US2616785A - Method of lowering the tendency towards setting of potassium nitrate and potassium nitrate of free-flowing form with a reduced tendency to setting - Google Patents
Method of lowering the tendency towards setting of potassium nitrate and potassium nitrate of free-flowing form with a reduced tendency to setting Download PDFInfo
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- US2616785A US2616785A US85024A US8502449A US2616785A US 2616785 A US2616785 A US 2616785A US 85024 A US85024 A US 85024A US 8502449 A US8502449 A US 8502449A US 2616785 A US2616785 A US 2616785A
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- potassium nitrate
- setting
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/20—Preventing the absorption of moisture or caking
Definitions
- potassium nitrate of free-flowing form with a reduced tendency to setting which is partic- I be applied to finely divided potassium nitrate produced by a crystallisation process capable of passing through e. g. a 30, 60 or 100 mesh sieve (BSS).
- BSS mesh sieve
- the method of lowering the tendency towards setting of potassium nitrate comprises treating'thc potassium nitrate with a dyestufi of sulphonated aromatic character which in solution in a saturated aqueous solution of potassium nitrate conditions said potassium nitrate solution to produce on crystallization potassium nitrate in the form of thin and fragile crystals, possessing [001] crystal "habit and being thereby friable owing to their facial development relative to the 'cleavageplanes of the crystals.
- ventio potassium nitrate which is in non-coherin'g and free-flowing form contains'a dy'es'tufi of sulphonated aromaticcliaracte'r which in solution in 'a-saturated aqueous solution of i-potassium nitrate conditions said "potassium nitrate solution to produce on crystallisation potassium nitrate 'inthe form of thin fr'ag'ile crystals, friable owing to their facial development relative to the cleavage planes.
- dyestuffs of sulphonated aro- 'Iriatic character which are soluble in saturated potassium nitrate solution but which in lesser degree than the above reduce "the setting tendency of potassium nitrate are:
- Dyes comprising 3 naphthol 6-sulphonic acid. or fi naphthol 3:6-disulphonic acid coupled with dia'z'oti'zed 's'ul'phoriated "aniline 'or 'toluidine.
- the following examples illustrate how potassium nitrate according to the invention can be produced.
- the parts are parts by weight.
- Example '1- A saturated aqueous solution at 40 C. of potassium nitrate containing'0.1% of the added dye 1:4 diamino anthraquinone 2-sodium sulphonate on cooling crystallises in the altered habit of hexagonal plate-like crystals of extreme fragility.
- Example 2 Potassium nitrate (1000 gm.) ground and sieved through a 100 BSS sieve, is mixedwith 10 ml. of water containing in solution 1 gm. of 1:4. diamino anthraquinone 2-sodium' sulphonate in a hot water jacketed mixing machine such as a Werner-Pfleiderer incorporator, so that the dye is uniformly distributed over the individual particles. Following evaporation of the added water in the incorpo'rator the finely divided potassium nitrate may be stored for long periods without the occurrence of any hard caking. Untreated potassium nitrate of similar grist is found to cake rapidly under similar conditions involving exposure to atmosphere moisture.
- Example -3 Potassium nitrate is crystallised with rapid cooling and stirring to give small crystals.
- the crystals are isolated, and intheir wet state are treated with .05% of the dye by spraying with a 10% aqueous solution of 1:4 diamino anthraquinone 2-sodium sulphonate and are then passed through a rotary drier so that the dyestuif is uniformly distributed.
- the dry salt emerging is found to be free from any tendency towards hard setting undernormal storage conditions.
- Example 4 The procedure is the same as for Example 1 except that 1:4:5z8 tetramino anthraquinone disulphonic acid (sodium salt) is used.
- Example 5 The procedure is the same as for Example z except that 124:5:8 tetramino anthraquinone disulphonic acid (sodium salt) is used.
- Example 6 The procedure is the same as for Example 3 except that 1:4:528 tetramino anthraquinone disulphonic acid (sodium salt) is used.
- Example 10 The procedure is the same as for Example" 2 except that Amaranth (C. I. No. 184) is used insulphonate. The finely divided potassium nitrate stead of 1:4 diamino anthraquinone 2-sodium Example 8 The procedure is the same as for Example '7 except that Tartrazine (C. I. No. 640) is used instead of Amaranth. The finely divided potassium nitrate obtained has the same character istics as the potassium nitrate of Example '7.
- Example 9 The procedure is the same as for Example 2 except that Carmoisine LS (S. I. No. 180) is used instead of Amaranth.
- Carmoisine LS S. I. No. 180
- the dry crystals produced show a somewhat lessened tendency to- Wards cohering on standing as compared with similar untreated material.
- Example 10 The procedure is the same as for Example 9 except that Acid Violet 4BNS (C. I. No. 698) is.
- a free flowing potassium nitrate comprising crystals of potassium nitrate containing per parts of potassium nitrate, from 0.01 to 0.10 parts of at least one sulphonated aromatic dyestuff distributed predominantly on the surface of the crystal which is soluble to at least the aforesaid extent in a saturated aqueous solution of potassium nitrate and conditions such solution to produce on crystallization potassium nitrate in the form 'of thin, fragile crystals, possessing [001] crystal habit and being thereby friable owing to their facial development relative to the cleavage planes.
- a free flowing potassium nitrate comprising crystals of potassium nitrate containing per 100 parts of potassium nitrate from 0.01 to 0.10 part of at least one sulphonated aromatic dyestuif predominantly distributed on the surface of the said crystals which is soluble to at least the aforesaid extent in a saturated aqueous solution of potassium nitrate and which in such solution conditions said solution to produce on crystallization potassium nitrate in the form of thin friable crystals, possessing [001] crystal habit and being thereby friable owing to their facial development relative to the cleavage planes.
- a method for the production of free flowing potassium nitrate in crystalline form which comprises eifecting crystallization of an aqueous solution of potassium nitrate containing from- 0. 01 to 0.1 part per 100 parts of potassium nitrate in solution of at least one sulphonated aromatic dyestufi which issoluble to at least the 5 comprises spraying wet potassium nitrate crys- REFERENCES CITED tals with an aqueous solutmn of the dyestufi-
- the following references are of record in the 7.
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Description
Patented Nov. 4, 1952 UNITED ST TE S METHOD OF LOWERING THE TENDENGY TOWARDS SETTING OF POTASSIUM NI- TRATE AND POTASSIUM NITRATE 'OF FREE-FLOWING FORM WITH A REDUCED TENDENCY TO SETTING Alexander Butch'art, North ore eentararus'sam Scotland, assig'nor to Imperial Chemical Industries Limited, a corporation of Great Britain No Drawing. Application April -1, -1 949,'Seria1No. 85,024. In Great Britain December 29, --1948 '8 Claims. (ores- 162') l The present invention is concerned with a method of lowering the tendency towards setting of potassium nitrate and. with providing potassium nitrate of free-flowing form with a reduced tendency to setting, which is partic- I be applied to finely divided potassium nitrate produced by a crystallisation process capable of passing through e. g. a 30, 60 or 100 mesh sieve (BSS). Naturally coarsely crystalline free-flowing potassium nitrate,ascrysta1lised in commercial manufacturing processes, for example, potassium nitrate capable of passing through a mesh sieve and retained by a 30 mesh sieve, can also beneficially be treated according to the invention, this coarsely crystalline salt, however, is less prone to setting than 'finely divided potassium nitrate.
This application is related to application Serial 'No. 85,728, filed April '5, 1949, to Butchart and Whetstone. That application'discloses and claims the formation of a free flowing ammonium sulphate by the addition thereto of small amounts of sulphonated aromatic dyestufi which is soluble in a saturated aqueous solution of ammonium sulphate and which in such'solution conditions it'to produce on-c'rystallization ammonium sulphate in the form of thin fragile crystals whichare friable owing to their facial development relative to the -cleav'ageplanes.
According to the present invention the method of lowering the tendency towards setting of potassium nitrate comprises treating'thc potassium nitrate with a dyestufi of sulphonated aromatic character which in solution in a saturated aqueous solution of potassium nitrate conditions said potassium nitrate solution to produce on crystallization potassium nitrate in the form of thin and fragile crystals, possessing [001] crystal "habit and being thereby friable owing to their facial development relative to the 'cleavageplanes of the crystals. I
According to the present "inventio potassium nitrate which is in non-coherin'g and free-flowing form contains'a dy'es'tufi of sulphonated aromaticcliaracte'r which in solution in 'a-saturated aqueous solution of i-potassium nitrate conditions said "potassium nitrate solution to produce on crystallisation potassium nitrate 'inthe form of thin fr'ag'ile crystals, friable owing to their facial development relative to the cleavage planes.
The phrase dyestufi of sulphonate'd aromatic character includes soluble -salts of an aromatic dyestuff having at least one =sulphonic acid ."group and "aromatic dyestufis having at least one sulphonic acid =sub'stituent :group .per dye 11101801118.
Particularly suitable dyestuffs "which most markedly lower the tendency towards setting of potassium nitrate are:
1:4 dia'mino anthraquinone '2-sodium sulphonate.
1:415:21 t'etra'mino anthraqui-none 'disulphonic acid (sodium salt).
Examples of dyestuffs of sulphonated aro- 'Iriatic character which are soluble in saturated potassium nitrate solution but which in lesser degree than the above reduce "the setting tendency of potassium nitrate are:
Edicol Amaranth (Colour Index No. 184
Dyes comprising 3 naphthol 6-sulphonic acid. or fi naphthol 3:6-disulphonic acid coupled with dia'z'oti'zed 's'ul'phoriated "aniline 'or 'toluidine.
Azofuchsin'e G (comu'ri'ndex No. 153) Fast Red E (Colour index-No. 182) Chlorazol Sky Blue (Colour Index lfio. 518) Acid Green M (Colour Indeir 180.669) V Tartrazine (Colour Index 'No. 640) The following dyestuffs exemplify those soluble in water, and-at leastslig'htly soluble '-in "saturated potassium nitrate solutions but which even so have onl'yaa slight tendency "to reduce the setting and also to maintain the free-flow- 'ing nature of potassium i'iitratez AeidMa'g'en'ta (Colour Inde'xNo. B92) C rmoisine-fins (Colour Index No.29)
3 Carmoisine LS (Colour Index No. 180) Bismarck Brown (Colour Index No. 331) Hydrazine Yellow SO (Colour Index No. 637) Acid Green G (Colour Index No. 666) Erioglaucine Extra (Colour Index No. 671) Acid Violet 4BNS (Colour Index No. 698) 1:5 diamino anthraquinone 2-sulphonic acid.
It has been found that the addition of, for example, between 0.01 and 0.10 part of 1:4 diamino anthraquinone 2-sodium sulphonate or 124:5:8 tetramino anthraquinone disulphonic acid (sodium salt) to 100 parts of potassium nitrate capable of passing through a 100 mesh screen lessens the tendency of thepotassium nitrate towards caking or setting.
The following examples illustrate how potassium nitrate according to the invention can be produced. The parts are parts by weight.
Example '1- A saturated aqueous solution at 40 C. of potassium nitrate containing'0.1% of the added dye 1:4 diamino anthraquinone 2-sodium sulphonate on cooling crystallises in the altered habit of hexagonal plate-like crystals of extreme fragility. v
Example 2 Potassium nitrate (1000 gm.) ground and sieved through a 100 BSS sieve, is mixedwith 10 ml. of water containing in solution 1 gm. of 1:4. diamino anthraquinone 2-sodium' sulphonate in a hot water jacketed mixing machine such as a Werner-Pfleiderer incorporator, so that the dye is uniformly distributed over the individual particles. Following evaporation of the added water in the incorpo'rator the finely divided potassium nitrate may be stored for long periods without the occurrence of any hard caking. Untreated potassium nitrate of similar grist is found to cake rapidly under similar conditions involving exposure to atmosphere moisture.
Example -3 Potassium nitrate is crystallised with rapid cooling and stirring to give small crystals. The crystals are isolated, and intheir wet state are treated with .05% of the dye by spraying with a 10% aqueous solution of 1:4 diamino anthraquinone 2-sodium sulphonate and are then passed through a rotary drier so that the dyestuif is uniformly distributed. The dry salt emerging is found to be free from any tendency towards hard setting undernormal storage conditions.
Example 4 The procedure is the same as for Example 1 except that 1:4:5z8 tetramino anthraquinone disulphonic acid (sodium salt) is used.
Example 5 The procedure is the same as for Example z except that 124:5:8 tetramino anthraquinone disulphonic acid (sodium salt) is used.
Example 6 The procedure is the same as for Example 3 except that 1:4:528 tetramino anthraquinone disulphonic acid (sodium salt) is used.
Example] The procedure is the same as for Example" 2 except that Amaranth (C. I. No. 184) is used insulphonate. The finely divided potassium nitrate stead of 1:4 diamino anthraquinone 2-sodium Example 8 The procedure is the same as for Example '7 except that Tartrazine (C. I. No. 640) is used instead of Amaranth. The finely divided potassium nitrate obtained has the same character istics as the potassium nitrate of Example '7.
Example 9 The procedure is the same as for Example 2 except that Carmoisine LS (S. I. No. 180) is used instead of Amaranth. The dry crystals produced show a somewhat lessened tendency to- Wards cohering on standing as compared with similar untreated material.
Example 10 The procedure is the same as for Example 9 except that Acid Violet 4BNS (C. I. No. 698) is.
used instead of Carmo-isine LS. The properties of the dry crystals are the same as thoseof Example 9. 1
I claim:
1. A free flowing potassium nitrate comprising crystals of potassium nitrate containing per parts of potassium nitrate, from 0.01 to 0.10 parts of at least one sulphonated aromatic dyestuff distributed predominantly on the surface of the crystal which is soluble to at least the aforesaid extent in a saturated aqueous solution of potassium nitrate and conditions such solution to produce on crystallization potassium nitrate in the form 'of thin, fragile crystals, possessing [001] crystal habit and being thereby friable owing to their facial development relative to the cleavage planes.
2. A free flowing potassium nitrate as recited in claim 1 in which the dyestuff is 1:4 diamino anthraquinone 2-sodium sulphonate.
3. A free flowing potassium nitrate as recited in claim 1 in which the dyestuif is 1:4:5 :8 tetramino anthraquinone disulphonic acid.
4. A free flowing potassium nitrate comprising crystals of potassium nitrate containing per 100 parts of potassium nitrate from 0.01 to 0.10 part of at least one sulphonated aromatic dyestuif predominantly distributed on the surface of the said crystals which is soluble to at least the aforesaid extent in a saturated aqueous solution of potassium nitrate and which in such solution conditions said solution to produce on crystallization potassium nitrate in the form of thin friable crystals, possessing [001] crystal habit and being thereby friable owing to their facial development relative to the cleavage planes.
5. A method for the production of free flowing potassium nitrate in crystalline form which comprises eifecting crystallization of an aqueous solution of potassium nitrate containing from- 0. 01 to 0.1 part per 100 parts of potassium nitrate in solution of at least one sulphonated aromatic dyestufi which issoluble to at least the 5 comprises spraying wet potassium nitrate crys- REFERENCES CITED tals with an aqueous solutmn of the dyestufi- The following references are of record in the 7. A method for the production of free flowing hi potassium nitrate as recited in claim 5 in which file of t s patent the said dyestuff is 1:4 diamino anthraquinone 2- 5 UNITED STATES PATENTS sodium sulphonate. Number Name Date 8. A method for the production of free flowing 1,056,365 Raschig Mar. 18, 1913 potassium nitrate as recited in claim 5 in which 1,550,064 Ehrlich Aug. 18, 1925 the said dyestuff is the sodium salt of 1:4:5z8 2,009,437 Coolidge et a] July 30, 1935 tetramino anthroquinone disulphonic acid. 10 2,377,670 Burdett et a1 June 5, 1945 2,383,763 Bloch et a1 Aug. 28, 1945 ALEXANDER BUTCHART. 2,408,059 Garfield et a1. Sept. 24, 1946
Claims (1)
1. A FREE FLOWING POTASSIUM NITRATE COMPRISING CRYSTALS OF POTASSIUM NITRATE CONTAINING PER 100 PARTS OF POTASSIUM NITRATE, FROM 0.01 TO 0.10 PARTS OF AT LEAST ONE SULPHONATED AROMATIC DYESTUFF DISTRIBUTED PREDOMINANTLY ON THE SURFACE OF THE CRYSTAL WHICH IS SOLUBLE TO AT LEAST THE AFORESAID EXTENT IN A SATURATED AQUEOUS SOLUTION OF POTASSIUM NITRATE AND CONDITIONS SUCH SOLUTION TO PRODUCE ON CRYSTALLIZATION POTASSIUM NITRATE IN THE FORM OF THIN, FRAGILE CRYSTALS, POSSESSING (001) CRYSTAL HABIT AND BEING THEREBY FRIABLE OWING TO THEIR FACIAL DEVELOPMENT RELATIVE TO THE CLEAVAGE PLANES.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB2616785X | 1948-12-29 |
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| Publication Number | Publication Date |
|---|---|
| US2616785A true US2616785A (en) | 1952-11-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| US85024A Expired - Lifetime US2616785A (en) | 1948-12-29 | 1949-04-01 | Method of lowering the tendency towards setting of potassium nitrate and potassium nitrate of free-flowing form with a reduced tendency to setting |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2720446A (en) * | 1950-09-25 | 1955-10-11 | Ici Ltd | Free-flowing ammonium nitrate |
| US2782094A (en) * | 1953-06-12 | 1957-02-19 | Ici Ltd | Potassium nitrate of reduced tendency to caking and setting |
| US2782095A (en) * | 1953-08-19 | 1957-02-19 | Ici Ltd | Sodium nitrate of reduced tendency to caking and setting |
| US2885262A (en) * | 1955-08-22 | 1959-05-05 | Olin Mathieson | Stabilized manganese dioxide |
| US3171717A (en) * | 1961-03-07 | 1965-03-02 | Nitroglycerin Ab | Free-flowing ammonium nitrate |
| US4131117A (en) * | 1976-12-21 | 1978-12-26 | Philip Morris Incorporated | Method for removal of potassium nitrate from tobacco extracts |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1056365A (en) * | 1912-04-11 | 1913-03-18 | Fritz Raschig | Explosive and process of producing same. |
| US1550064A (en) * | 1925-05-05 | 1925-08-18 | Verona Chemical Co | Explosive |
| US2009437A (en) * | 1932-05-24 | 1935-07-30 | Du Pont | Noncaking pigment |
| US2377670A (en) * | 1943-08-26 | 1945-06-05 | Remington Arms Co Inc | Ammunition priming mixtures |
| US2383763A (en) * | 1942-11-10 | 1945-08-28 | Palestine Potash Ltd | Crystallization of salts from aqueous solutions |
| US2408059A (en) * | 1940-07-03 | 1946-09-24 | Olin Ind Inc | Manufacture of diazodinitrophenol |
-
1949
- 1949-04-01 US US85024A patent/US2616785A/en not_active Expired - Lifetime
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1056365A (en) * | 1912-04-11 | 1913-03-18 | Fritz Raschig | Explosive and process of producing same. |
| US1550064A (en) * | 1925-05-05 | 1925-08-18 | Verona Chemical Co | Explosive |
| US2009437A (en) * | 1932-05-24 | 1935-07-30 | Du Pont | Noncaking pigment |
| US2408059A (en) * | 1940-07-03 | 1946-09-24 | Olin Ind Inc | Manufacture of diazodinitrophenol |
| US2383763A (en) * | 1942-11-10 | 1945-08-28 | Palestine Potash Ltd | Crystallization of salts from aqueous solutions |
| US2377670A (en) * | 1943-08-26 | 1945-06-05 | Remington Arms Co Inc | Ammunition priming mixtures |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2720446A (en) * | 1950-09-25 | 1955-10-11 | Ici Ltd | Free-flowing ammonium nitrate |
| US2782094A (en) * | 1953-06-12 | 1957-02-19 | Ici Ltd | Potassium nitrate of reduced tendency to caking and setting |
| US2782095A (en) * | 1953-08-19 | 1957-02-19 | Ici Ltd | Sodium nitrate of reduced tendency to caking and setting |
| US2885262A (en) * | 1955-08-22 | 1959-05-05 | Olin Mathieson | Stabilized manganese dioxide |
| US3171717A (en) * | 1961-03-07 | 1965-03-02 | Nitroglycerin Ab | Free-flowing ammonium nitrate |
| US4131117A (en) * | 1976-12-21 | 1978-12-26 | Philip Morris Incorporated | Method for removal of potassium nitrate from tobacco extracts |
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