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US3892610A Expired / Lapsed US ⏱️ 0.0 years remaining

Freeze drying process of making ultra-fine ammonium perchlorate and product

Assignee: Hercules LLC
•
Filing: 1973-01-08
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Granted: 1975-07-01
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Expires: 1993-01-08
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Abstract

Abstract Manufacture of ultra-fine ammonium perchlorate for incorporation into propellants, including the steps of A. FORMING AN AQUEOUS SOLUTION OF AMMONIUM PERCHLORATE (AP), and admixing said solution with an organic liquid immiscible with water and substantially a nonsolvent for AP, b. incorporating into the resulting admixture a branched chain hydroxy terminated polybutadiene (HTPB) having a molecular weight not exceeding about 2500, and a defined diester, and agitating the resulting water, AP, diester, and HTPB to form an emulsion comprising said organic liquid as continuous phase and said aqueous ammonium perchlorate solution as dispersed phase, C. FREEZING THE EMULSION, D. SUBLIMING THE ORGANIC LIQUID AND ICE FROM THE FROZEN EMULSION, AND E. RECOVERING RESIDUAL ULTRA-FINE AMMONIUM PERCHLORATE PARTICLES AS PRODUCT OF THE PROCESS. A composite propellant containing, as a binder, a branched chain HTPB having a molecular weight not exceeding about 2500, a defined diester as a plasticizer, and finely ammonium perchlorate as an oxidizer produced in accordance with process above described. Ultra-fine ammonium perchlorate produced in accordance with process above described.

Inventors

  • 👤 John R Huzinec

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-09 02:35
CPC Classifications
C; C01; C01B; C01B11/00; C01B11/16; C01B11/18; C01B11/185; C06; C06B; C06B21/00; C06B21/0091; C06B29/00; C06B29/02; C06B29/08; C06B29/22; Y; Y10; Y10S; Y10S149/00; Y10S149/11; Y10S149/113

Claims Analysis

Total Claims: 10
Claim 1
Independent Claim 177 words
A PROCESS FOR PREPARATION OF ULTRA-FINE AMMONIUM PERCHLORATE PARTICLES FOR INCORPORATION AS OXIDIZER INTO COMPOSITE PROPELLANTS COMPRISING: DISSOLVING AMMONIUM PERCHLORATE IN WATER TO FORM AN AQUEOUS SOLUTION OF AMMONIUM PERCHLORATE, ADMIXING SAID AQUEOUS SOLUTION OF AMMONIUM PERCHLORATE WITH AN ORGANIC LIQUID IMMISCIBLE WITH WATER AND SUBSTANTIALLY A NONSOLVENT FOR AMMONIUM PERCHLORATE FOR THE FORMATION OF AN EMULSION COMPRISING SAID ORGANIC LIQUID AS CONTINOUS PHASE AND SAID AQUEOUS SOLUTION AS DISPERSED PHASE THEREIN, INCORPORATING INTO THE RESULTING ADMIXTURE A BRANCHED CHAIN HYDROXY TERMINATED POLYBUTADIENE (HTPB) HAVING A MOLECULAR WEIGHT NOT EXCEEDING ABOUT 2,500 AS AN EMULSIFIER FOR THE FOMATION OF SAID EMULSION, AND A DIESTER OF AN ALCOHOL HAVING AT LEAST 2 CARBON ATOMS IN THE MOLECULE AND A DICARBOXYLIC ACID HAVING AT LEAST 3 CARBON ATOMS IN THE MOLECULE AS A STABILIZER FOR SAID EMULSION, AND AGITATING THE RESULTING MIXTURE OF WATER, AMMONIUM PERCHLORATE, DIESTER, AND HTPB TO FORM SAID EMULSION, FREEZING SAID EMULSION, SUBLIMING THE SAID ORGANIC LIQUID AND ICE FROM THE FROZEN EMULSION AND RECOVERING RESIUAL FINE AMMONIUM PERCHLORATE PARTICLES AS RPODUCT OF THE PROCESS.
Claim 2
Dependent Claim 177 words
A PROCESS FOR PREPARATION OF ULTRA-FINE AMMONIUM PERCHLORATE PARTICLES FOR INCORPORATION AS OXIDIZER INTO COMPOSITE PROPELLANTS COMPRISING: DISSOLVING AMMONIUM PERCHLORATE IN WATER TO FORM AN AQUEOUS SOLUTION OF AMMONIUM PERCHLORATE, ADMIXING SAID AQUEOUS SOLUTION OF AMMONIUM PERCHLORATE WITH AN ORGANIC LIQUID IMMISCIBLE WITH WATER AND SUBSTANTIALLY A NONSOLVENT FOR AMMONIUM PERCHLORATE FOR THE FORMATION OF AN EMULSION COMPRISING SAID ORGANIC LIQUID AS CONTINOUS PHASE AND SAID AQUEOUS SOLUTION AS DISPERSED PHASE THEREIN, INCORPORATING INTO THE RESULTING ADMIXTURE A BRANCHED CHAIN HYDROXY TERMINATED POLYBUTADIENE (HTPB) HAVING A MOLECULAR WEIGHT NOT EXCEEDING ABOUT 2,500 AS AN EMULSIFIER FOR THE FOMATION OF SAID EMULSION, AND A DIESTER OF AN ALCOHOL HAVING AT LEAST 2 CARBON ATOMS IN THE MOLECULE AND A DICARBOXYLIC ACID HAVING AT LEAST 3 CARBON ATOMS IN THE MOLECULE AS A STABILIZER FOR SAID EMULSION, AND AGITATING THE RESULTING MIXTURE OF WATER, AMMONIUM PERCHLORATE, DIESTER, AND HTPB TO FORM SAID EMULSION, FREEZING SAID EMULSION, SUBLIMING THE SAID ORGANIC LIQUID AND ICE FROM THE FROZEN EMULSION AND RECOVERING RESIUAL FINE AMMONIUM PERCHLORATE PARTICLES AS RPODUCT OF THE PROCESS.
Claim 3
Dependent Claim 11 words
A process of claim 1 wherein said diester is dioctyl adipate.
Claim 4
Dependent Claim 11 words
A process of claim 1 wherein said diester is isodecyl pelargmate.
Claim 5
Dependent Claim 35 words
A process of claim 1 wherein the aqueous solution of ammonium perchlorate comprises, on a weight basis from about 85 to about 95 percent water, and from about 15 to about 5 percent ammonium perchlorate.
Claim 6
Dependent Claim 27 words
A process of claim 4 wherein the weight ratio of the aqueous ammonium perchlorate solution to the said organic liquid is from about 5:1 to about 21:1.
Claim 7
Dependent Claim 24 words
A process of claim 5 wherein the molecular weight of said hydroxy terminated polybutadiene is within the range of from about 1,000 to 2,500.
Claim 8
Dependent Claim 20 words
A process of claim 6 wherein said organic ester is selected from the group of dioctyl adipate and isodecyl pelargmate.
Claim 9
Dependent Claim 52 words
A process of claim 7 wherein sufficient of each of said hydroxy terminated polybutadiene and said diester is incorporated into said emulsion to provide particulate ammonium perchlorate product containing on a weight basis from 1 to 3 percent of said hydroxy terminated polybutadiene and from 0.1 to 0.3 percent of said diester.
Claim 10
Dependent Claim 13 words
Finely divided ammonium perchlorate produced in accordance with the process of claim 1.

References Cited (Backward Citations)

US3350245A Cited
US3695952A Cited
US3651008A Cited
US3666575A Cited
US3685163A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1978-06-30 1978-12-30 1979-07-01 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1982-06-30 1982-12-30 1983-07-01 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1986-06-30 1986-12-30 1987-07-01 $7700.00 Window Closed / Lapsed

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