameter of preparation is at 50～500 mu m ranges.
The invention still further relates to efficient dense spherical agglomerating particles by the ultra-fine boron powder of method for preparing.
Compared to existing technology, the present invention has following advantage:
(1) it is controlled to utilize spraying drying to prepare grain graininess, good sphericity, and good flowing properties, species distribution is even, is fit to the advantage of mass production, can prepare the tiny spherical agglomerated boron powder particles of 25～80 μ m efficiently;
(2) the fine grain size reunion boron powder particles that adopts spraying drying to prepare serves as parent nucleus supply centrifugal granulating, the final centrifugal granulating that adopts is prepared reunion boron powder, has solved centrifugal granulating and has been difficult to nuclei of origin, the serious and low difficult problem of preparation efficiency of powder loss for ultra-fine boron powder;
(3) pass through to regulate spraying drying and centrifugal granulating technological parameter in the preparation process, can be so that reunion boron powder footpath be controlled, structural strength is high, by adding function ingredients in suitable particle size grating and the coacervate, can promote fiery explosive and propelling agent addition and efficiency of combustion well with the boron powder fuel.
Description of drawings
Figure 1 shows that preparation technology's the route map of a preferred embodiment of the efficient dense spherical agglomerating particles of ultra-fine boron powder of the present invention.
Figure 2 shows that the spraying drying synoptic diagram in the technology shown in Figure 1.
Figure 3 shows that the centrifugal granulating synoptic diagram in the technology shown in Figure 1.
Figure 4 shows that the parent nucleus of preparing by the spraying drying in the method for the present invention.
Figure 5 shows that the spherical agglomerated particle of preparing by method of the present invention.
Description of reference numerals
21 slips
22 hot blasts (mist projection granulating)
23 dedustings
24 discharge ports
31 for powder
32 whitewashings
33 hot blasts (centrifugal granulating).
Embodiment
According to Fig. 1, the present invention at first carries out a certain amount of ultra-fine boron powder vacuum drying and handles, and after the oven dry boron powder is joined in the ball grinding cylinder, adds binding agent, organic thinner and functional agent afterwards in proportion and carries out ball milling slurrying.The purpose of ball milling slurrying is to guarantee that each component thorough mixing of slip of mist projection granulating is even, avoids the part of ultra-fine boron powder to assemble reunion.Prepare the required slip 21 of mist projection granulating behind the ball milling.
Adopt the mist projection granulating method to carry out agglomeration granulation the slip 21 for preparing, control the size and the pattern of agglomeration granulation by the parameters such as import/export temperature, spray velocity and feeding rate of regulating hot blast 22, after dedusting 23, obtain small size particle from discharge port 24.The small size particle that mist projection granulating is prepared serves as the parent nucleus of centrifugal granulating after solidification treatment.
Parent nucleus is added in the centrifugal granulator; by a certain amount of parent nucleus of input on centrifugal turntable; parent nucleus centrifugal force, frictional force and with the baffle plate shock action under; on the fillet surface of rotating disk and entire body, form the particle flux of vortex movement; be the binding agent of jet atomization according to rule at the surface of this particle flux whitewashing 32(simultaneously) and supply powder 31(promptly to supply with powder); and constantly be blown into hot blast 33; parent nucleus is constantly grown up; by control centrifugal granulating parameter, can realize the densification reunion boron powder that controllable granularity, preparation efficiency height, good sphericity and proper sphere degree are high.
Following illustrative example:
Example 1:
(1) the boron powder being carried out 70 ℃ of vacuum dryings handles, treatment time 1-6 hour, at room temperature adopting mass ratio is boron powder: HTPB: ethyl acetate: tolylene diisocyanate=100:20:250:9 prepares burden, adopt roller ball mill mode batch mixing, batch mixing made the spraying slip that satisfies the granulation requirement in 3～5 hours;
(2) based on above-mentioned slip, adopt spraying drying, hot blast turnover/mouth temperature is got 100/70 ℃, and fresh feed pump is selected the input speed of 0.9Kg/h for use, regulate spray velocity and prepare the agglomerating particles of particle diameter, adopt this agglomerating particles to serve as the centrifugal granulating parent nucleus at 40～60 μ m;
(3), adopt the centrifugal granulation granulation, by regulating rotating speed, binding agent flow, regulating final agglomerating particles size for powder speed based on above-mentioned parent nucleus.
Performance test:
1, utilize scanning electronic microscope (SEM) that the reunion boron powder of preparation is observed, the parent nucleus that spraying drying is prepared is seen accompanying drawing 4, and the reunion boron powder particles of preparing is seen accompanying drawing 5.Can find that by SEM figure the reunion boron powder sphericity for preparing is very high, the smooth surface pore-free.
2, ultra-fine boron powder and reunion boron powder are carried out specific surface area, flowing property and loose density contrast, test result sees Table 1.
Performance comparison before and after table 1 is reunited
| ? | Loose density (g/cm 3） | Mobile (s/50g) | Specific surface area (m 2/g） |
| Ultra-fine boron powder | 0.21 | Do not have | 55.475 |
| Reunion boron powder | 0.60 | 168.89 | 0.943 |
As seen from Table 1, the reunion boron powder of preparation is compared raw-material ultra-fine boron powder, and loose density promotes nearly 3 times, tangible flowing property has been arranged, and specific surface area reduces effectively.
Example 2:
(1) the boron powder being carried out vacuum drying at 90 ℃ handles, treatment time 1-6 hour, after the oven dry boron powder is placed ball grinding cylinder, the preparation mass ratio is boron powder: HTPB: the mixture of ethyl acetate: hexamethylene-diisocyanate=100:8:250:2.5, adopt roller ball mill mode batch mixing, make the spraying slip that satisfies the granulation requirement;
(2) based on above-mentioned slip, adopt spraying drying, hot blast turnover/mouth temperature is taken at 130/100 ℃, and fresh feed pump is selected the input speed greater than 0.5Kg/h for use, can make the fine grain size agglomerating particles, adopts this agglomerating particles to serve as the centrifugal granulating parent nucleus;
(3), adopt the centrifugal granulation granulation, by regulating rotating speed, binding agent flow, regulating final agglomerating particles size for powder speed based on above-mentioned parent nucleus.
Performance test:
1, the boron powder before and after reuniting is carried out the boron content measuring, test result sees Table 2.
Boron content contrast before and after table 2 is reunited
| ? | Effective boron content (%) |
| Ultra-fine boron powder | 95.475 |
| Reunion boron powder | 85.587 |
As seen from Table 2, the reunion boron powder of preparation is compared raw-material ultra-fine boron powder, and effective boron content slightly descends, but boron content still keeps higher level.
Example 3:
(1) the ultra-fine boron powder that vacuum drying is handled at room temperature adds in the ball grinding cylinder, by mass ratio is the boron powder: polyvinyl alcohol: deionized water: silane coupling agent KH-560=100:20:300:2.5 adds in ball grinding cylinder, adopt roller ball mill mode batch mixing, batch mixing made the spraying slip that satisfies the granulation requirement in 5 hours;
(2) based on above-mentioned slip, adopt spraying drying, hot blast turnover/mouth temperature is taken at 140/120 ℃, fresh feed pump is selected the input speed of 0.8Kg/h for use, can make the fine grain size agglomerating particles, the reunion boron powder particles of preparation is carried out the vacuum solidification processing, adopt this reunion boron powder particles to serve as the centrifugal granulating parent nucleus;
(3), adopt the centrifugal granulation granulation, by regulating rotating speed, binding agent flow, regulating final agglomerating particles size for powder speed based on above-mentioned parent nucleus.
Ultra-fine boron powder and reunion boron powder are carried out than the flowing property contrast, and test result sees Table 3.
Flowing property contrast before and after table 3 is reunited
| ? | Mobile (s/50g) |
| Ultra-fine boron powder | Do not have |
| Reunion boron powder | 178.92 |
As seen from Table 3, the reunion boron powder of preparation is compared raw-material ultra-fine boron powder, and the good mobility energy is arranged.
Claims (7)
1. the preparation method of the efficient dense spherical agglomerating particles of a ultra-fine boron powder is characterized by, and may further comprise the steps:
(1) vacuum drying: ultra-fine boron powder is carried out 70～90 ℃ of vacuum dryings handle, the treatment time is 1～6 hour;
(2) spraying drying prepares parent nucleus: the boron powder after the described processing of step (1) is added in the ball grinding cylinder, add binding agent, thinner and functional agent in proportion, the mass ratio of boron powder, binding agent, thinner and functional agent is 100:6～20:100～300:1～15, prepare slip by 3～30 hours roller ball mills, adopt the spray-drying process method to prepare the tiny spherical agglomerated particle of 25～80 μ m;
(3) centrifugal granulating: above-mentioned tiny spherical agglomerated particle is directly served as parent nucleus in the introducing centrifugal granulator after thermofixation is handled,, form the big agglomerating particles of dense spherical through centrifugal granulating;
(4) solidification treatment: the resulting big agglomerating particles of step (3) placed be cured processing in the vacuum drying oven, solidification value is more than 70 ℃, and be 2～4 days set time.
2. the preparation method of the efficient dense spherical agglomerating particles of ultra-fine boron powder according to claim 1 is characterized in that: the described ultra-fine boron powder of step (1) is the amorphous boron powder of particle diameter at 0.1～10 μ m.
3. the preparation method of the efficient dense spherical agglomerating particles of ultra-fine boron powder according to claim 1 is characterized in that: the described binding agent of step (2) is polyurethane prepolymer class binding agent or polyvinyl alcohol; Thinner is ethyl acetate, ethanol, acetone or deionized water; Functional agent is cyanate solidifying agent, silane coupling agent or Borate Ester as Coupling.
4. the preparation method of the efficient dense spherical agglomerating particles of ultra-fine boron powder according to claim 1 is characterized in that: the described spray drying process of step (2) is centrifugal, pressure type or pneumatic spray drying method.
5. the preparation method of the efficient dense spherical agglomerating particles of ultra-fine boron powder according to claim 1 is characterized in that: the described centrifugal granulating parent nucleus of step (3) is the prepared tiny spherical agglomerated particle of 25～80 μ m of step (2).
6. the preparation method of the efficient dense spherical agglomerating particles of ultra-fine boron powder according to claim 1 is characterized in that: the big reunion grain diameter of preparation is at 50～500 mu m ranges.
7. the efficient dense spherical agglomerating particles of a ultra-fine boron powder, it is prepared by any preparation method among the claim 1-6.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104607102A (en) * | 2014-12-23 | 2015-05-13 | 江苏金石研磨有限公司 | A manufacturing method of a high-strength small-size mill ball |
| CN105328200A (en) * | 2014-07-15 | 2016-02-17 | 昆山玛冀电子有限公司 | Atomization pelleting method for soft magnetic powder |
| CN106348308A (en) * | 2016-08-31 | 2017-01-25 | 赵放 | High-melting-point metal powder, solid propellant and process for preparing same by using boron powder |
| CN108586177A (en) * | 2018-05-04 | 2018-09-28 | 北京理工大学 | A method of improving activity Ti/2B nano-powders and explosive compatibility |
| CN110041080A (en) * | 2019-05-24 | 2019-07-23 | 丹东市化工研究所有限责任公司 | A method of preparing near-spherical hexagonal boron nitride agglomerated particle |
| CN114751733A (en) * | 2022-04-25 | 2022-07-15 | 中国振华集团云科电子有限公司 | Production method of spherical ceramic filler with low temperature coefficient |
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| CN101734680A (en) * | 2009-12-14 | 2010-06-16 | 武汉理工大学 | Method for preparing spherical amorphous boron powder by spray drying method |
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| CN101531556A (en) * | 2009-04-24 | 2009-09-16 | 西安近代化学研究所 | Method for granulating amorphous boron powder |
| CN101734680A (en) * | 2009-12-14 | 2010-06-16 | 武汉理工大学 | Method for preparing spherical amorphous boron powder by spray drying method |
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|---|---|---|---|---|
| CN105328200A (en) * | 2014-07-15 | 2016-02-17 | 昆山玛冀电子有限公司 | Atomization pelleting method for soft magnetic powder |
| CN104607102A (en) * | 2014-12-23 | 2015-05-13 | 江苏金石研磨有限公司 | A manufacturing method of a high-strength small-size mill ball |
| CN106348308A (en) * | 2016-08-31 | 2017-01-25 | 赵放 | High-melting-point metal powder, solid propellant and process for preparing same by using boron powder |
| CN106348308B (en) * | 2016-08-31 | 2018-12-11 | 赵放 | High-melting metal powder, solid propellant and its with boron powder preparation technique |
| CN108586177A (en) * | 2018-05-04 | 2018-09-28 | 北京理工大学 | A method of improving activity Ti/2B nano-powders and explosive compatibility |
| CN108586177B (en) * | 2018-05-04 | 2020-10-02 | 北京理工大学 | Method for improving compatibility of active Ti/2B nano powder and explosive |
| CN110041080A (en) * | 2019-05-24 | 2019-07-23 | 丹东市化工研究所有限责任公司 | A method of preparing near-spherical hexagonal boron nitride agglomerated particle |
| CN114751733A (en) * | 2022-04-25 | 2022-07-15 | 中国振华集团云科电子有限公司 | Production method of spherical ceramic filler with low temperature coefficient |
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