Method of producing high bulk density spheroidal nitroguanidine
A process for producing high bulk density spheroidal nitroguanidine by fong a solution of from 2 to 9 weight percent of nitroguanidine, 0.5 to 2.0 weight percent of methylcellulose, and 0.5 to 2.0 weight percent of partially hydrolyzed poly(vinyl alcohol) in water at a temperature of from 50.degree. C. to 100.degree. C., and then cooling the solution at a rate of from I to 20.degree. C./minute until the solution temperature is less than 40.degree. C.
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Claims
1. A process for recrystallizing nitroguanidine comprising:
- (1) forming an aqueous nitroguanidine solution at a temperature of from about 50.degree. C. to about 100.degree. C. which comprises
- (a) from 2 to 9 weight percent of nitroguanidine;
- (b) from 0.5 to 2.0 weight percent of methyl cellulose,
- (c) from 0.5 to 2.0 weight percent of a polyvinyl alcohol; and with
- (d) water being the remainder of the solution;
- (2) cooling the aqueous nitroguanidine solution under continuous and vigorous agitation at a cooling rate of from 1.degree. C./minutes to 20.degree. C./minute until the temperature of the solution is below 40.degree. C.; and
- (3) isolating the product spheroidal nitroguanidine crystals.
2. The process of claim 1 wherein nitroquandine comprises from 6 to 8 weight percent of the nitroguanidine solution in step (1).
3. The process of claim 1 wherein methyl cellulose comprises from 0.6 to 1.0 weight percent of the nitroguanidine solution in step (1).
4. The process of claim 1 wherein the polyvinyl alcohol comprises from 0.6 to 1.0 weight percent of the nitroguandine solution in step (1).
5. The process of claim 1 wherein the temperature in step (1) is from 50.degree. C. to 100.degree. C.
6. The process of claim 1 wherein the cooling rate in step (2) is from 1.degree. C. to 20.degree. C./min.
7. The process of claim 1 wherein the aqueous nitroguanidine solution is agitated in step (2) by stirring.
Type: Grant
Filed: Jun 23, 1988
Date of Patent: Feb 2, 1999
Assignee: The United States of America as represented by the Secretary of the Navy (Washington, DC)
Inventors: Kerry L. Wagaman (Waldorf, MD), Chester F. Clark (Waldorf, MD), William S. Jones (La Plata, MD), Steven L. Collignon (Waldorf, MD), Christopher C. Wilmot (Centreville, VA)
Primary Examiner: Edward A. Miller
Attorneys: Kenneth E. Walden, Roger D. Johnson
Application Number: 7/210,886
International Classification: C06B 2100;