US985724A - Method of producing ammonium perchlorate. - Google Patents
Method of producing ammonium perchlorate. Download PDFInfo
- Publication number
- US985724A US985724A US53776210A US1910537762A US985724A US 985724 A US985724 A US 985724A US 53776210 A US53776210 A US 53776210A US 1910537762 A US1910537762 A US 1910537762A US 985724 A US985724 A US 985724A
- Authority
- US
- United States
- Prior art keywords
- perchlorate
- ammonium
- sulfate
- ammonium perchlorate
- producing ammonium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- GDDNTTHUKVNJRA-UHFFFAOYSA-N 3-bromo-3,3-difluoroprop-1-ene Chemical compound FC(F)(Br)C=C GDDNTTHUKVNJRA-UHFFFAOYSA-N 0.000 title description 9
- 238000000034 method Methods 0.000 title description 7
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 10
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 9
- 229910052938 sodium sulfate Inorganic materials 0.000 description 9
- 235000011152 sodium sulphate Nutrition 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 7
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 6
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 6
- 235000011130 ammonium sulphate Nutrition 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 241000501754 Astronotus ocellatus Species 0.000 description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 description 2
- 229910001488 sodium perchlorate Inorganic materials 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfate Natural products OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/16—Perchloric acid
- C01B11/18—Perchlorates
Definitions
- OSCAR BIBG'EB Gammon or mlmsno, nvns'rn, SWEDEN, ASSIGNOR 'ro OSCAR sacrum CARLSON, F STOCKHOLM, SWEDEN.
- dunn perchlorate by means of ammonium nitrate has also been patented, but this method is, from a technical cndfeconomical point of view, inferior to the first mentioned one.
- ammonium perchloratcby means of crystallisation irom thcvlye obtained by addingammunium' sul-- Fate to'sodiuin perchlorate after the said live has'been sufficiently concentrated in any d'e-- sired manner
- ammonium perchlorate will settle on cooling the-said lyc. out at a certain point the byproduct, viz. sodium sulfate, will also crystallize, oantaining molecules-of water of crystallization.
- amnc onium perchlorate which is still in the mother liqnor, the latter is concentrated by boiling, whereby waterfrec sodium sulfate deposits while the liquor is hot and is separated before the same has become cold. In this manner a fresh portion of ammonium perchlorate is obtained, and so on.
- the ammo nium perchlorate obtained in this way conto ins but a small quantity of sodium sulfate, as the solubility of the ,waterfrec so dium sulfate increases when temperature decreases.
- the amnc onium perchlorate can be. quantitatively u'tilizcd'at the same time as the sodium sulfate is obtained free from water and am- 11nonia.
- the mother liquors may be einployed to dissolve fresh quantities of so If one should not wish to use dium perchlorate and ammonium sulfate. In these operatlons waterfree' sodium sulfate also deposits from the solutions and is then removed.
- the lead is in this case evidel ltly protected against the act-ion oil.
- the covering of lead sulfa tew W'hen u1 mn o uiuu1 chlcricl or ammonium nitrate is usech.
- nitrous gases are easily' evolved, an intermediate insulation of nitrogeu-chlorid (N01,). This is no! only dangerous for the health oft-he men, hut also causes :1 loss of valuable mnmmiin-nitrogen; This inconvenience is n-oiclerl when anuncnium sulfate is wsecl,
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Cosmetics (AREA)
Description
, No Drawing.
{Tooll wh'ooi it may concern:
UNITED salaries PATENT OFFICE.
OSCAR BIBG'EB Gammon, or mlmsno, nvns'rn, SWEDEN, ASSIGNOR 'ro OSCAR sacrum CARLSON, F STOCKHOLM, SWEDEN.
reunion or PRODUCING Amvromtnir rnncnnona'rn.
Specification 0! Letters Patent.
Application filed January 13, 1910. Serial No. 537,762.
Patented Feb. 28,1911.
lie it. lcnown that I, QBCAR"BIRGER Cam.-
son', a subject of the King of Swcdel'l, and.
resident of Mnsbo, A'vest a, in the Kingdom of Sweden, have inventedrertain new and useful Improvements in the Method of Producing Ammonium Perchlorate, of which the following is a specification.
In practice it has been found impossible to produc ammonium porchlora'te directly from ammonium chlorid by clccl'zrolysis on account of the instability of the intermedimouium salt. in'the market, and the. present ingwcdium perchlorate ntc product, viz. the ununonium chlorate. Cno has, therefore, lieen leftto the conv cn nion, by moons of ammonium chlorid, of sodium perchlorate, which can be produced by electrolysis. A method of converting so-.
dunn perchlorate by means of ammonium nitrate has also been patented, but this method is, from a technical cndfeconomical point of view, inferior to the first mentioned one. a
. Experience has, however, proved that it is possible in prnctlce to use for the said purpose ammonium sulfate, the cheapest aminvcntion has for its object a method of-prd dueingan'nnqnium perchlorate by convertby moans of ammonium sulfate. k
If one tries'to separate ammonium perchloratcby means of crystallisation irom thcvlye obtained by addingammunium' sul-- Fate to'sodiuin perchlorate after the said live has'been sufficiently concentrated in any d'e-- sired manner, ammonium perchlorate will settle on cooling the-said lyc. out at a certain point the byproduct, viz. sodium sulfate, will also crystallize, oantaining molecules-of water of crystallization. On
' account of this a fresh quantity of ammoni'um perchlorate inclosed Wlthin the sodium sulfate will also be deposited. It is therefore very difiicult and expensive to separate 4E ammonium.perchlorate "from the by-prodnot 'in this way. This fact- .whichis based upon the known condition oforystallization ofsodium sulfate, is evidently the reason why ammonium Sulfate has not hitherto ammonium perchlorate. Further investigations have .proved, that the greatest part of the ammonium perchlorate has, contrary to expectat-ion, crystallized before the crystallization of the sodium sulfate takes place, and morephenomena of supersaturation, at
perchlorate, which is still in the mother liqnor, the latter is concentrated by boiling, whereby waterfrec sodium sulfate deposits while the liquor is hot and is separated before the same has become cold. In this manner a fresh portion of ammonium perchlorate is obtained, and so on. The ammo nium perchlorate obtained in this way conto ins but a small quantity of sodium sulfate, as the solubility of the ,waterfrec so dium sulfate increases when temperature decreases. In the above manner the amnc onium perchlorate can be. quantitatively u'tilizcd'at the same time as the sodium sulfate is obtained free from water and am- 11nonia. evaporation, the mother liquors may be einployed to dissolve fresh quantities of so If one should not wish to use dium perchlorate and ammonium sulfate. In these operatlons waterfree' sodium sulfate also deposits from the solutions and is then removed.
It has been found that, on account of the f conditions of solubility, it is possible to pro coed in two ways in practically making the conversion. According to the first way hot solutions of ammonium sulfate and sodium perchlorate are mixcdtogcthw-oue of these solutions may also be replaced by the corresponding salt in solid stute-=whcreupon the ammonium perchlorate deposits, when the solution is cooled. According to the secmid way cold solutions are used; one of these may also be replaced bysolid salt. In this -the. temperature will rise from 35-40 because heat is developed in the conversion; 'l .he greatestjamt of tho salt. dcposlts during the mlxmg operatiolu Temperature 1s then allowed to fall to about. +22,-and ammo nium perchlorateds"separated from the mother. liqucrrbefore the sodium sulfate with 10 molecules of water of crystalliza tion begins to crystallize.
The above mentioned method of 'produe iilg ammonium perchlorate alsoofi'crs other l liquid by a 'lutions may beused in th case the cisterns are Stance be employed.
, which evidently depends on advantages tlmn.'tl10se,' which are due tethe lower rice of ammonium sulfate.
In the foregoing it is stated, that cold 50- e conversion, whereby steam is ecouomizecl and; furthermore, the cost of installation will be very low as no crystallization cisterns are neerled for the raw salt, which deposits directly (luring the mixing operation. Furthern'mrc, the use of metallic vessels is obj ectionable when mmnon'ium chloricl 01' ammonium nitrute are used as raw materials, as in this acted upon by the liqlf, on the coutrz'uy, he used, ciste l'ns'of land may for; in-
The lead is in this case evidel ltly protected against the act-ion oil. the covering of lead sulfa tew W'hen u1 mn o uiuu1 chlcricl or ammonium nitrate is usech. nitrous gases are easily' evolved, an intermediate insulation of nitrogeu-chlorid (N01,). This is no! only dangerous for the health oft-he men, hut also causes :1 loss of valuable mnmmiin-nitrogen; This inconvenience is n-oiclerl when anuncnium sulfate is wsecl,
uizl, fate ammonium sul Sodium nitrate and sodium chlorid will be less soluble at lower. tom Je'reture, while sodium sulfate as stated aliove becomes more easily soluble. When-usiu a OItlOn of the by-prouct deposits toget er with the ammonium perchloiate.
monium sulfate-and crystallizing out the a'mm'onium perchlorate while the temperature is not lower than 22 0., substantially as described. i In witness whereof, I-'lmve hereunto signed my name in thc presence of two subscribing witnesses. .OSGAB B-IRGER GARLSON.
Vlitnesses AXEL Ennuc'uu,
OSCAR, GRA-L-IN.
the old methods
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US53776210A US985724A (en) | 1910-01-12 | 1910-01-12 | Method of producing ammonium perchlorate. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US53776210A US985724A (en) | 1910-01-12 | 1910-01-12 | Method of producing ammonium perchlorate. |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US985724A true US985724A (en) | 1911-02-28 |
Family
ID=3054068
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US53776210A Expired - Lifetime US985724A (en) | 1910-01-12 | 1910-01-12 | Method of producing ammonium perchlorate. |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US985724A (en) |
-
1910
- 1910-01-12 US US53776210A patent/US985724A/en not_active Expired - Lifetime
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