WO2004039722A1 - Method for production of nitrate-containing products from undercooling melts - Google Patents
Method for production of nitrate-containing products from undercooling melts Download PDFInfo
- Publication number
- WO2004039722A1 WO2004039722A1 PCT/NO2002/000400 NO0200400W WO2004039722A1 WO 2004039722 A1 WO2004039722 A1 WO 2004039722A1 NO 0200400 W NO0200400 W NO 0200400W WO 2004039722 A1 WO2004039722 A1 WO 2004039722A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- weight
- melt
- nitrate
- particles
- water
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/38—Magnesium nitrates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/48—Methods for the preparation of nitrates in general
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/36—Nitrates
- C01F11/44—Concentrating; Crystallisating; Dehydrating; Preventing the absorption of moisture or caking
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C1/00—Ammonium nitrate fertilisers
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C1/00—Ammonium nitrate fertilisers
- C05C1/02—Granulation; Pelletisation; Stabilisation; Colouring
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C5/00—Fertilisers containing other nitrates
- C05C5/02—Fertilisers containing other nitrates containing sodium or potassium nitrate
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C5/00—Fertilisers containing other nitrates
- C05C5/04—Fertilisers containing other nitrates containing calcium nitrate
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
Definitions
- the invention concerns production of nitrate-containing products (fertilizers, technical products) from undercooling melts.
- the CN melt In order to use devices like centrifugal or nozzle prilling equipment or pan/ drum granulators, the CN melt has to have compositions that contain 5-8 weight % ammonium nitrate (AN).
- AN ammonium nitrate
- the object of the invention is to obtain a method to produce high quality solid CN-water particles easily, in large quantities. Another object is to obtain a production method that could be applied generally for nitrate containing salts that very often tend to form super cooling melts.
- the invention thus concerns a method for the production of nitrate containing products (fertilizers, technical products) from undercooling melts, wherein a XN - water solution is evaporated up to a content of 50-99.8 weight % XN, where X is one or more selected from Ca, Mg, NEU, Na and K, and N means nitrate.
- XN is one or more selected from Ca, Mg, NEU, Na and K
- N means nitrate.
- the preferred range of XN is 70-99.5 weight %.
- the melt is cooled down to and kept at a temperature at or below the crystallisation point and finely divided solid XN powder consisting of the equilibrium phases is added to the melt. Melt drops are then formed and allowed to cool and solidify during up to 70 seconds, preferably 20-70 seconds. It is preferred to use a cooling belt for solidification of the particles.
- the belt is cooled by air, water, oil or another medium.
- the melt temperature is preferably kept 0-10°C below the crystallization point of the melt.
- CN*2H 2 O and CN *3H 2 O are used as seed particles.
- the particles formed have a particle size between 0,2 and 0,8 mm, preferably between 0,4 and 0,6 mm.
- Particles could be made from a melt consisting of 74 weight % calcium nitrate, 14 weight % potassium nitrate and 12 weight % water.
- Solid particles can also be produced consisting of a homogenous mixture of nitrates, chlorides and crystal water. An example of this is particles made from a melt consisting essentially of 50 weight % calcium nitrate, 4 weight % ammonium nitrate, 26.5 weight % calcium chloride and 18-20 weight % water.
- Example 1 Granules CN-water solutions were evaporated to above 70, 75 and 78 weight % CN .
- Example 2 Prills Melts with the CN concentrations mentioned above, were kept at temperatures close to the crystallization point given by the literature. Finely crushed NH-CN were mixed into the melt subsequent to pumping the melt at high pressure to nozzles where drops were formed and allowed to cool down to 20°C for 5-10 seconds. As cooling medium oil and air were tried. Solid particles did not form due to undercooling.
- melt-droplets turned into slurries with no particle strength as they cooled down.
- Trial 3 CN melt having 23 weight % water and 77 weight % CN were allowed to cool on a plate for 48 hours at 20°C. A white solid material was formed during this time
- melt composition was 25 weight %/ 75 weight % and 21.5 weight %/ 78,5 weight % (H 2 O/CaN).
- Trial 5 Same procedure as in Trial 4, after reducing the temperature of the melt (23% weight % H O/77% weight % CN) to approximately 45°C the finely divided solid material was mixed in as seeding particles. As crystals started to form in the beaker, drops were allowed to fall on the cooling plate and simultaneously pure melt (23 weight %l 11 weight %) with temperature below 50°C was added to the beaker, while stirring.
- Trial 5 in Example 3 was repeated by replacing CN melt with 1: MgN-water melt having composition 67 weight % MgN and 33 weight % H 2 O (boiling point 180 °C) and 2: MgN- water melt with composition 58 weight % MgN and 42 weight %(boiling point 155°C). Both melt 1 and 2 were cooled down to 30°C by procedure mentioned in trial 5 (Example 3). Letting composition 1 and 2 solidify in an exsiccator for 3 days, and then crush the solids formed into a fine powder made seeding material.
- MgN*4H 2 O and MgN *6H 2 O were made also without seeding material as the MgN*6H 2 O melt very easily solidified.
- Example 6 Making pastilles of MgN- AN and CN
- a melt consisting of 67 weight % CN, 4.0 weight % AN, 10 weight % MgN and 20 weight % water was held at 110°C.
- the melt was cooled down to 65°C and seeding material thoroughly mixed in as drops were allowed to fall on a cold metal plate.
- Example 7 Mixture of CN , AN and CaCb
- a melt consisting of 50 weight % CN, 4 weight % AN, 26.5 weight % CaCl 2 and 18-20 weight % water was made by melting a mixture of NH-CN and CaCl 2 *2H 2 O (130-140°C).
- a melt consisting of 74 weight % CN, 14 weight % KN and 12 weight % water was made by evaporating water from a CN -KN -H 2 O solution.
- the melt temperature was reduced to 86°C, app. 5-6°C above crystallization point.
- 3 weight % finely grained seed material was thoroughly mixed in and droplets allowed falling on to a cold metal plate (23°C).
- the right seeding material was made by letting the melt composition crystallise in an exsiccator over 2-3 days and then grind to powder the solid formed.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Fertilizers (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
Description
Claims
Priority Applications (28)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
UAA200505207A UA80163C2 (en) | 2002-11-01 | 2002-01-11 | Process for obtaining of nitrate containing products from undercooled melts |
SI200220044A SI21742A (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate-containing products from undercooling melts |
CA002503842A CA2503842C (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate-containing products from undercooling melts |
MXPA05004624A MXPA05004624A (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate-containing products from undercooling melts. |
CNB028298349A CN1307090C (en) | 2002-11-01 | 2002-11-01 | Method for prodn, of nitrate-Containing products from undercooling metals |
PT02778107T PT1556308E (en) | 2002-11-01 | 2002-11-01 | METHOD FOR PRODUCING PRODUCTS CONTAINING NITRATES FROM OVERFLOW MELTING |
AU2002339757A AU2002339757B9 (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate-containing products from undercooling melts |
NZ539890A NZ539890A (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate-containing products from undercooling melts |
SK5036-2005A SK287778B6 (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate containing products from under-cooled melts |
BRPI0215929-5A BR0215929B1 (en) | 2002-11-01 | 2002-11-01 | method for the production of nitrate products (fertilizers) from subcooling fusions. |
AT02778107T ATE324352T1 (en) | 2002-11-01 | 2002-11-01 | METHOD FOR PRODUCING NITRATE CONTAINING PRODUCTS FROM SUPERCOOLING MELTS |
ROA200500397A RO121775B1 (en) | 2002-11-01 | 2002-11-01 | Process for producing nitrate-containing products from undercooling melts |
ES02778107T ES2261746T3 (en) | 2002-11-01 | 2002-11-01 | PROCEDURE FOR THE PRODUCTION OF PRODUCTS CONTAINING NITRATE FROM SUB-COOLED GROUNDED MASSES. |
DE60211039T DE60211039T2 (en) | 2002-11-01 | 2002-11-01 | PROCESS FOR PRODUCING NITRATE-CONTAINING PRODUCTS FROM UNDER COOLING MELTS |
PCT/NO2002/000400 WO2004039722A1 (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate-containing products from undercooling melts |
DK02778107T DK1556308T3 (en) | 2002-11-01 | 2002-11-01 | Method for making nitrate-containing products from undercooled melting agents |
EA200500754A EA008385B1 (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate-containing products from undercooling melts |
US10/533,417 US7500995B2 (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate-containing products from undercooling melts |
EP02778107A EP1556308B1 (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate-containing products from undercooling melts |
JP2004548172A JP4435689B2 (en) | 2002-11-01 | 2002-11-01 | Process for producing nitrate-containing products from undercooled melts |
HU0500835A HU230118B1 (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate-containing products from undercooling melts |
CZ2005-315A CZ306507B6 (en) | 2002-11-01 | 2002-11-01 | A method of manufacturing products containing nitrates from undercooled melts |
EG2003101006A EG23430A (en) | 2002-11-01 | 2003-10-28 | Method for production of nitrate-containing products from undercooling melts. |
NO20051857A NO20051857L (en) | 2002-11-01 | 2005-04-15 | Process for producing nitrate-containing products from undercooling melts |
IL168185A IL168185A (en) | 2002-11-01 | 2005-04-21 | Method for production of nitrate-containing products from undercooling melts |
BG109137A BG66487B1 (en) | 2002-11-01 | 2005-04-26 | Method for production of nitrate-containing products from undercooling melts |
HRP20050374AA HRP20050374B1 (en) | 2002-11-01 | 2005-04-27 | Method for production of nitrate-containing products from undercooling melts |
CY20061100952T CY1105077T1 (en) | 2002-11-01 | 2006-07-07 | METHOD FOR PRODUCING PRODUCTS WHICH COMPRESS NITRATE FROM LOW TEMPERATURE MELTS FROM MELTING TEMPERATURE |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/NO2002/000400 WO2004039722A1 (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate-containing products from undercooling melts |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2004039722A1 true WO2004039722A1 (en) | 2004-05-13 |
Family
ID=32294153
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/NO2002/000400 WO2004039722A1 (en) | 2002-11-01 | 2002-11-01 | Method for production of nitrate-containing products from undercooling melts |
Country Status (28)
Country | Link |
---|---|
US (1) | US7500995B2 (en) |
EP (1) | EP1556308B1 (en) |
JP (1) | JP4435689B2 (en) |
CN (1) | CN1307090C (en) |
AT (1) | ATE324352T1 (en) |
AU (1) | AU2002339757B9 (en) |
BG (1) | BG66487B1 (en) |
BR (1) | BR0215929B1 (en) |
CA (1) | CA2503842C (en) |
CY (1) | CY1105077T1 (en) |
CZ (1) | CZ306507B6 (en) |
DE (1) | DE60211039T2 (en) |
DK (1) | DK1556308T3 (en) |
EA (1) | EA008385B1 (en) |
EG (1) | EG23430A (en) |
ES (1) | ES2261746T3 (en) |
HR (1) | HRP20050374B1 (en) |
HU (1) | HU230118B1 (en) |
IL (1) | IL168185A (en) |
MX (1) | MXPA05004624A (en) |
NO (1) | NO20051857L (en) |
NZ (1) | NZ539890A (en) |
PT (1) | PT1556308E (en) |
RO (1) | RO121775B1 (en) |
SI (1) | SI21742A (en) |
SK (1) | SK287778B6 (en) |
UA (1) | UA80163C2 (en) |
WO (1) | WO2004039722A1 (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2012007331A1 (en) * | 2010-07-16 | 2012-01-19 | Sandvik Materials Technology Deutschland Gmbh | Method for producing tablets containing ammonium nitrate |
WO2015197595A1 (en) | 2014-06-23 | 2015-12-30 | Yara International Asa | Method for producing anhydrous calcium nitrate powder |
WO2017178342A1 (en) * | 2016-04-14 | 2017-10-19 | Yara International Asa | Particulate calcium nitrate composition for fertigation comprising nitrate-based micronutrients and method for production thereof |
EP3348538A1 (en) | 2017-01-16 | 2018-07-18 | YARA International ASA | Calcium nitrate and potassium nitrate fertiliser particles |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
NO20131471A1 (en) * | 2013-11-05 | 2015-05-06 | Yara Int Asa | Solid mortar accelerator accelerator, process for producing such mortar accelerator, dry mortar mix and mortar paste |
DE102014217603A1 (en) * | 2014-09-03 | 2016-03-03 | Sandvik Materials Technology Deutschland Gmbh | Process and apparatus for producing L-menthol in solid form |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB392531A (en) * | 1930-11-01 | 1933-05-16 | Lonza Ag | Process for the production of distributable and non-caking fertilisers containing calcium nitrate |
GB510053A (en) * | 1937-08-04 | 1939-07-26 | Azogeno Soc Anonima | Process for the crystallisation of alkaline earth metal nitrates |
GB768040A (en) * | 1953-11-05 | 1957-02-13 | Norsk Hydro Elek Sk Kvelstofak | Improvements in or relating to the crystallisation of nitrates from nitric acid solutions of calcium phosphate |
US4569677A (en) * | 1983-03-07 | 1986-02-11 | Unie Van Kunstmestfabrieken B.V. | Process for separating off calcium nitrate tetrahydrate by crystallization |
WO2000002831A1 (en) * | 1998-07-08 | 2000-01-20 | Norsk Hydro Asa | Method for manufacturing a calcium nitrate melt and products thereof |
WO2001083374A2 (en) * | 2000-05-03 | 2001-11-08 | Omnia Fertilizer Limited | Method for producing calcium nitrate granules |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE69924169T2 (en) * | 1998-02-27 | 2006-02-02 | Sandvik Intellectual Property Hb | Method and device for drop-shaped application of flowable masses on a conveyor belt |
-
2002
- 2002-01-11 UA UAA200505207A patent/UA80163C2/en unknown
- 2002-11-01 EP EP02778107A patent/EP1556308B1/en not_active Expired - Lifetime
- 2002-11-01 EA EA200500754A patent/EA008385B1/en not_active IP Right Cessation
- 2002-11-01 AT AT02778107T patent/ATE324352T1/en active
- 2002-11-01 SK SK5036-2005A patent/SK287778B6/en not_active IP Right Cessation
- 2002-11-01 SI SI200220044A patent/SI21742A/en not_active IP Right Cessation
- 2002-11-01 BR BRPI0215929-5A patent/BR0215929B1/en not_active IP Right Cessation
- 2002-11-01 MX MXPA05004624A patent/MXPA05004624A/en active IP Right Grant
- 2002-11-01 JP JP2004548172A patent/JP4435689B2/en not_active Expired - Fee Related
- 2002-11-01 NZ NZ539890A patent/NZ539890A/en not_active IP Right Cessation
- 2002-11-01 WO PCT/NO2002/000400 patent/WO2004039722A1/en active IP Right Grant
- 2002-11-01 PT PT02778107T patent/PT1556308E/en unknown
- 2002-11-01 AU AU2002339757A patent/AU2002339757B9/en not_active Ceased
- 2002-11-01 ES ES02778107T patent/ES2261746T3/en not_active Expired - Lifetime
- 2002-11-01 US US10/533,417 patent/US7500995B2/en not_active Expired - Fee Related
- 2002-11-01 CA CA002503842A patent/CA2503842C/en not_active Expired - Fee Related
- 2002-11-01 HU HU0500835A patent/HU230118B1/en not_active IP Right Cessation
- 2002-11-01 CZ CZ2005-315A patent/CZ306507B6/en not_active IP Right Cessation
- 2002-11-01 RO ROA200500397A patent/RO121775B1/en unknown
- 2002-11-01 CN CNB028298349A patent/CN1307090C/en not_active Expired - Lifetime
- 2002-11-01 DK DK02778107T patent/DK1556308T3/en active
- 2002-11-01 DE DE60211039T patent/DE60211039T2/en not_active Expired - Lifetime
-
2003
- 2003-10-28 EG EG2003101006A patent/EG23430A/en active
-
2005
- 2005-04-15 NO NO20051857A patent/NO20051857L/en not_active Application Discontinuation
- 2005-04-21 IL IL168185A patent/IL168185A/en not_active IP Right Cessation
- 2005-04-26 BG BG109137A patent/BG66487B1/en unknown
- 2005-04-27 HR HRP20050374AA patent/HRP20050374B1/en not_active IP Right Cessation
-
2006
- 2006-07-07 CY CY20061100952T patent/CY1105077T1/en unknown
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB392531A (en) * | 1930-11-01 | 1933-05-16 | Lonza Ag | Process for the production of distributable and non-caking fertilisers containing calcium nitrate |
GB510053A (en) * | 1937-08-04 | 1939-07-26 | Azogeno Soc Anonima | Process for the crystallisation of alkaline earth metal nitrates |
GB768040A (en) * | 1953-11-05 | 1957-02-13 | Norsk Hydro Elek Sk Kvelstofak | Improvements in or relating to the crystallisation of nitrates from nitric acid solutions of calcium phosphate |
US4569677A (en) * | 1983-03-07 | 1986-02-11 | Unie Van Kunstmestfabrieken B.V. | Process for separating off calcium nitrate tetrahydrate by crystallization |
WO2000002831A1 (en) * | 1998-07-08 | 2000-01-20 | Norsk Hydro Asa | Method for manufacturing a calcium nitrate melt and products thereof |
WO2001083374A2 (en) * | 2000-05-03 | 2001-11-08 | Omnia Fertilizer Limited | Method for producing calcium nitrate granules |
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2012007331A1 (en) * | 2010-07-16 | 2012-01-19 | Sandvik Materials Technology Deutschland Gmbh | Method for producing tablets containing ammonium nitrate |
US9366485B2 (en) | 2010-07-16 | 2016-06-14 | Sandvik Materials Technology Deutschland Gmbh | Method for producing tablets containing ammonium nitrate |
EA024242B1 (en) * | 2010-07-16 | 2016-08-31 | Сэндвик Материалз Текнолоджи Дойчланд Гмбх | Method for producing tablets containing ammonium nitrate |
WO2015197595A1 (en) | 2014-06-23 | 2015-12-30 | Yara International Asa | Method for producing anhydrous calcium nitrate powder |
WO2017178342A1 (en) * | 2016-04-14 | 2017-10-19 | Yara International Asa | Particulate calcium nitrate composition for fertigation comprising nitrate-based micronutrients and method for production thereof |
EP3348538A1 (en) | 2017-01-16 | 2018-07-18 | YARA International ASA | Calcium nitrate and potassium nitrate fertiliser particles |
WO2018130677A1 (en) | 2017-01-16 | 2018-07-19 | Yara International Asa | Calcium nitrate and potassium nitrate fertiliser particles |
CN111108078A (en) * | 2017-01-16 | 2020-05-05 | 亚拉国际有限公司 | Calcium nitrate and potassium nitrate fertilizer particles |
US11485689B2 (en) | 2017-01-16 | 2022-11-01 | Yara International Asa | Calcium nitrate and potassium nitrate fertiliser particles |
US12103896B2 (en) | 2017-01-16 | 2024-10-01 | Yara International Asa | Calcium nitrate and potassium nitrate fertiliser particles |
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