CN108892597A - A kind of method of agglomeration of boron magnesium composite powder - Google Patents
A kind of method of agglomeration of boron magnesium composite powder Download PDFInfo
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- CN108892597A CN108892597A CN201810815637.4A CN201810815637A CN108892597A CN 108892597 A CN108892597 A CN 108892597A CN 201810815637 A CN201810815637 A CN 201810815637A CN 108892597 A CN108892597 A CN 108892597A
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- composite powder
- agglomeration
- added
- ethyl acetate
- boron magnesium
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B29/00—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate
- C06B29/22—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate the salt being ammonium perchlorate
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0033—Shaping the mixture
- C06B21/0066—Shaping the mixture by granulation, e.g. flaking
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B27/00—Compositions containing a metal, boron, silicon, selenium or tellurium or mixtures, intercompounds or hydrides thereof, and hydrocarbons or halogenated hydrocarbons
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
Abstract
It is that there are limitations in order to solve the problems, such as the use of complicated prior art processes process, distilled water and polyethylene glycol the invention discloses a kind of method of agglomeration of boron magnesium composite powder.The method of agglomeration includes the following steps：A. into dispersion cup, hydroxyl-terminated polybutadiene prepolymer, diisocyanate curing agent and T-12 are sequentially added, ethyl acetate is uniformly mixed and obtains suspension；B. LiF, AP and the mixing of part B-Mg composite powder are sequentially added in suspension, in pasty material, residue B-Mg composite powder is added, by vacuumizing after mixing, vacuum degree 60kPa obtains granular material；C. granular material is poured into swing pelletizer, control sieve is 20-30 mesh, by material crushing, forces down sieve, dry materials under sieve are obtained purpose product.
Description
Technical field
The present invention relates to a kind of method of agglomeration of boron magnesium composite powder more particularly to PBX binary explosives, fuel-rich propellant
With the method for agglomeration of B-Mg composite powder.
Background technique
Active metal all has very high quality calorific value and volume calorific value, from the angle of energy and density such as B, Mg, Al
Consider, oxidation reaction calorific value all reached 6-10 times or so of trinitrotoluene, all contained huge chemical energy, can be with
As the high energy material for improving explosive wastewater energy.Due to containing B in amorphous boron powder2O3、H3BO3Equal acid impurities, reported in literature
Its pH of suspension reaches 4.0~4.5.The hydroxyl of the acid impurities and common end hydroxy butadiene (HTPB) binder prepolymer
Reaction easily is crosslinked, increases the viscosity of explosive slurry, processing performance deteriorates, or even can not cast；And the fusing point of boron
With boiling point height, it is difficult to fusing and gasification, burning is surface oxidation process, thus the ignition performance of boron powder and combustibility are poor,
Engineer application difficulty is big.
To improve boron powder technique and burning problem in explosive wastewater application, so that itself and Mg powder is formed B-Mg composite powder, can show
It writes and improves boron fuel burning and technological forming performance.But B-Mg composite powder granularity is smaller, reach 1 micron hereinafter, specific surface area compared with
Greatly, the additional amount in explosive wastewater is also restrained, it is necessary to reunite to the powder, form the particle of certain particle size distribution
Object increases the additional amount in explosive wastewater formula；And in the composite powder, the activity of Mg is higher, the O in easy and air2, vapor etc.
It reacts and inactivates, reunion can ensure that active component is protected inside particle.Currently, there is not yet B-Mg composite powder method of agglomeration
Report, it is known that amorphous boron powder method of agglomeration in, patent 200910022197.8, which is once reported, prepares ball using spray drying process
The method of shape amorphous boron powder, this method comprises the following steps：(1) slurrying：Boron powder and distilled water are pressed 30：70~40：60
Mass ratio is uniformly mixed, and additive, first ultrasonic disperse 15~30 minutes is added by the amount of boron silty amount 2~6%；(2) then magnetic
Power stirs 15~30 minutes, obtains boron slurry material；(3) sodium hydroxide solution is added in boron slurry material, by the pH value of boron slurry material
9~12 are adjusted to, obtains adjusting the boron powder slurry after pH value；(4) it is spray-dried：PH is adjusted to step (3) using spray drying
Boron powder slurry after value is spray-dried；(5) it is dried in vacuo：The spherical boron powder that step (4) is obtained is put into vacuum oven
In, 70~90 DEG C drying 1~2 hour, obtain spherical amorphous boron powder.This method can prepare the boron powder of granulating, but using steaming
Distilled water limits the use of B-Mg composite powder as solvent, because magnesium powder is reacted with water；Reunion processing step up to 5 steps, preparation
Process is complicated, influences the consistency of performance of reunion sample；Use polyethylene glycol as agglomerator, due to polyethylene glycol and terminal hydroxy group
Polybutadiene binder (HTPB) physics is incompatible, the Agglomerated Boron powder for causing the above method to prepare, incompatible with explosive wastewater system.
Summary of the invention
For overcome the deficiencies in the prior art, the present invention provides that a kind of technical process is simple and HTPB binder compatibility
The method of agglomeration of good B-Mg composite powder.
The method of agglomeration of boron magnesium (B-Mg) composite powder provided by the invention, includes the following steps：
A. hydroxyl-terminated polybutadiene prepolymer, isocyanate curing agent, curing catalysts, ethyl acetate are added and are mediated
Machine, 40 DEG C of mixing 20min；
B. be added lithium fluoride, ultrafine ammonium perchlorate and 70% B-Mg composite powder, stirring paddle of kneading machine revolving speed be 20~
Residue B-Mg composite powder is added after 25r/min, 20min, then mediates 30min, kneading process vacuumizes, and vacuum degree 60kPa makes object
Material becomes granular material；
C. stop mediating, gained granular material is poured into swing pelletizer, 20-30 mesh screen is crossed, by screenings 70
DEG C dry 72h, obtains purpose product；
Wherein, in the inventory without ethyl acetate of every 100g, B-Mg composite powder is 80g, polyurethane adhesives pre-polymerization
Object is 10g~15g, and isocyanate curing agent is 0.5~2g, and curing catalysts dibutyl tin dilaurate is 0.05g, lithium fluoride
For 0.5~1.5g, ultrafine ammonium perchlorate is 3~9g, and 50ml~60ml ethyl acetate is added.
Advantages of the present invention：(1) operation of the present invention step is few, and only 3 steps can be completed, and background technique operating procedure is more,
Need 5 steps that could complete altogether；(2) present invention is not reacted, method using ethyl acetate as solvent with boron powder, B-Mg composite powder
Wide adaptability, and background technique using distilled water as solvent, not can be carried out the reunion of B-Mg composite powder；(3) present invention adopts
Use HTPB as reunion binder, prepared agglomerated materials and explosive wastewater Miscibility are preferable, and background technique is using poly-
Ethylene glycol is incompatible as the explosive wastewater system of binder with using HTPB as agglomerator；(4) present invention employs LiF, AP etc. to fire
Promotor is burnt, the burning of reunion material is conducive to, and background technique is then without the technological approaches.
Specific embodiment
Granularity (the d of B-Mg composite powder used in the present invention50) it is 1 μm, Beijing Mine and Metallurgy General Inst produces, and HTPB binder is pre-
Polymers (hydroxyl value：0.67mmol/g), TDI, IPDI, T-12, LiF, AP, ethyl acetate etc. are market purchase chemicals.
Below with reference to embodiment, invention is further described in detail, and the B-Mg composite powder of preparation is 1000g.
Embodiment 1
142.56g HTPB, 7.44g TDI and 0.5g T-12,600ml ethyl acetate are added to the kneading pot of kneader
In, uniformly, the B-Mg composite powder of the ultra-fine AP of 10gLiF, 39.5g (1 μm) and 560g, premix is added in 40 DEG C of mixing 20min to premix
Start to mediate after uniformly, rotating speed of agitator is 20~25r/min, stops mediating after 20min, it is compound that residue 240gB-Mg is added
Powder mediates 30min, and kneading process vacuumizes mixture, and vacuum degree 60kPa makes material eventually become granular material,
Swing pelletizer is poured into, control sieve is 24 mesh, by large granular materials crushing, sieve is forced down, by granular material under sieve
Charging tray is poured into, dry 72h, obtains purpose product at a temperature of 70 DEG C.
1.B/HTPB mixture rheology testing
Test equipment is RS-300 rheometer.HTPB binder and reunion B-Mg composite powder (or amorphous boron powder) are pressed 6：
4 mass ratio is configured to uniform mixture, test b/HTPB mixture rheological property after 50 DEG C of heat preservation 0.5h, as a result with mixing
The yield value and shear rate of body are 10s-1When apparent viscosity indicate.It is compound with the B-Mg of non-aggregated processing under the same conditions
Powder raw material is compared, and test result is shown in Table 1.
The performance of 1 reunion B-Mg composite powder of table
| Sample ID | Yield value (Pa) | Apparent viscosity (Pas) |
| The compound powder raw material of B-Mg | 85.3 | 64.5 |
| Reunion B-Mg composite powder | 45.1 | 30.1 |
2. the application in propellant
The reunion B-Mg composite powder that embodiment 1 obtains has carried out fuel-rich propellant sample preparation, is formulated and is：Reunion B-Mg
Composite powder 40%, HTPB binder system 25%, AP35%.Sample preparation methods according to conventional composite propellant method for making sample,
By mediating, the apparent viscosity in Composite Propellant Slurry 5h is surveyed, the results are shown in Table 2.
Under identical propellant formulation and process conditions, untreated B-Mg composite powder is apparent in kneading starting process Traditional Chinese medicine pulp
Viscosity increases, and mediate Composite Propellant Slurry can not.
The apparent viscosity of 2 Composite Propellant Slurry of table changes with time trend
| Incorporation time (h) | 1 | 2 | 3 | 4 | 5 |
| Apparent viscosity (Pas) | 871 | 905 | 954 | 987 | 1021 |
Embodiment 2
This example implementation method and example 1 are essentially identical, except that HTPB binder prepolymer dosage is 100g, TDI is used
Amount is 5.26g, and ultra-fine AP (1 μm) additional amount is 84.24g.
As a result test method see the table below 3 with embodiment 1.
The performance of 3 reunion B-Mg composite powder of table
| Sample ID | Yield value (Pa) | Apparent viscosity (Pas) |
| The compound powder raw material of B-Mg | 85.3 | 64.5 |
| Reunion B-Mg composite powder | 54.2 | 55.3 |
Claims (3)
1. a kind of method of agglomeration of boron magnesium composite powder, it is characterised in that include the following steps：
A. by hydroxyl-terminated polybutadiene prepolymer, isocyanate curing agent, curing catalysts, ethyl acetate be added kneader, 40
DEG C mixing 20min；
B. be added lithium fluoride, ultrafine ammonium perchlorate and 70% B-Mg composite powder, stirring paddle of kneading machine revolving speed be 20~25r/
Residue B-Mg composite powder is added after min, 20min, then mediates 30min, kneading process vacuumizes, vacuum degree 60kPa, make material at
For granular material；
C. stop mediating, gained granular material is poured into pelletizer, crosses 20-30 mesh screen, by 70 DEG C of screenings dry 72h,
Obtain purpose product；
Wherein, in the inventory without ethyl acetate of every 100g, B-Mg composite powder is 80g, and polyurethane adhesives prepolymer is
10g~15g, isocyanate curing agent are 0.5~2g, and curing catalysts dibutyl tin dilaurate is 0.05g, and lithium fluoride is
0.5~1.5g, ultrafine ammonium perchlorate are 3~9g, and 50ml~60ml ethyl acetate is added.
2. the method for agglomeration of boron magnesium composite powder according to claim 1, it is characterised in that the isocyanate curing agent is
Toluene di-isocyanate(TDI) or isoflurane chalcone diisocyanate.
3. the method for agglomeration of boron magnesium composite powder according to claim 1, it is characterised in that the ultrafine ammonium perchlorate grain
Degree is 1 μm.
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| CN201810815637.4A CN108892597A (en) | 2018-07-24 | 2018-07-24 | A kind of method of agglomeration of boron magnesium composite powder |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
-
2018
- 2018-07-24 CN CN201810815637.4A patent/CN108892597A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 任全彬: "《固体火箭冲压发动机燃烧基础》", 31 July 2016, 国防工业出版社 * |
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