US3954526A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method for making coated ultra-fine ammonium perchlorate particles and product produced thereby
Assignee: ATK Launch Systems LLC
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Filing: 1971-02-22
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Granted: 1976-05-04
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Expires: 1991-02-22
Abstract
Abstract Sub-micron particle size ammonium perchlorate particles are made by mixing a solution of ammonium perchlorate in a volatile liquid with a second less volatile liquid which is miscible with the first liquid and is a non-solvent for ammonium perchlorate. The resulting mixture is heated to vaporize the volatile liquid and form a suspension of fine ammonium perchlorate particles in the second liquid. A particle coating agent soluble in the second liquid is used to limit particle growth. The particles are coated with the coating agent and may be recovered from the suspension by vaporization of the second liquid to form a powder, or by partial evaporization of the second liquid to form a concentrated slurry or paste in which the ammonium perchlorate is the disperse phase. The ultra-fine particles formed are suitable for use in propellant formulations.
Inventors
- 👤 Grafton F. Mangum
- 👤 Rudy E. Rogers
- 👤 Edward J. Schreck
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 09:15
CPC Classifications
C; C06; C06B; C06B21/00; C06B21/0083; Y; Y10; Y10S; Y10S149/00; Y10S149/11; Y10S149/113
Claims Analysis
Total Claims: 31
Claim 1
Independent Claim
107 words
A method of making ultra-fine ammonium perchlorate particles which comprises mixing a solution of ammonium perchlorate in a volatile liquid with a second less volatile liquid which is miscible with the first liquid and is a non-solvent for ammonium perchlorate, said mixture having dissolved therein a small amount of a coating agent selected from linear carboxylterminated, liquid, hydrocarbon polymers, finely divided inert solids, surface active agents and mixtures thereof, simultaneously agitating said mixture and vaporizing said solvent liquid to form a suspension of fine ammonium perchlorate particles in said second liquid and evaporating at least a part of said second liquid to recover said ammonium perchlorate particles.
Claim 2
Independent Claim
107 words
A method of making ultra-fine ammonium perchlorate particles which comprises mixing a solution of ammonium perchlorate in a volatile liquid with a second less volatile liquid which is miscible with the first liquid and is a non-solvent for ammonium perchlorate, said mixture having dissolved therein a small amount of a coating agent selected from linear carboxylterminated, liquid, hydrocarbon polymers, finely divided inert solids, surface active agents and mixtures thereof, simultaneously agitating said mixture and vaporizing said solvent liquid to form a suspension of fine ammonium perchlorate particles in said second liquid and evaporating at least a part of said second liquid to recover said ammonium perchlorate particles.
Claim 3
Dependent Claim
16 words
A method according to claim 1 wherein said coating agent is dissolved in said second liquid.
Claim 4
Dependent Claim
33 words
A method according to claim 1 wherein said coating agent is a liquid carboxyl-terminated hydrocarbon polymer, said ammonium perchlorate particles have a sub-micron particle size and said particles are coated with said polymer.
Claim 5
Dependent Claim
15 words
A method according to claim 1 wherein said coating agent is a surface active agent.
Claim 6
Dependent Claim
16 words
A method according to claim 1 wherein said coating agent is a finely divided inert solid.
Claim 7
Dependent Claim
14 words
A method according to claim 1 wherein said first liquid is methanol or acetone.
Claim 8
Dependent Claim
16 words
A method according to claim 1 wherein said second liquid is symmetrical tetrachlorodifluoroethane, chlorobenzene or xylene.
Claim 9
Dependent Claim
14 words
A method according to claim 1 wherein said mixture is agitated with ultra-sonic vibrations.
Claim 10
Dependent Claim
20 words
A method according to claim 8 wherein said ultra-sonic vibrations are in the range 10 to 100 KH z .
Claim 11
Dependent Claim
14 words
A method according to claim 3 wherein said hydrocarbon polymer is a carboxyl-terminated polybutadiene.
Claim 12
Dependent Claim
16 words
A method according to claim 3 wherein said hydrocarbon polymer is a butadiene acrylic acid copolymer.
Claim 13
Dependent Claim
32 words
A method according to claim 1 wherein said second liquid is heated to a temperature above the boiling point of said volatile liquid before said solution and said second liquid are mixed.
Claim 14
Dependent Claim
28 words
A method according to claim 1 wherein said second liquid is heated to a temperature near its boiling point before said solution and said second liquid are mixed.
Claim 15
Dependent Claim
48 words
A method according to claim 1 in which said coating agent is a liquid hydrocarbon used in an amount of at least 15% by weight of said ammonium perchlorate particles and said second solvent is evaporated to form a paste in which said ammonium perchlorate particles are dispersed.
Claim 16
Dependent Claim
47 words
A method according to claim 1 in which said coating agent is a liquid hydrocarbon polymer used in an amount of 0.5 to 5% by weight of said ammonium perchlorate particles and said second solvent is evaporated to form finely divided perchlorate particles coated with said polymer.
Claim 17
Independent Claim
98 words
A method of making ultra-fine ammonium perchlorate which comprises continuously mixing a solution of ammonium perchlorate in a volatile liquid with a second less volatile liquid which is miscible with the first liquid and has a small amount of coating agent dissolved therein, maintaining the resulting mixture at an elevated temperature to continuously vaporize said volatile liquid therefrom and cause fine ammonium perchlorate particles to form in said second liquid in suspension, continuously removing said suspension from said mixture and vaporizing at least a portion of said second liquid therefrom to recover fine particles of ammonium perchlorate therefrom.
Claim 18
Independent Claim
98 words
A method of making ultra-fine ammonium perchlorate which comprises continuously mixing a solution of ammonium perchlorate in a volatile liquid with a second less volatile liquid which is miscible with the first liquid and has a small amount of coating agent dissolved therein, maintaining the resulting mixture at an elevated temperature to continuously vaporize said volatile liquid therefrom and cause fine ammonium perchlorate particles to form in said second liquid in suspension, continuously removing said suspension from said mixture and vaporizing at least a portion of said second liquid therefrom to recover fine particles of ammonium perchlorate therefrom.
Claim 19
Dependent Claim
10 words
Sub-micron particles of ammonium perchlorate coated with a coating agent.
Claim 20
Dependent Claim
10 words
Sub-micron particles of ammonium perchlorate coated with a coating agent.
Claim 21
Dependent Claim
11 words
Sub-micron particles of ammonium perchlorate coated with a surface active agent.
Claim 22
Dependent Claim
11 words
Sub-micron particles of ammonium perchlorate coated with a surface active agent.
Claim 23
Dependent Claim
12 words
Sub-micron particles of ammonium perchlorate coated with a finely divided inert powder.
Claim 24
Dependent Claim
12 words
Sub-micron particles of ammonium perchlorate coated with a finely divided inert powder.
Claim 25
Dependent Claim
12 words
Sub-micron particles of ammonium perchlorate coated with a carboxyl-terminated, linear hydrocarbon polymer.
Claim 26
Dependent Claim
12 words
Sub-micron particles of ammonium perchlorate coated with a carboxyl-terminated, linear hydrocarbon polymer.
Claim 27
Dependent Claim
18 words
Sub-micron particles of ammonium perchlorate coated with a carboxyl-terminated polybutadiene having a molecular weight of 500 to 10,000.
Claim 28
Dependent Claim
18 words
Sub-micron particles of ammonium perchlorate coated with a carboxyl-terminated polybutadiene having a molecular weight of 500 to 10,000.
Claim 29
Dependent Claim
45 words
A composition having a paste-like consistency said composition consisting essentially of a dispersion of sub-micron particles of ammonium perchlorate dispersed in a liquid hydrocarbon polymer, said composition containing from about 15% to about 25%, based on the weight of ammonium perchlorate, of said liquid polymer.
Claim 30
Dependent Claim
45 words
A composition having a paste-like consistency said composition consisting essentially of a dispersion of sub-micron particles of ammonium perchlorate dispersed in a liquid hydrocarbon polymer, said composition containing from about 15% to about 25%, based on the weight of ammonium perchlorate, of said liquid polymer.
Claim 31
Dependent Claim
22 words
A composition according to claim 22 wherein said liquid polymer is a carboxyl-terminated poly-butadiene having a molecular weight of 500 to 10,000.
References Cited (Backward Citations)
GB191514866A
Cited
US2027114A
Cited
GB689283A
Cited
US2973257A
Cited
US3563966A
Cited
US3190776A
Cited
US3235589A
Cited
US3523839A
Cited
US3222231A
Cited
US3160535A
Cited
US3226784A
Cited
US3452445A
Cited
US3539377A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1979-05-04 | 1979-11-03 | 1980-05-04 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-05-04 | 1983-11-03 | 1984-05-04 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-05-04 | 1987-11-03 | 1988-05-04 | $7700.00 | Window Closed / Lapsed |