CN102989362A - Efficient granulation method of amorphous boron powder - Google Patents
Efficient granulation method of amorphous boron powder Download PDFInfo
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- CN102989362A CN102989362A CN2012105559978A CN201210555997A CN102989362A CN 102989362 A CN102989362 A CN 102989362A CN 2012105559978 A CN2012105559978 A CN 2012105559978A CN 201210555997 A CN201210555997 A CN 201210555997A CN 102989362 A CN102989362 A CN 102989362A
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Abstract
The invention discloses an efficient granulation method of amorphous boron powder, which comprises the following steps of: uniformly pre-mixing ethyl acetate and thermoplastic adhesive at a mass ratio of (30-60):(6-10); then adding ammonium perchlorate of which the weight is 0-3 times that of the amorphous boron powder and thermoplastic adhesive into the premix, and mixing; and finally processing the granular material with a 30-mesh standard sieve, and drying. According to the invention, the thermoplastic adhesive is used as an adhesive of boron powder and can be easily dispersed to form a solution in an ethyl acetate solvent; and when the solvent is heated and removed, the thermoplastic adhesive is uniformly transferred to the surface of aggregated boron powder particles to form a dense shell layer, thus the particles have relatively high strength, and insufficient strength of the particles caused by incomplete curing of the thermosetting adhesive is avoided. The method disclosed by the invention has short preparation period and high yield, and is convenient for batch production.
Description
Technical field
The present invention relates to a kind of efficient prilling process of amorphous boron powder, refer more particularly to the kneading prilling process that fuel-rich propellant is used amorphous boron powder.
Background technology
The specific impulse of solid rocket ramjet is higher than solid propellant rocket, is a most rising class engine of 21 century.The propellant that solid rocket ramjet adopts is fuel-rich propellant.Boron not only has very high mass-burning calorific value and volume calorific value as a kind of fuel, and its combustion product also has plurality of advantages such as " cleanings ", and the development boron-propellant has caused that at present various countries generally pay attention to.
Owing to contain B in the amorphous boron powder
2O
3, H
3BO
3Deng acid impurities, its pH of suspension value of reported in literature reaches 4.0～4.5.Cross-linking reaction easily occurs in the hydroxyl of this acid impurities and end hydroxy butadiene commonly used (HTPB) binder prepolymer, and the viscosity of Composite Propellant Slurry is increased, and processing performance worsens, even can't cast; And the fusing point of boron and boiling point are high, are difficult to fusing and gasification, and its burning is the surface oxidation process, thereby the ignition performance of boron powder and combustibility are poor, and combustion speed and burning rate pressure exponent are low, and engineering application difficulty is large.So amorphous boron powder need be processed, to guarantee processing performance and the combustibility of propellant.
Be processing performance and the combustibility of improving boron-based fuel-rich, mainly studied two kinds of methods of surperficial coating and agglomeration granulation both at home and abroad.It is one of important method of processing of boron powder that the surface coats, because suitable covering can improve technique, the ignition and combustion of propellant, the covering that is used for improving ignition has GAP(glycidol nitrine polyethers), NaN
3, LiF, Ti, B
4C, Mg etc., the covering that improves processing performance has the AP(ammonium perchlorate), Viton A(fluorubber), the TDI(toluene di-isocyanate(TDI)), alcohols, silane etc.Though the surface coats technique and the combustibility that can to a certain degree improve propellant, the granularity of Boron Coated powder is little, and specific area is large, and the addition of boron powder is difficult to improve, and limited to the raising effect of firing speed and burning rate pressure exponent.
From satisfying the engineering application demand, the boron powder is carried out the steps necessary that granulation is the boron-based fuel-rich raw material disposal.At present in the domestic known amorphous boron powder prilling process, publication number is that the CN10734680A(application number is 200910273247.X) patent of invention reported the method for utilizing spray drying process to prepare spherical amorphous boron powder, the agglomerated particle sphericity of this method preparation, particle dispersion and mobile performance are good, can make the coating of powder and reunite step realization, and particle can keep original proterties, and can realize mass production, be fit to commercial Application, but the Agglomerated Boron powder that the method is produced adopts polyethylene glycol as binder system, because it is inert binder, be unfavorable for that agglomerated boron particles is in the igniting of the cracked and boron particles of combustion process, burning, and this spray-drying agglomeration process process is complicated, and equipment is difficult to cleaning.Publication number is that the CN102219232A(application number is 201110077836.8) patent of invention reported with polyurethane such as HTPB, polyvinyl alcohol and made binding agent; adopt spray drying process to make parent nucleus; then add in the centrifugal granulator constantly whitewashing and for powder, under the effects such as centrifugal force and impact, grow up into gradually the large agglomerated particle of dense spherical.The method can make the controlled Agglomerated Boron powder of aggregated particle size, but polyurethane is inert binder still, is unfavorable for the ignition and combustion of boron powder; This polyurethane is thermosetting adhesive, is difficult to effectively solidify in solid phase, causes agglomerated particle intensity lower; And preparation process is complicated, reaches 30h, is difficult to industry and amplifies.
Chinese invention patent ZL2009100221978 discloses a kind of prilling process of amorphous boron powder, the method adds ethyl acetate, polyurethane adhesives prepolymer, isocyanates curing agent and curing catalysts successively in the kneading pot of vertical kneader, with gained granular material dry 72h under 70 ℃ of temperature, obtain the purpose product at last.The method preparation time is long, is unfavorable for equally large-scale industrialization production.
Summary of the invention
The objective of the invention is to adopt room temperature be solid-state, can promote the thermoplasticity binder of amorphous boron powder burning to make binding agent, provide the efficient prilling process of the amorphous boron powder that a kind of preparation process is simple, the cycle is short, to overcome the deficiencies in the prior art.
Implementation procedure of the present invention is as follows:
A kind of efficient prilling process of amorphous boron powder may further comprise the steps:
(1) 30～60:6～10 premixs are even in mass ratio with ethyl acetate, thermoplasticity binder, and the control temperature of charge is 35～40 ℃;
(2) ammonium perchlorate of amorphous boron powder and 0～3 times of weight of thermoplasticity binder is added in the above-mentioned premix mix;
(3) the gained granular material is crossed 30 mesh standard sieves, drying,
Described thermoplasticity binder is trade mark F-2603 fluorubber or 3,3-, two azido-methyl oxygen fourth ring/3-azido-methyls-3-methyl oxygen fourth ring copolymer BAMO-AMMO.
In the above-mentioned steps (1), 40～50:8～9 premixs are even in mass ratio with ethyl acetate, thermoplasticity binder.
In the above-mentioned steps (2), the amorphous boron powder of 10～15 times of thermoplasticity binder quality added in the above-mentioned premix mix, amorphous boron powder adds in batches, adds 70% of boron powder gross mass the 1st time, add for the 2nd time 20%, the 3 time of boron powder gross mass add remaining 10%.
Amorphous boron powder takes the advantage of batch charging mode to be, for the first time add the boron powder after, will form a kind of doughy mix with liquid component, shearing, extruding by paddle can make material more closely knit, improve bulk density; For the second time, added boron powder plays peptizaiton for the third time, will make agglomerating material progressively be dispersed into granule, the lower granularity that meets the demands that becomes of final constantly stirring.
The granularity of above-mentioned ammonium perchlorate is 1～3 μ m.
In the above-mentioned steps (3), the gained granular material crossed 30 mesh standard sieves after, the crushing of bulky grain boron powder, force down screen cloth, material is mediated 10min afterwards in 70 ℃ of vacuum drying in kneading pot.Being blended in the vertical kneader of material carried out, and vertical kneader preferably adopts planetary paddle.
The thermoplasticity binder refers to that a class vitrification point is higher, room temperature is solid-state polymer.Thermoplasticity binder of the present invention is trade mark F-2603 fluorubber or 3,3-, two azido-methyl oxygen fourth ring/3-azido-methyls-3-methyl oxygen fourth ring copolymer BAMO-AMMO.
Advantage of the present invention and good effect:
(1) the efficient granulation process of amorphous boron powder of the present invention adopts the thermoplasticity binder as the binding agent of boron powder, in ethyl acetate solvent, be easy to be dispersed into solution, add heat abstraction and work as solvent, it will evenly move in Agglomerated Boron powder particles surface, form fine and close shell, make particle have higher intensity, avoided thermosetting adhesive because solidifying the low deficiency of granule strength that not exclusively causes;
(2) the efficient granulation process of amorphous boron powder of the present invention adopts the thermoplasticity binder as the binding agent of boron powder, and the F-2603 combustion decomposition forms fluorine ion, produces HF and B
2O
3The oxide layer reaction rises and drives away B
2O
3The effect of oxide layer, the inner boron particles ignition and combustion of promotion; The BAMO-AMMO combustion decomposition can discharge a large amount of heat, makes boron particles reach sufficiently high temperature and burns, and these two kinds of thermoplasticity binders all have the effect that improves the burning of boron powder;
(3) this method of agglomeration equipment simple, be easy to cleaning, and manufacturing cycle is short, productive rate is high, is convenient to mass production.
The specific embodiment
The used amorphous boron powder of the present invention, fluorubber F-2603, ethyl acetate etc. are market and buy chemicals, 3,3-two azido-methyl oxygen fourth ring/3-azido-methyl-3-methyl oxygen fourth ring copolymers (BAMO-AMMO) are prepared by Liming chemical Inst, number average relative molecular mass 25000, vitrification point-28.3 ℃.
The efficient prilling process of amorphous boron powder of the present invention may further comprise the steps:
1, in the kneading pot of vertical kneader, add successively ethyl acetate, thermoplasticity binder, ethyl acetate and thermoplasticity binder be 30～60:6～10 in mass ratio, wherein the thermoplasticity binder is fluorubber (F-2603) or energetic thermoplastic elastomers 3,3-two azido-methyl oxygen fourth ring/3-azido-methyl-3-methyl oxygen fourth ring copolymers (BAMO-AMMO); Even with the bamboo chip premix, start heating circulation system, temperature of charge was 35～40 ℃ during control was mediated, if temperature is lower than 35 ℃, the molecule segment of thermoplasticity binder is spread apart fully, is difficult to the boron powder that bonds more, but temperature is higher than 40 ℃, ethyl acetate will be volatilized fast, be difficult to make amorphous boron powder fully to infiltrate.
2, in above-mentioned premix, adding respectively is the amorphous boron powder of 10～15 times of solid state heat plastic binder quality and 0～3 times thin AP, take the batch charging mode, 70% and all thin AP that add the amorphous boron powder gross mass for the 1st time, begin to mediate after premix is even, all kneading process control rotating speed of agitator are 20～25r/min, stop to mediate the material on cleaning paddle and the pot wall behind the 20min; Add 20% of amorphous boron powder gross mass the 2nd time, mediate 10min behind the premix, then stop to mediate, the material on slurry and the pot wall is mediated in cleaning; Add for the 3rd time remaining 10%, mediate 20min behind the premix, then stop to mediate, the material on slurry and the pot wall is mediated in cleaning.
3, prepare requirement according to granularity, pour the gained granular material into 30 mesh standard sieves, granular material is crossed sieve classification, screen cloth is crushed, forced down to large granular materials, all materials are added kneading pot, stop behind the kneading 10min, this mixed process can be driven away the burr of particle surface, make particle more smooth, improve favourable to the processing performance of medicine slurry; Pour the gained granular material into charging tray at last, vacuum drying 4h under 70 ℃ of temperature obtains the purpose product.
For short grained boron powder is bonded to bulky grain by binder, in propellant sample kneading preparation process, find: when the mass ratio of solid packing and liquid adhesive component reaches the 9:1 left and right sides, because the binder constituent content is few, progressively adding along with solid packing, Composite Propellant Slurry progressively becomes the medicine group that is difficult to flow by flow regime, if further add solid packing, medicine group and filler will form the granule of dispersion under the shearing of paddle, extruding, these granules can progressively be rolled into spherula under the rotation of paddle.According to above-mentioned experimental phenomena, select HTPB binder prepolymer as agglomerator, HTPB and isocyanates curing agent are reacted in solution form lattice chain, then adding the part amorphous boron powder mediates agglomerating, the boron powder is adsorbed between the lattice chain, volatilization along with the increase of boron powder addition and solvent, agglomerating mixture is dispersed into little fast and granule under the shearing of paddle, these granules progressively form spherical granule at rolling process, make at last solvent evaporates, the HTPB lattice chain solidifies rear and the boron powder becomes the spherula with some strength, thereby reaches the purpose of granulation.
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
In the kneading pot of the vertical kneader of 2L, add successively 50ml ethyl acetate, 7.0g fluorubber (F-2603) dissolves fluorubber with the bamboo chip premix fully, starts heating circulation system, and temperature of charge was 40 ℃ during control was mediated.(B content is 92% with amorphous boron powder, granularity is 1 μ m) divided for 3 steps added in the kneading pot, add 60.2g the 1st time, and the thin AP(granularity of adding 7.0g is 1 μ m), begin to mediate after premix is even, all kneading process control rotating speed of agitator are 20～25r/min, stop to mediate the material on cleaning paddle and the pot wall behind the 20min; Add 17.2g boron powder the 2nd time in kneading pot, mediate 10min behind the premix, then stop to mediate, the material on slurry and the pot wall is mediated in cleaning; In kneading pot, add 8.6g boron powder the 3rd time, mediate 20min behind the premix, then stop to mediate; the material on slurry and the pot wall is mediated in cleaning; prepare requirement according to granularity, pour the gained granular material into 30 mesh standard sieves, granular material is crossed sieve classification; screen cloth is crushed, forced down to large granular materials; all materials are added kneading pot, stop behind the kneading 10min, pour the gained granular material into charging tray; vacuum drying 4h under 70 ℃ of temperature obtains granular boron powder.
Performance test
1, pH test
Tester is PHS-25 digital display pH meter.
Method of testing: amorphous boron powder and distilled water are configured to suspension by the mass ratio of 5:100, stir evenly the pH value of rear test suspension liquid, and contrast with untreated amorphous boron powder raw material under the same conditions, and test result sees Table 1.
2, fire trial
Adopt CO
2Laser Ignition System under the test parameters of hot spot 5mm, wavelength 10.6 μ m, has been tested when the laser ignition energy is 23W and different the reunion has been processed the ignition-delay period of sample, the results are shown in Table 1.
3, B/HTPB mixture rheology testing
Process amorphous boron powder with the HTPB granulation and be contrast, tester is the RS-300 flow graph.
Method of testing: HTPB binder and amorphous boron powder are configured to uniform mixture by the mass ratio of 6:4, test b/HTPB mixture rheological property behind 50 ℃ of insulation 0.5h, the result is take the yield value of mixture and shear rate as 10s
-1The time apparent viscosity represent.Use with this patent same procedure Agglomerated Boron powder as binding agent and contrast with untreated amorphous boron powder raw material, employing HTPB under the same conditions, test result sees Table 1.
By above-mentioned performance test data as seen, the amorphous boron powder that this prilling process obtains is because granularity increases, and specific area reduces, the B of particle surface
2O
3, H
3BO
3Significantly reduce Deng acid impurities, simultaneously the fluorubber binder in the particle has played coating function to the boron powder, thus granulation to process the demonstration of amorphous boron powder neutral, and reduce with yield value and the apparent viscosity of HTPB mixture; Fire trial shows that obviously shorten the period of delay that amorphous boron powder is processed in the fluorubber granulation, and ignition performance improves.
4, the application in propellant
The processing amorphous boron powder that embodiment 1 obtains has carried out the sample preparation of fuel-rich propellant prescription, and filling a prescription is: the amorphous boron powder 35% of granulation, HTPB binder system 27%, AP32%, Mg-Al alloy 6%.Sample preparation methods through mediating, is surveyed the apparent viscosity in this Composite Propellant Slurry 5h according to conventional composite propellant method for making sample, the results are shown in Table 2.
Under the identical propellant formulation and process conditions, obviously change is glutinous mediating beginning process Traditional Chinese medicine pulp for the amorphous boron powder that is untreated, and cross-linking reaction occurs, and Composite Propellant Slurry can't be mediated.
Studies show that use the amorphous boron powder of granulation in propellant, the apparent viscosity of propellant is low, processing performance satisfies the casting requirement.
Embodiment 2
Similar to Example 1, different is that the thermoplasticity binder is 3,3-, two azido-methyl oxygen fourth ring/3-azido-methyl-3-methyl oxygen fourth ring copolymers (BAMO-AMMO).
Performance test
Tester and method of testing the results are shown in following table 3 with embodiment 1.
Embodiment 3
Similar to Example 1, different is that the fluorubber consumption is 9.0g.
Performance test
Tester and method of testing the results are shown in following table 4 with embodiment 1.
Claims (8)
1. the efficient prilling process of an amorphous boron powder is characterized in that may further comprise the steps:
(1) 30～60:6～10 premixs are even in mass ratio with ethyl acetate, thermoplasticity binder, and the control temperature of charge is 35～40 ℃;
(2) ammonium perchlorate of amorphous boron powder and 0～3 times of weight of thermoplasticity binder is added in the above-mentioned premix mix;
(3) the gained granular material is crossed 30 mesh standard sieves, drying,
Described thermoplasticity binder is trade mark F-2603 fluorubber or 3,3-, two azido-methyl oxygen fourth ring/3-azido-methyls-3-methyl oxygen fourth ring copolymer.
2. the efficient prilling process of amorphous boron powder according to claim 1, it is characterized in that: in the step (1), 40～50:8～9 premixs are even in mass ratio with ethyl acetate, thermoplasticity binder.
3. the efficient prilling process of amorphous boron powder according to claim 1 is characterized in that: in the step (2), the amorphous boron powder of 10～15 times of thermoplasticity binder quality added in the above-mentioned premix mix.
4. the efficient prilling process of amorphous boron powder according to claim 3, it is characterized in that: amorphous boron powder adds in batches, add for the 1st time 70%, the 2 time of boron powder gross mass add 20%, the 3 time of boron powder gross mass add remaining 10%.
5. the efficient prilling process of amorphous boron powder according to claim 1, it is characterized in that: the granularity of ammonium perchlorate is 1～3 μ m.
6. according to claim 1 to the efficient prilling process of 5 one of any described amorphous boron powders, it is characterized in that: in the step (3), after the gained granular material crossed 30 mesh standard sieves, screen cloth is crushed, forced down to bulky grain boron powder, and material is mediated 10min afterwards in 70 ℃ of vacuum drying in kneading pot.
7. the efficient prilling process of amorphous boron powder according to claim 6, it is characterized in that: being blended in the vertical kneader of material carried out.
8. the efficient prilling process of amorphous boron powder according to claim 7, it is characterized in that: vertical kneader adopts planetary paddle.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108456123A (en) * | 2018-02-09 | 2018-08-28 | 张晓成 | High-energy agent preparation method, high-energy agent and pyrotechnic composition and its firecracker Safe production method |
| CN110975749A (en) * | 2019-12-02 | 2020-04-10 | 山东益丰生化环保股份有限公司 | Method for granulating powder thiourea |
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| CN108456123A (en) * | 2018-02-09 | 2018-08-28 | 张晓成 | High-energy agent preparation method, high-energy agent and pyrotechnic composition and its firecracker Safe production method |
| CN110975749A (en) * | 2019-12-02 | 2020-04-10 | 山东益丰生化环保股份有限公司 | Method for granulating powder thiourea |
| CN110975749B (en) * | 2019-12-02 | 2021-11-02 | 山东益丰生化环保股份有限公司 | Method for granulating powder thiourea |
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Application publication date: 20130327 |