Alchemist
July 22nd, 2002, 10:57 PM
Hello all,
The other night I dreamed I made Potassium Dinitramide (KDN) and Ammonium Dinitramide at home and it worked. Here are the details of my dream.
Precursors are:
70.35 grams of Sulfamic Acid, this can be bought at most hardware stores as grout and tile cleaner.
53 grams of Potassium Hydroxide, I got mine at a industrial cleaning supply house. I do NOT know if Sodium Hydroxide will work as yet!
264 ML of 95% Ethanol, mine was home made.
45 ML of 90-95% Nitric acid, again home made.
16 ML of 98% Sulfuric Acid, hardware store drain cleaner.
Approx. 10 ML of Acetone from the hardware store.
100 ML of 99% Isopropyl Alcohol.
DRY ICE as needed!
Step 1:Potassium salt of Sulfamic Acid
Procedure:
Prepare a suspension by adding 70.35 grams of sulfamic acid into 50 milliliters of water. Prepare a second mixture by dissolving 44 grams of potassium hydroxide into 50 milliliters of water. Thereafter, add the potassium hydroxide solution to
the sulfamic acid suspension with rapid stirring. After which, pour the entire mixture into 214 milliliters of 95% ethanol while stirring the ethanol. After which, filter-off the precipitated potassium salt of sulfamic acid, wash with 50 milliliters of 95% ethanol, several times using the same washing portion, and then vacum or air-dry the product. After the product has been sufficiently dried, grind it up into a fine powder for use in step 2.
Step 2:Preparation of potassium dinitramide
Place 45 milliliters of 90% nitric acid into a beaker, and then add 16 milliliters of 98% sulfuric acid. Thereafter, cool the acid mixture to -30 Celsius by mean of a dry ice/acetone bath.
Then, carefully, and gradually add 17 grams of the potassium salt of sulfamic acid (prepared in step I), in 500-milligram portions, to the nitrating acid mixture over a period of about 20 minutes. During the addition, rapidly stir the nitrating acid mixture and maintain its temperature at -30 Celsius. After the addition(20 minutes), immedially pour the entire reaction mixture into a beaker filled with 150 grams of crushed ice and 150 millilitcrs of water. Immediatly thereafter, place this ice water mixture into a dry ice/acetone bath, and then rapidly add 9 grams of a cold potassium hydroxide solution prepared by dissolving 9 grams of potassium hydroxide into 20 milliliters of ice-cold watcr. During the potassium hydroxide addition, rapidly stir the reaction mixture while keeping its temperature below 0 Celsius. Note. the solution should tum a greenish-yellow color. After the addition of the potassium hydroxide, place the reaction mixture into rotary evaporator, and evaporate-off the water under vacuum until dry solid remains. If rotary evaporator is unavailable, place reaction mixture into a shallow pan, and then blow air over the surface until dry solid remains. When dry solid remains, recover the dry solid, and then mix with 10 milliliters of acetone, and then add 100 milliliters of isopropyl alcohol. Then stir the mixture rapidly for several minutes. After which, place the mixture into a clean rotary evaporator, and evaporate-off the acetone, and some of the isopropyl alcohol under vacuum. If a rotary evaporator is unavailable, place the mixture into a distillation apparatus, and carefully distill-off the acetone and some of the isopropyl alcohol. Once the acetone has been removed, stop the evaporation, and then cool the mixture to room temperature. When the acetone is removed, the KDN will
precipitate. Thereafter, filter-off the precipitated KDN, and then vacuum dry or air-dry the product. The result will be about
10.7 grams of relatively pure KDN.
To make Ammonium Dinitramide mix a solution of KDN in water, with a solution of Ammonium Sulfate in water. Stir for several minuites then addl Isopropyl Alcohol and continue to stir for several more minutes ! Then filter off the Potassium Sulfate and let the Ammonium Dinitamide air dry. Then redisollve in Isopropyl again and air dry a secound time!
*** If you try this please give me your feed back on how it worked for you.
*** MEGA, this would be a good one for your sight!
P.S., this is almost a exact copy of U.S. pat. # 5,976,483. I used the same quanities as they did. I wanted it to be like there's for my first test. One change was to use Acetone in the freezing bath. The only point here though is to get the temp. to -30 degree's C.
The important factors seem to be the temp's and VERY good stirring! A good mechanical stirer would be a benifit here!
See the pat. for even more details.
This stuff is great and I think better than or as good as Chlorate and Perchlorate!
More later!!!
<small>[ July 23, 2002, 03:31 PM: Message edited by: Alchemist ]</small>
The other night I dreamed I made Potassium Dinitramide (KDN) and Ammonium Dinitramide at home and it worked. Here are the details of my dream.
Precursors are:
70.35 grams of Sulfamic Acid, this can be bought at most hardware stores as grout and tile cleaner.
53 grams of Potassium Hydroxide, I got mine at a industrial cleaning supply house. I do NOT know if Sodium Hydroxide will work as yet!
264 ML of 95% Ethanol, mine was home made.
45 ML of 90-95% Nitric acid, again home made.
16 ML of 98% Sulfuric Acid, hardware store drain cleaner.
Approx. 10 ML of Acetone from the hardware store.
100 ML of 99% Isopropyl Alcohol.
DRY ICE as needed!
Step 1:Potassium salt of Sulfamic Acid
Procedure:
Prepare a suspension by adding 70.35 grams of sulfamic acid into 50 milliliters of water. Prepare a second mixture by dissolving 44 grams of potassium hydroxide into 50 milliliters of water. Thereafter, add the potassium hydroxide solution to
the sulfamic acid suspension with rapid stirring. After which, pour the entire mixture into 214 milliliters of 95% ethanol while stirring the ethanol. After which, filter-off the precipitated potassium salt of sulfamic acid, wash with 50 milliliters of 95% ethanol, several times using the same washing portion, and then vacum or air-dry the product. After the product has been sufficiently dried, grind it up into a fine powder for use in step 2.
Step 2:Preparation of potassium dinitramide
Place 45 milliliters of 90% nitric acid into a beaker, and then add 16 milliliters of 98% sulfuric acid. Thereafter, cool the acid mixture to -30 Celsius by mean of a dry ice/acetone bath.
Then, carefully, and gradually add 17 grams of the potassium salt of sulfamic acid (prepared in step I), in 500-milligram portions, to the nitrating acid mixture over a period of about 20 minutes. During the addition, rapidly stir the nitrating acid mixture and maintain its temperature at -30 Celsius. After the addition(20 minutes), immedially pour the entire reaction mixture into a beaker filled with 150 grams of crushed ice and 150 millilitcrs of water. Immediatly thereafter, place this ice water mixture into a dry ice/acetone bath, and then rapidly add 9 grams of a cold potassium hydroxide solution prepared by dissolving 9 grams of potassium hydroxide into 20 milliliters of ice-cold watcr. During the potassium hydroxide addition, rapidly stir the reaction mixture while keeping its temperature below 0 Celsius. Note. the solution should tum a greenish-yellow color. After the addition of the potassium hydroxide, place the reaction mixture into rotary evaporator, and evaporate-off the water under vacuum until dry solid remains. If rotary evaporator is unavailable, place reaction mixture into a shallow pan, and then blow air over the surface until dry solid remains. When dry solid remains, recover the dry solid, and then mix with 10 milliliters of acetone, and then add 100 milliliters of isopropyl alcohol. Then stir the mixture rapidly for several minutes. After which, place the mixture into a clean rotary evaporator, and evaporate-off the acetone, and some of the isopropyl alcohol under vacuum. If a rotary evaporator is unavailable, place the mixture into a distillation apparatus, and carefully distill-off the acetone and some of the isopropyl alcohol. Once the acetone has been removed, stop the evaporation, and then cool the mixture to room temperature. When the acetone is removed, the KDN will
precipitate. Thereafter, filter-off the precipitated KDN, and then vacuum dry or air-dry the product. The result will be about
10.7 grams of relatively pure KDN.
To make Ammonium Dinitramide mix a solution of KDN in water, with a solution of Ammonium Sulfate in water. Stir for several minuites then addl Isopropyl Alcohol and continue to stir for several more minutes ! Then filter off the Potassium Sulfate and let the Ammonium Dinitamide air dry. Then redisollve in Isopropyl again and air dry a secound time!
*** If you try this please give me your feed back on how it worked for you.
*** MEGA, this would be a good one for your sight!
P.S., this is almost a exact copy of U.S. pat. # 5,976,483. I used the same quanities as they did. I wanted it to be like there's for my first test. One change was to use Acetone in the freezing bath. The only point here though is to get the temp. to -30 degree's C.
The important factors seem to be the temp's and VERY good stirring! A good mechanical stirer would be a benifit here!
See the pat. for even more details.
This stuff is great and I think better than or as good as Chlorate and Perchlorate!
More later!!!
<small>[ July 23, 2002, 03:31 PM: Message edited by: Alchemist ]</small>