CA1106154A - Granulation of potash salts - Google Patents

Granulation of potash salts

Info

Publication number
CA1106154A
CA1106154A CA288,799A CA288799A CA1106154A CA 1106154 A CA1106154 A CA 1106154A CA 288799 A CA288799 A CA 288799A CA 1106154 A CA1106154 A CA 1106154A
Authority
CA
Canada
Prior art keywords
binder
phosphate
potassium
potash
potash salt
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
Application number
CA288,799A
Other languages
French (fr)
Inventor
William B. Dancy
Kenneth L. Nichols
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
International Minerals and Chemical Corp
Original Assignee
International Minerals and Chemical Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by International Minerals and Chemical Corp filed Critical International Minerals and Chemical Corp
Application granted granted Critical
Publication of CA1106154A publication Critical patent/CA1106154A/en
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00Sulfates or sulfites of sodium, potassium or alkali metals in general
    • C01D5/12Preparation of double sulfates of magnesium with sodium or potassium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/28Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic using special binding agents
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00Halides of sodium, potassium or alkali metals in general
    • C01D3/22Preparation in the form of granules, pieces, or other shaped products
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00Sulfates or sulfites of sodium, potassium or alkali metals in general
    • C01D5/004Preparation in the form of granules, pieces or other shaped products
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D7/00Carbonates of sodium, potassium or alkali metals in general
    • C01D7/38Preparation in the form of granules, pieces or other shaped products
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D9/00Nitrates of sodium, potassium or alkali metals in general
    • C01D9/18Preparation in the form of shaped products, e.g. granules
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C5/00Fertilisers containing other nitrates
    • C05C5/005Post-treatment
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05DINORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D1/00Fertilisers containing potassium
    • C05D1/005Fertilisers containing potassium post-treatment

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Fodder In General (AREA)
  • Fertilizers (AREA)
  • Glanulating (AREA)

Abstract

ABSTRACT
A process for the granulation of potash salts to produce granules in high yield by the steps of mixing the potash salt with an inorganic phosphate binder and water, granulating the mixture and drying it.

Description

i~CI 6159L

GRANULATION OF POT~SH SALTS
This invention relates to the granulation of potash salts. In a particular aspect this invention relates to the granulation of potash salts by incorporation of a binder prior to the granulation step.
Potash salts do not easily form large crystals or particles, yet they are needed for use in mixed fertilizers to prevent segregation. Also particles in the desired size range must be strong enough to resist degradation during handling and mixing steps. However, due to lack of plas-ticity, potash salts resist granulation by conventional rotary drum or pan granulators. Granules formed in these devices lack degradation resistance when dried and the yield of granules in the desired 6 x 14 mesh Tyler size range is low, e.g. frequently in the 10% range. Conse quently, recycle rates are very high resulting in exor-bitant production costs.
Thus there is a need for a process for granulating potash salts in high yield in the desired granulation range which will have good structural stability during storage, handling and use.
It is an object of this invention to provide a process for the granulation of potash salts.
It is another object of this invention to provide a process for the granulation of potash salts by incor-porating therein a binder.
Yet another object is to provide a composition of potash salt and binder in granulated form.
Other objects will be apparent to those skilled in the art from the disclosure herein.
-2-~ ~61S4 It is the discovery of this invention to provide a process for the granulation of potash salts to produce granules in high yield in the desired size range by the step of mixing the potash salt with an inorganic phosphate salt binder and water, and granulating the mixture and drying it.
In the process of the present invention the potash salt is mixed with the phosphate binder in a ratio of about 30-300 lb (1.5 to 15~) preferably about 100-300 lb (5 to 15% of binder per ton of crystals; the amount re-quired is variable, depending on the binder selected and the material to be granulated. Water is added, either before or after mixing the potash salt with the binder, in an amount of 150-400 lb per ton of mixture (7.5 to 20%), the exact amount depending on the moisture content, the type and particle size of the potash and binder being used in the operation. The mixing is carried out in a conven-tional drum or pan granulator and additional water can be added as required to maximize the production of the pre-ferred size granules. The preferred water content is fromabout 10 to about 15%. The mixture is then fed to a con-ventional dryer.
The potash salts which can be granulated by the process of this invention include but are not limited to potassium chloride, potassium carbonate, potassium sulfate, potassium nitrate, langbeinite, and mixtures thereof.
Suitakle binders include monoammonium phosphate, diammonium phosphate, mono- or disodium phosphate, mono-or dipotassium phosphate, or a mixture thereof. Also di-basic magnesium phosphate is a suitable binder. All of 1~`615~

these compounds are known in the art and most of them arecommercially available. The usual commercial grades are suitable for the practice of this invention.
A preferred binder is monoammonium phosphate which can be suitably formed at the time of use. A particularly preferred binder is a mixture of mono- and diammonium phosphates obtained by reacting ammonia with phosphoric acid in a mole ratio of about 1.1-1.5 to 1. Mono- or di-ammonium phosphate, or mixture thereof, can be formed in situ by premixing the potash salt with a suitable amount of phosphoric acid, then ammoniating the mixture in an ammoniator-granulator known in the art, e.y. a TVA rotary-drum granulator as described by F . T . Nielsson, U.S.
Patents 2,729,554 and 2,741,545. A preferred source of phosphoric acid is the grade known as wet-process acid because it contains a minor amount of iron, aluminum and other metallic impurities which improve the strength of the potash granules. When the monoammonium phosphate is formed in situ, water is preferably added to the potash salt prior to introduction of the phosphoric acid. The ammoniation step can be carried out preferably with anhydrous ammonia, but aqua am~onia can also be used if desired. ~n this case the amount of water added as aqua ammonia should be taken into consideration when adding additional water for the granulation step.
When magnesium phosphate is to be used as the binder, it can also be conveniently formed in situ during the granulation step. The magnesium is added to the potash salt as the oxide, hydroxide or carbonate and phos-phoric acid - preferably wet process phosphoric acid - is 111t~6~54 sparged into the mixture. me magnesium compound and phos-phoric acid are used at a mole ratio, generally, of between 0.5-1.5:1, preferably 1:1.
When langbeinite is to be granulated, it is prefer-ably in a form wherein it contains at least 20% of minus 200 mesh Tyler size granules and a minimum amount of plus 30 mesh granules, preferably less than 5%.
Another embodiment of this invention is that gran-ulation of other potash salts than langbèinite can be enhanced by adding a small amount of pulverized langbeinite or other suitable source of magnesium to the potash. Such suitable sources of magnesium include, in addition to the magnesium phosphate cited above, the oxide, the chloride, the sulfate, the carbonate, the nitrate,~etc. Langbeinite is used at a rate of 30-70 lb per ton of potash salt.
Other magnesium salts are used at a rate equivalent to 20-40 lb of magnesium sulfate per ton of potash sal~.
The granulation step is carried out in the conven-tional manner at the conventional temperatures, e.g. from 160 to 200~F. Similarly the drying step i9 carried out in the conventional manner.
In accordance with the foregoing, it is an embodi-ment of this invention to provide a composition adapted for granulation comprising a potash salt and an inorganic phosphate binder. More particularly, it is an embodiment of this invention to provide a composition suitable for granulation comprising a potash salt, an inorganic phos-phate binder therefor in an a unt of about 30-300 lbs per ton of potash salt and water in an amount of about 150-400 lb per ton of potash salt wherein the potash salt ~1~6~S4 is potassium chloride, potassium sulfate, potassium car-bonate or langbeinite or mixtures thereof. Preferred mixtures include those wherein langbeinite is a minor component. The inorganic phosphate is supplied by mono-or diammonium phosphate, mono- or disodium phosphate, mono- or dipotassium phosphate or mono- or dibasic magne-sium phosphate or mixtures thereof. It is also contem-plated that another embodiment of this invention is to provide granulated compositions of the foregoing materials having a composition, d y basis, of from about 85-98.5%
potash salt and 15-1.5% binder, respectively. In addi-tion, the granulated composition may contain residual water of varying amounts, although usually the composition will be substantially water-free.
The invention will be better understood by refer-ring to the following examples. These examples are intended merely to illustrate the invention and it is not intended that the invention be limited thereby.

Example l ; Langbeinite fines were obtained from a dust collec-tor and were used for granulation. It analyzed 5% plus 35 mesh and 26% minus 200 mesh. The granulator was run at 15 tons/hour, using 300 lbs of a mixture of mono- and di-ammonium phosphate per ton of langbeinite. The ammonium phosphate was formed in situ by introducing wet process phosphoric acid in the appropriate proportions and ammon-iating the mixture at a mole ratio of about 1.5 moles anhydrous ammonia per mole of phosphoric acid.

Granulation was carried out in a TVA rotary-drum ammoniator (F. T. Nielsson U.S. Patents 2,729,554 and 2,741,545). Water was added as necessary to provide good granulation characteristics. The granulator drum was operated at a temperature of 178-182F. The moisture content of the granulated product as it exited from the granulator was 14~. It was then sent to a drier having an inlet temperature of 980 to 1020F. The temperature of the exit gases was 200-225F and that of the dried product was 110-120F.
Satisfactory granulation was obtained as shown by the screen analysis in Table 1.

ll~`G~5~a o ~r o ~D

~D
o o o o In .

o ~ O a~ :

a ~ O~ -~ .
,~ ~ ~ ~ o E~ o .
o ~ ~
- ~ ,` ,f, a~
CO ~D ~

". CO
o ô

aJ
r~
U~ ~ ~
U~ ~o ~ o o ~ o ,, ~ ,, o ~ o 'd ~:: o ~: o .
.

lS~

Degradation tests were performed and it was found that 8.4% degradation occurred. This compares favorably with the degradation rate of granular potassium sulfate and diammonlum phosphate. The physical quality of the product was acceptable.

Example 2 The experiment of Example 1 was repeated in all essential details except that the mono- and diammonium phosphate content was reduced to 100 lb/ton. Satisfactory granulation was obtained as shown by the screen analysis in Table 1. In degradation tests, there was a 7.4%
degradation of the granules. Physical quality was accept-able.

Example 3 Potassium chloride, 1 ton, is mixed with mono-ammonium phosphate, 100 lb, and water, 200 lb (10%), in a pan granulator and granulated at 180~F as is known in the art. The material exiting the granulator i9 dried, cooled and delivered to storage. The physical quality is accept-able.

;

Example 4 The experiment of Example 3 is repeated in all essential details except that potassium carbonate is sub-stituted for potassium chloride, diammonium phosphate is substituted for monoammonium phosphate and 20~ water is added. The physical quality of the granules is satisfactory.

.
_g_ 1~6~L5~

Example 5 The experiment of Example 3 is repeated in all essential details except that potassium sulfate is sub-stituted for potassium chloride, monosodium phosphate, 30 lb/ton, is substituted for monoammonium phosphate and 7.5%
water is used. The physical quality of the granules is acceptable.

Example 6 The experiment of Example 3 is repeated in all essential details except that potassium nitrate is sub-stituted for potassium chloride and monopotassium phos-phate, 100 lb/ton, is substituted for monoammonium phos-phate. The physical quality of the granules is acceptable.

Example 7 The experiment of Example 1 is repeated in all - essential details except that disodium hydrogen phosphate is substituted for ammonium phosphate. The physical quality of the granules is acceptable.

Example 8 The experiment of Example 7 is repeated in all essential details except that dipotassium hydrogen phos-phate is substituted for disodium hydrogen phosphate.

The physical quality of the granules is acceptable.

.:

,~ -10-LS~

Example 9 The experiment of Example 3 is repeated in all essential details except that langbeinite is substituted for ammonium phosphate. The physical quality of the granules is acceptable.

Example 10 The experiment of Example 1 is repeated in all essential details except that potassium chloride is sub-stituted for langbeinite and magnesium oxide is substi-tuted for ammonia in an amount to provide an equi-molar ratio with the phosphoric acid. The physical quality of the resulting granules is acceptable.

Claims (22)

The embodiments of the invention in which an exclusive property or privilege is claimed are defined as follows:
1. A process for the granulation of potash salts selected from potassium chloride, potassium sulfate, potassium carbonate, potassium nitrate, langbeinite, and mixtures thereof, comprising the steps of (a) mixing the potash salt with a mono- or di- basic ammonium, potassium or sodium phosphate binder or a dibasic magnesium phosphate binder or mixtures thereof, and water, said potash salt being mixed with said binder in a ratio of about 30-300 lb. per ton of crystals, and the amount of water added ranging from 150 to 400 lb. per ton of mixture;
(b) granulating the mixture; and (c) drying it; said process including the feature that when said potash salt is other than langbeinite, an amount of langbeinite, ranging from 30-70 lb.
per ton of potash salt, and/or another source of magnesium selected from magnesium chloride, magnesium sulfate, magnesium carbonate, magnesium nitrate, and magnesium oxide, in an amount equivalent to 20-40 lb. of magnesium sulfate per ton of potash salt, is mixed with the potash and the binder.
2. The process of claim 1 wherein the binder is used in an amount of about 100 to 300 lb per ton of potash salt.
3. The process of claim 1 wherein the potash salt is potassium chloride.
4. The process of claim 1 wherein the potash salt is potassium nitrate.
The process of claim 1 wherein the potash salt is potassium sulfate.
6. The process of claim 1 wherein the potash salt is potassium carbonate.
7. The process of claim 1 wherein the potash salt is langbeinite.
8. The process of claim 1 wherein the binder is monoammonium phosphate.
9. The process of claim 1 wherein the binder is diammonium phosphate.
10. The process of claim 1 wherein the binder is monopotassium phosphate.
11. The process of claim 1 wherein the binder is dipotassium phosphate.
12. The process of claim 1 wherein the binder is monosodium phosphate.
13. The process of claim 1 wherein the binder is disodium phosphate.
14. The process of claim 1 wherein langbeinite, and another source of magnesium selected from magnesium chloride and magnesium nitrate is mixed with the potash and the binder.
15. A process for granulating langbeinite comprising the steps of delivering the langbeinite to a granulator; adding from 7.5 to 20% water; adding a mixture of mono- and diammonium phosphates obtained by reacting ammonia and phosphoric acid in a mole ratio of about 1.1-1.5:1, said mixture of mono- and diammonium phosphates being employed in an amount ranging from 30 to 300 lb. per ton of crystals; granulating the mixture thereby obtained; and drying same.
16. The process of claim 15 wherein the phosphoric acid is wet process phosphoric acid.
17. The process of claim 15 wherein the mixture of mono- and diammonium phosphates is formed in situ.
18. A composition adapted for granulation comprising a potash salt and an inorganic binder in which the potash salt is potassium chloride, potassium nitrate, potassium sulfate, potassium carbonate, langbeinite or mixtures thereof, and wherein the phosphate binder is mono- or diammonium phosphate, mono- or disodium phosphate, mono- or dipotassium phosphate, or mixtures thereof, the ratio of said phosphate binder to said potash salt ranging from about 30 to 300 lb.
binder per ton of crystals.
19. A granulated composition comprising 85 to 98.5% potash salt selected from potassium chloride, potassium sulfate, potassium carbonate, potassium nitrate, langbeinite, and mixtures thereof, and 15 to 1.5% of a mono- or dibasic ammonium, sodium or potassium phosphate binder, or a mixture thereof.
20. The composition of claim 18 wherein the potash salt is langbeinite and the binder is a mixture of mono- and diammonium phosphates formed by reacting ammonia and phosphoric acid in a mole ratio of about 1.3-1.7 to 1.
21. The composition of claim 19 wherein the potash salt is potassium sulfate or potassium nitrate.
22. The composition of claim 18 wherein the ratio of said phosphate binder to said potash salt ranges from about 100 to 300 lb.per ton of crystals.
CA288,799A 1976-12-02 1977-10-14 Granulation of potash salts Expired CA1106154A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US74665876A 1976-12-02 1976-12-02
US746,658 1976-12-02

Publications (1)

Publication Number Publication Date
CA1106154A true CA1106154A (en) 1981-08-04

Family

ID=25001785

Family Applications (1)

Application Number Title Priority Date Filing Date
CA288,799A Expired CA1106154A (en) 1976-12-02 1977-10-14 Granulation of potash salts

Country Status (5)

Country Link
BE (1) BE861386A (en)
CA (1) CA1106154A (en)
DE (1) DE2748220A1 (en)
FR (1) FR2372654A1 (en)
IT (1) IT1090600B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104876246A (en) * 2014-02-27 2015-09-02 莱州诚源盐化有限公司 A producing method of industrial large-granule salt

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2446595B1 (en) * 1979-01-17 1987-07-17 Rocchesani Nicolas OUTDOOR-CONDUCTED BEE BREEDING AND FEEDING TRAY FOR INTENSIVE BEEKEEPING
IT1174208B (en) * 1984-06-19 1987-07-01 Italkali PROCEDURE FOR THE PRODUCTION OF POTASSIC SULPHATE AND MAGNESIA POTASSIC SULPHATES GRANULATED, AND GRANULATED SO PRODUCED
DE102016010584A1 (en) * 2016-09-02 2018-03-08 K+S Aktiengesellschaft Process for the preparation of potassium chlorite granules
DE102016010586A1 (en) 2016-09-02 2018-03-08 K+S Aktiengesellschaft Process for the preparation of potassium chloride granules
DE102016010585A1 (en) * 2016-09-02 2018-03-08 K+S Aktiengesellschaft Process for the preparation of potassium chlorite granules
DE102017125467A1 (en) * 2017-10-30 2019-05-02 K+S Aktiengesellschaft Process for the preparation of granules containing potassium, magnesium and sulfate
DE102017010086A1 (en) * 2017-10-30 2019-05-02 K+S Aktiengesellschaft Granules containing polyhalite

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE392952C (en) * 1922-07-21 1924-03-25 F Quade Dr Process for the production of a water non-attractive mixed fertilizer from calcium nitrate
GB389082A (en) * 1930-07-05 1933-02-27 Ruhrchemie Ag Process for the production of mixed salts containing ammoniacal and nitrate-nitrogen jointly
FR722708A (en) * 1930-09-10 1932-03-24 Kali Forschungsanstalt Gmbh Improvements in processes for obtaining mixed granulated fertilizers
FR1044243A (en) * 1951-10-29 1953-11-16 Saint Gobain Fertilizer granulation process
IL23702A (en) * 1965-06-09 1968-10-24 Hamelah M Granulated potassium chloride and process of producing it

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104876246A (en) * 2014-02-27 2015-09-02 莱州诚源盐化有限公司 A producing method of industrial large-granule salt

Also Published As

Publication number Publication date
BE861386A (en) 1978-03-31
DE2748220A1 (en) 1978-06-08
FR2372654A1 (en) 1978-06-30
IT1090600B (en) 1985-06-26

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