CN101531556B - Method for granulating amorphous boron powder - Google Patents
Method for granulating amorphous boron powder Download PDFInfo
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- CN101531556B CN101531556B CN2009100221978A CN200910022197A CN101531556B CN 101531556 B CN101531556 B CN 101531556B CN 2009100221978 A CN2009100221978 A CN 2009100221978A CN 200910022197 A CN200910022197 A CN 200910022197A CN 101531556 B CN101531556 B CN 101531556B
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Abstract
The invention discloses a method for granulating amorphous boron powder, and in particular relates to a method for kneading and granulating amorphous boron powder for fuel-rich propellant. The method for granulating amorphous boron powder comprises the following steps: (1) premixing ethyl acetate, liquid polyurethane adhesive prepolymer, isocyanate curing agents and curing catalyst well according to a mass ratio which is 40-50:8-9:1-2:0.1-0.05 and controlling material temperature to between 35 and 40 DEG C; (2) mixing the amorphous boron powder with the premixed material; and (3) passing the obtained granular material through a 30-mesh standard sieve and drying the obtained granular material. In the process of granulating the amorphous boron powder, the method adopts the ethyl acetate which has little harm to environment and low dosage as a solvent for dispersing adhesive, and adopts a star-type stirring paddle to ensure that agglomerate mixtures can be denser under the cutting and extruding action of the stirring paddle. Granules obtained by the method are high in strength, are not easy to break when the granules are applied in formulations of fuel-rich propellant, and enable medicine pulp to be low in yield value and apparent viscosity.
Description
Technical field
The present invention relates to a kind of method for granulating amorphous boron powder, refer more particularly to the kneading prilling process of fuel-rich propellant with 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 propelling agent that solid rocket ramjet adopts is a fuel-rich propellant.Boron not only has very high mass-burning calorific value and volume calorific value as a kind of fuel, and its products of combustion 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 acidic impurities, its pH of suspension value of reported in literature reaches 4.0～4.5.Crosslinking reaction easily takes place in the hydroxyl of this acidic impurities and hydroxy-terminated polybutadienes commonly used (HTPB) tamanori 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 height, being difficult to fusing and gasification, its burning is the surface oxidation process, thereby the ignition characteristic of boron powder and combustionproperty are poor, and combustion speed and burning rate pressure exponent are low, and engineering application difficulty is big.So amorphous boron powder need be handled, to guarantee the processing performance and the combustionproperty of propelling agent.
Be processing performance and the combustionproperty of improving the boracic fuel-rich propellant, mainly studied two kinds of methods of surperficial coating and agglomeration granulation both at home and abroad.It is one of important method of handling of boron powder that the surface coats, because suitable coating can improve technology, igniting and the burning of propelling agent, the coating that is used to improve ignition has GAP (Racemic glycidol nitrine polyethers), NaN
3, LiF, Ti, B
4C, Mg etc., the coating that improves processing performance has AP (ammoniumper chlorate), Viton A (viton), TDI (tolylene diisocyanate), alcohols, silane etc.Though the surface coats technology and the combustionproperty that can to a certain degree improve propelling agent, the granularity of Boron Coated powder is little, and specific surface area is big, and the add-on 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, it is the steps necessary that boracic fuel-rich propellant starting material are handled that the boron powder is carried out granulation.In the present known amorphous boron powder prilling process; United States Patent (USP) 3646174 was once reported a kind of technology of amorphous boron powder agglomeration granulation; this method is with the 100g amorphous boron powder; CTPB tamanori prepolymer; (Freon 113 to be dissolved in the volatile Freon 113 of 125mL for solidifying agent and curing catalysts (6g altogether); Freon 113); 48 ℃ of heating; take out and stir 10min under the certain vacuum; continuously stirring 15min under 266Pa～400Pa vacuum tightness then; after being interrupted stirring, can obtain spherical agglomerated particle; and Freon 113 removes in the whole volatilizations of granulation process; the boron powder is solidified 18h with CTPB mixing gained particle at 71 ℃; obtain final granulating boron powder; wherein, (particle of 0.99mm～0.295mm) accounts for 95% of total mass to the 16-48 order.This method can prepare granular boron powder, but a large amount of the use has the hydrochloric ether of destruction to make solvent to atmospheric ozone layer, and chlorinated hydrocarbon solvent directly is thrown into air, can't reclaim, and belongs to the great processing method of environmental disruption; It is wide that gained granulating boron powder degree distributes, and the primary combustion ejection efficiency is low, secondary combustion is difficult to igniting and abundant problem such as burning and macrobead boron powder exists, no actual application value, so the yield rate of this method is low.
Summary of the invention
The kneading prilling process of the amorphous boron powder that the purpose of this invention is to provide that a kind of technological process is little to environmental hazard, boron powder degree is easy to control, yield rate is high is to overcome the deficiencies in the prior art.
Implementation procedure of the present invention is as follows:
Method for granulating amorphous boron powder may further comprise the steps:
(1) ethyl acetate, liquid polyurethane tamanori prepolymer, isocyanates solidifying agent and curing catalysts are pressed mass ratio 40～50: 8～9: 1～2: 0.1～0.05 premix is even, and the control temperature of charge is 35～40 ℃;
(2) amorphous boron powder of 10～13 times of polyurethane adhesives prepolymer quality is added in the above-mentioned Preblend mix, amorphous boron powder is taked the batch charging mode, add for the 1st time 70%, the 2 time of boron powder total mass add 20%, the 3 time of boron powder total mass add remaining 10%.
(3) the gained granular material is crossed 30 mesh standard sieves after, macrobead boron powder crushing, force down screen cloth, all materials are added in kneading pots mediate 10min, afterwards at 70 ℃ of temperature dryings.
The polyurethane adhesives prepolymer refers to that a class contains the polymkeric substance of carbamate groups in molecule, is polymerized by multi-hydroxy compound and multicomponent isocyanate based compound.Liquid polyurethane tamanori prepolymer of the present invention is hydroxy-terminated polybutadienes (HTPB) or polyoxyethylene glycol-tetrahydrofuran copolymer (PET).Described isocyanates solidifying agent is tolylene diisocyanate (TDI), isoflurane chalcone diisocyanate (IPDI) or polyisocyanates (N-1OO); Described curing catalysts is triphenyl bismuth (TPB).
Amorphous boron powder is taked the batch charging mode, for the first time add the boron powder after, will form a kind of doughy mix with liquid ingredient, shearing, extruding by stirring rake can make material more closely knit, tap density can improve; For the second time, added boron powder plays dissemination for the third time, will make agglomerating material progressively be dispersed into small-particle, becomes the granularity that meets the demands under the final constantly stirring.
Being blended in the vertical kneader of the method for the invention material carried out, and vertical kneader preferably adopts planetary stirring rake.
Advantage of the present invention is as follows:
(1) granulation process of amorphous boron powder of the present invention adopts ethyl acetate as the solvent that disperses tamanori, and it is little to environmental hazard, and consumption is few, and the quantity of solvent of every 100g boron powder is 50mL only, and discharge amount of pollution is little, the technological process environmental protection;
(2) in preparation process, the macrobead boron powder that will not possess using value by standard sieve is crushed, and can improve yield rate; Also can reach the purpose of control boron powder degree by sieving;
(3) because vertical kneader adopts is planetary stirring rake, between the stirring rake, with the pot wall the gap little, can not only guarantee that material is uniformly dispersed, and agglomerating mixture can be more closely knit under the shearing of stirring rake, extruding, the gained granule strength is big, non-friable when in the fuel-rich propellant prescription, using, make the yield value and the apparent viscosity of medicine slurry less.
Adopt the present invention that amorphous boron powder is carried out granulation and handle, the amorphous boron powder particles below 50 orders and distilled water are configured to suspension by 5: 100 mass ratio, surveying its pH value is 7.1～7.4; Above-mentioned amorphous boron powder particles mixes with 6: 4 mass ratio with HTPB, is respectively 76.5Pa and 51.4Pas at the yield value and the apparent viscosity of 50 ℃ of following mixtures, does not increase in time; Contain the interior apparent viscosity of above-mentioned amorphous boron powder particulate fuel-rich propellant medicine slurry 5h less than 1500Pas, working life is longer.
Embodiment
The used amorphous boron powder of the present invention, HTPB, PET, TDI, IPDI, N-1OO, TPB, ethyl acetate etc. are market and buy chemical.
Method for granulating amorphous boron powder of the present invention may further comprise the steps:
1, in the kneading pot of vertical kneader, add ethyl acetate successively, the polyurethane adhesives prepolymer, isocyanates solidifying agent and curing catalysts, ethyl acetate, liquid polyurethane tamanori prepolymer, isocyanates solidifying agent and curing catalysts are pressed mass ratio 40～50: 8～9: 1～2: 0.1～0.05, wherein the polyurethane adhesives prepolymer is hydroxy-terminated polybutadienes (HTPB) or polyoxyethylene glycol-tetrahydrofuran copolymer (PET), and the isocyanates solidifying agent is tolylene diisocyanate (TDI), isoflurane chalcone diisocyanate (IPDI) or polyisocyanates (N-1OO); 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 ℃, crosslinking reaction can not fully take place in polyurethane adhesives prepolymer and isocyanates solidifying agent, but temperature is higher than 40 ℃, and ethyl acetate will be volatilized fast, is difficult to make amorphous boron powder fully to soak into.
2, amorphous boron powder was divided 3 steps added in the solution of step a, add 70% of boron powder total mass for the 1st time, begin to mediate after premix is even, all kneading processes control rotating speed of agitator are 20～25r/min, stop to mediate the material on cleaning stirring rake and the pot wall behind the 30min; Add 20% of boron powder total mass the 2nd time in kneading pot, mediate 10min behind the premix, stop then mediating, the material on slurry and the pot wall is mediated in cleaning; Add 10% of boron powder total mass the 3rd time in kneading pot, mediate 20min behind the premix, stop then mediating, 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, particulate materials is crossed screen sizing, screen cloth is crushed, forced down to large granular materials, all materials are added kneading pot, stop behind the kneading 10min, this mixing process can be driven away the burr of particle surface, make particle more smooth, improve favourable the processing performance of medicine slurry; Pour the gained granular material into charging tray at last, dry 72h under 70 ℃ of temperature obtains the purpose product.
For short grained boron powder is bonded to macrobead by tamanori, in propelling agent sample kneading preparation process, find: when the mass ratio of solid packing and liquid adhesive component reaches 9: 1 left and right sides, because the tamanori component concentration is few, progressively adding along with solid packing, Composite Propellant Slurry is progressively become by flow state and is difficult to mobile medicine group, if further add solid packing, medicine group and filler will form the dispersive small-particle under the shearing of stirring rake, extruding, these small-particles can progressively be rolled into microsphere under the rotation of stirring rake.According to above-mentioned experimental phenomena, select HTPB tamanori prepolymer as agglomerator, HTPB and isocyanates solidifying agent are reacted in solution form lattice chain, adding the part amorphous boron powder then mediates agglomerating, the boron powder is adsorbed between the lattice chain, volatilization along with increase of boron powder add-on and solvent, agglomerating mixture is dispersed into little fast and small-particle under the shearing of stirring rake, these small-particles progressively form spherical small-particle at rolling process, make solvent evaporates at last, the HTPB lattice chain solidifies the back and becomes the microsphere with certain intensity with the boron powder, 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 the 50ml ethyl acetate successively, 9.40g HTPB tamanori prepolymer (hydroxyl value: 0.67mmol/g), 0.60g TDI solidifying agent and 0.1gTPB curing catalysts, even with the bamboo chip premix, start heating circulation system, temperature of charge was 40 ℃ during control was mediated.Divided for 3 steps added in the kneading pot amorphous boron powder (B content is 92%, and granularity is 1 μ m), the 1st adding 70g, 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 stirring rake and the pot wall behind the 30min; Add 20g boron powder the 2nd time in kneading pot, mediate 10min behind the premix, stop then mediating, the material on slurry and the pot wall is mediated in cleaning; In kneading pot, add 10g boron powder the 3rd time, mediate 20min behind the premix, stop then mediating; 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, particulate materials is crossed screen sizing; 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; dry 72h under 70 ℃ of temperature obtains granular boron powder.Performance test
1.pH test
Testing tool is a PHS-25 digital display pH meter.
Testing method: amorphous boron powder and distilled water are configured to suspension by 5: 100 mass ratio, stir evenly the pH value of back test suspension liquid, and contrast with untreated amorphous boron powder raw material under the same conditions, and test result sees Table 1.
2.B/HTPB mixture rheology testing
Testing tool is the RS-300 rheometer.
Testing method: HTPB tamanori and amorphous boron powder are configured to uniform mixture by 6: 4 mass ratio, test b/HTPB mixture rheological property behind 50 ℃ of insulation 0.5h, the result is 10s with the yield value and the shearing rate of mixture
-1The time apparent viscosity represent.Contrast with untreated amorphous boron powder raw material under the same conditions, test result sees Table 1:
The performance of table 1 amorphous boron powder
| The sample title | pH | Yield value (Pa) | Apparent viscosity (Pas) |
| The amorphous boron powder raw material | 5.13 | 85.3 | ?64.5 |
| Amorphous boron powder is handled in granulation | 7.32 | 76.5 | ?51.4 |
By above-mentioned performance test data as seen, the amorphous boron powder that this prilling process obtains is because granularity increases, and specific surface area reduces, the B of particle surface
2O
3, H
3BO
3Significantly reduce Deng acidic impurities, simultaneously the polyurethane adhesives in the particle has played the coating effect to the boron powder, thereby granulation handles the demonstration neutrality of amorphous boron powder, and reduces with the yield value and the apparent viscosity of HTPB mixture.
3. the application in propelling agent
The processing amorphous boron powder that embodiment 1 obtains has carried out the specimen 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 compositepropellent method for making sample, the results are shown in Table 2.
Under the identical propellant formulation and processing condition, obviously change is glutinous mediating beginning process Chinese medicine slurry for the amorphous boron powder that is untreated, and crosslinking reaction takes place, and Composite Propellant Slurry can't be mediated.
The apparent viscosity of table 2 Composite Propellant Slurry is trend over time
| Mixing time (h) | Apparent viscosity (Pas) |
| ?1 | 1251 |
| ?2 | 1305 |
| ?3 | 1364 |
| ?4 | 1442 |
| ?5 | 1547 |
Studies show that use the amorphous boron powder of granulation in propelling agent, the apparent viscosity of propelling agent is low, processing performance satisfies the casting requirement.
Embodiment 2
This routine implementation method and example 2 are basic identical, and different is that the tamanori prepolymer adopts polyoxyethylene glycol-tetrahydrofuran copolymer (PET), and consumption is 9.10g, and solidifying agent adopts N-100, and consumption is 0.90g.
Performance test
Testing tool and testing method the results are shown in following table 3 with embodiment 1.
The performance of table 3 amorphous boron powder
| The sample title | pH | Yield value (Pa) | Apparent viscosity (Pas) |
| The amorphous boron powder raw material | 5.13 | 85.3 | ?64.5 |
| Amorphous boron powder is handled in granulation | 7.21 | 72.7 | ?50.1 |
Embodiment 3
This routine implementation method and example 1 are basic identical, and different is that solidifying agent adopts IPDI, and consumption is 0.70g, and the HTPB consumption is 9.30g.
Performance test
Testing tool and testing method the results are shown in following table 4 with embodiment 1.
The performance of table 4 amorphous boron powder
| The sample title | pH | Yield value (Pa) | Apparent viscosity (Pas) |
| The amorphous boron powder raw material | 5.13 | 85.3 | ?64.5 |
| Amorphous boron powder is handled in granulation | 7.35 | 75.4 | ?52.7 |
Claims (6)
1. method for granulating amorphous boron powder may further comprise the steps:
(1) it is even ethyl acetate, liquid polyurethane tamanori prepolymer, isocyanates solidifying agent and curing catalysts to be pressed mass ratio 40～50:8～9:1～2:0.1～0.05 premix, and the control temperature of charge is 35～40 ℃;
(2) amorphous boron powder of 10～13 times of polyurethane adhesives prepolymer quality is added in the above-mentioned Preblend mix, amorphous boron powder is taked the batch charging mode, add for the 1st time 70%, the 2 time of boron powder total mass add 20%, the 3 time of boron powder total mass add remaining 10%;
(3) the gained granular material is crossed 30 mesh standard sieves after, macrobead boron powder crushing, force down screen cloth, all materials are added in kneading pots mediate 10min, afterwards at 70 ℃ of temperature dryings.
2. method for granulating amorphous boron powder according to claim 1 is characterized in that: the polyurethane adhesives prepolymer is hydroxy-terminated polybutadienes or polyoxyethylene glycol-tetrahydrofuran copolymer.
3. method for granulating amorphous boron powder according to claim 1 is characterized in that: the isocyanates solidifying agent is tolylene diisocyanate, isoflurane chalcone diisocyanate or polyisocyanates.
4. method for granulating amorphous boron powder according to claim 1 is characterized in that: curing catalysts is a triphenyl bismuth.
5. according to one of any described method for granulating amorphous boron powder of claim 1 to 4, it is characterized in that: being blended in the vertical kneader of material carried out.
6. method for granulating amorphous boron powder according to claim 5 is characterized in that: vertical kneader adopts planetary stirring rake.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20230093642A1 (en) * | 2021-08-23 | 2023-03-23 | Northrop Grumman Systems Corporation | Methods of passivating fuel materials for use in solid propellants, and related solid fuels, ramjet engines, and methods |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805238A (en) * | 2010-03-23 | 2010-08-18 | 西安近代化学研究所 | Preparation method of high-strength spherical agglomerated boron particles |
| CN102219232B (en) * | 2011-03-30 | 2013-05-01 | 北京矿冶研究总院 | Efficient compact spherical agglomerated particle of superfine boron powder and preparation method thereof |
| CN102989362A (en) * | 2012-12-20 | 2013-03-27 | 西安近代化学研究所 | Efficient granulation method of amorphous boron powder |
| CN103086816B (en) * | 2013-01-28 | 2015-07-15 | 北京矿冶研究总院 | Method for coating metal on surface of agglomerated boron powder |
| CN108892597A (en) * | 2018-07-24 | 2018-11-27 | 西安近代化学研究所 | A kind of method of agglomeration of boron magnesium composite powder |
| CN109824464B (en) * | 2019-02-25 | 2021-04-16 | 江苏智仁景行新材料研究院有限公司 | Preparation method of dispersed boron-magnesium oxide-resistant composite powder |
| CN115108873B (en) * | 2022-06-08 | 2023-06-02 | 西安兰科工控技术有限责任公司 | Granulating method of high-activity nano aluminum powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20230093642A1 (en) * | 2021-08-23 | 2023-03-23 | Northrop Grumman Systems Corporation | Methods of passivating fuel materials for use in solid propellants, and related solid fuels, ramjet engines, and methods |
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