Claims
- 1. A method for preparing a solid propellant mixture of aggregated oxidant and fuel particles in a binder, comprising the steps of:
- (a) admixing solid particles in a solution of the binder in a mixing container equipped with a variable-speed impeller and a countersolvent supply system, wherein the solid particles have a size smaller than a desired particle size of the aggregated particles;
- (b) adding a first countersolvent portion to the admixture of step (a) while maintaining agitation; wherein the first countersolvent portion is less than or about equal to an amount needed for coacervation without effecting coacervation;
- (c) while agitating with the impeller, metering a second countersolvent portion from the countersolvent supply system into the mixture of step (b) to exceed the countersolvent-solvent ratio required for coacervation to precipitate the binder and form aggregated particles, wherein a countersolvent metering rate and impeller speed are matched to obtain the desired particle size distribution of the aggregated particles;
- (d) admixing excess countersolvent into the mixture from step (c) while maintaining agitation with the impeller;
- (e) maintaining agitation of the mixture from step (d) for a period of time to allow the binder in the aggregated particles to harden;
- (f) optionally rinsing the hardened aggregated particles from step (e) with additional countersolvent.
- 2. The method of claim 1 wherein the solid particles comprise an oxidant and a fuel.
- 3. The method of claim 2 wherein the particles comprise zirconium and potassium perchlorate.
- 4. The method of claim 1 wherein the binder comprises an elastomer.
- 5. The method of claim 4 wherein the elastomer is a terpolymer of hexafluoropropylene, vinylidene fluoride and tetrafluoroethylene.
- 6. The method of claim 1 wherein steps (a) and (b) include the sequential steps of charging the mixing container with the binder solution, fuel particles, optional processing aids, and a countersolvent preload comprising all or part of the first countersolvent portion, mixing the contents of the mixing container, and while maintaining mixing of the mixing container, adding a charge of oxidant particles to the mixing container.
- 7. The method of claim 6 wherein the oxidant particle charge addition, countersolvent metering step (b) and excess countersolvent admixing step (c) are remotely actuated.
- 8. The method of claim 1 including empirically determining the coacervation point for the countersolvent-solvent system as a function of temperature and estimating the countersolvent ratio of the coacervation point for step (b) based on the empirical determination.
- 9. The method of claim 8 wherein step (b) includes the sequential steps of adding a preload of countersolvent to within about 20 percent of the countersolvent-solvent ratio of the coacervation point to avoid coacervation, allowing the admixture to thermally equilibrate, measuring the temperature of the admixture, and calculating the countersolvent-solvent ratio needed for coacervation at the measured temperature, and then adding the second countersolvent portion to the admixture in step (c) to exceed the calculated ratio of countersolvent to solvent.
- 10. The method of claim 9 wherein the countersolvent metering rate in step (c) is relatively slower than a rate of countersolvent addition in step (b).
- 11. The method of claim 9 including terminating the countersolvent metering of step (c) and maintaining agitation of the mixture with the impeller for a period of time effective to aggregate the particles to the desired particle size distribution prior to step (d).
- 12. The method of claim 1 wherein the rinsing step (f) includes stopping agitation of the mixture and allowing the aggregated particles to settle, decanting supernatant and adding additional countersolvent.
- 13. The method of claim 1 wherein the countersolvent supply system includes first and second countersolvent supply modes, wherein the first mode has a high countersolvent flow rate for steps (b) or (d) relative to a low countersolvent flow rate of the second mode for step (c).
- 14. The method of claim 13 wherein the countersolvent supply system includes a first flow path for delivering countersolvent to the mixing container at the relatively high flow rate of the first countersolvent supply mode, and a second countersolvent flow path in parallel with the first flow path for delivering countersolvent to the mixing container at the relatively low flow rate of the second countersolvent supply mode.
- 15. The method of claim 14 wherein the countersolvent supply system includes a valve in a countersolvent flow path operable in a continuously open mode delivering countersolvent to the mixing container at the relatively high flow rate of the first countersolvent supply mode, and operable in a pulsed open and closed mode at a frequency selected to provide the relatively low flow rate of the second countersolvent supply mode.
- 16. The method of claim 12 wherein the rinsing step (f) further includes comparing the mixing container weight with a remote sensor before and after the decantation step to confirm removal of the supernatant liquid.
- 17. The method of claim 16 wherein the rinsing step (f) further includes comparing the mixing container weight before and after the additional countersolvent addition to confirm the countersolvent addition, and stirring the mixing container with the impeller.
- 18. The method of claim 9 wherein the temperature of the mixing container is measured with a remote sensor.
- 19. A method for preparing a solid propellant mixture of aggregated oxidant and fuel particles in a binder having a predetermined particle size distribution, comprising the steps of:
- (a) charging a mixing container, equipped with a variable-speed impeller and a countersolvent supply system, with a solution of the binder, the fuel particles and optional processing aids;
- (b) admixing a first countersolvent portion into the charge of step (a) while maintaining agitation, wherein the first countersolvent portion is less than or about equal to an amount needed for coacervation without causing coacervation;
- (c) while maintaining mixing of the admixture from step (b), adding a charge of the oxidant particles thereto;
- (d) allowing the admixture from step (c) to thermally equilibrate;
- (e) measuring the temperature of the admixture from step (d);
- (f) determining the countersolvent-solvent ratio required for coacervation at the measured temperature;
- (g) while agitating the mixing container with the impeller, metering a second countersolvent portion from the countersolvent supply system into the admixture from step (d) in excess of the coacervation point to precipitate the binder and form aggregated particles, wherein a countersolvent metering rate and impeller speed are matched to obtain the predetermined particle size distribution of the aggregated particles;
- (h) admixing excess countersolvent into the mixture from step (g) while maintaining agitation with the impeller;
- (i) maintaining agitation of the mixture from step (h) for a period of time to allow the binder in the aggregated particles to harden;
- (j) stopping agitation of the mixture from step (i) and allowing the aggregated particles to settle in the mixing container;
- (k) decanting supernatant from the mixing container;
- (l) adding additional countersolvent to the mixing container, agitating the mixing container and repeating steps (j) and (k).
- 20. The method of claim 19 wherein the amount of the first countersolvent portion comprises at least about 80 percent of the amount of countersolvent needed for coacervation.
Parent Case Info
This application is a division of application Ser. No. 08/917,581, filed Aug. 20, 1997, now U.S. Pat. No. 5,879,079.
ORIGIN OF THE INVENTION
The invention described herein was made in the performance of work under a NASA contract and is subject to the provisions of Section 305 of the National Aeronautics and Space Act of 1958, Public Law 85-568 (72 Stat. 435; 42 U.S.C. 2457).
US Referenced Citations (22)
Divisions (1)
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Number |
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917581 |
Aug 1997 |
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