DE1592581C3

DE1592581C3 - Process for the preparation of a granulated phosphate fertilizer

Info

Publication number: DE1592581C3
Application number: DE19641592581
Authority: DE
Inventors: Ruediger Lothar Von 6200 Wiesbaden Reppert
Original assignee: Individual
Current assignee: Individual
Priority date: 1964-07-02
Filing date: 1964-07-02
Publication date: 1974-07-04
Also published as: DE1592581B2; DE1592581A1

Description

3 43 4

tretende, reaktionsheiße und in einer Korngröße von Teilen befreit. Stündlich werden 5000 kg des Phos-0,15 bis maximal 4 mm, vorzugsweise 0,5 bis 1,5 mm, phates in einem nach dem Schleuder- und Wirbelvorliegende Granulat anschließend einer Kühl- bzw. verfahren arbeitenden großen Mischer mit 5 % Wasser Trockenvorrichtung, vorzugsweise einer Wirbel- befeuchtet und gleichzeitig mit 24 % 9 8°/oiger Schwefelschicht-Apparatur, zugeführt. Die bevorzugte Wirbel- S säure bedüst.stepping, reactive hot and freed from parts in one grain size. Every hour 5000 kg of Phos-0.15 up to a maximum of 4 mm, preferably 0.5 to 1.5 mm, phates in one after the spinning and vortexing Granulate then a cooling or process working large mixer with 5% water Drying device, preferably a vortex humidified and at the same time with 24% 9 8% sulfur layer apparatus, fed. The preferred eddy acid spray.

schicht-Apparatur ist in besonders vorteilhafter Weise Der im Mischer erfolgende Misch-,'Aufschließals Mehrkammer-Wirbelschicht-Apparatur ausgebil- und Granuliervorgang ist bereits nach wenigen Sedet: Sie besteht aus einem waagerechten Behälter, künden beendet, und die reaktionsheiße, noch etwas in den gegeneinander versetzte, unmittelbar auf dem feuchte Masse wird dann einer Mehrkammer-Wirbel-Siebboden aufsitzende Zwischenwände eingesetzt sind. io schicht-Apparatur, wie sie vorstehend bereits be-Durch den Siebboden wird von unten her Luft in die schrieben wurde, zugeführt, in der das Material Kammer eingeblasen; über dem Siebboden und zwi- gekühlt wird. Nach Durchlauf en dieser Mehrkammerschen den einzelnen Trennwänden befinden sich Wirbelschicht-Apparatur liegt das gleichmäßig ge-Schaufelwellen, die das von der eingeblasenen Luft körnte Produkt in einer Korngröße zwischen 0,75 aufgewirbelte Material ständig umwenden und von 15 und 2 mm vor, es ist schon so rieselfähig, daß es ent-Kammerabschnitt zu Kammerabschnitt weiterbeför- weder direkt auf Lager gelegt, in Silos gebracht oder dem. Nach Verlassen dieser Mehrkammer-Wirbel- direkt in Säcke abgefüllt werden kann.
schicht-Apparatur liegt das aufgeschlossene und ab- Die Zusammensetzung des erhaltenen Phosphatgekühlte Material in einer Korngröße von 0,15 bis Düngemittels beträgt 28,5% Gesamt-P₂O₅, 14,6% 4 mm vor, wobei etwa 90% in einer Körnung von 20 citronensäurelösliches P₂O₅, 8,2% citratlösliches 0,5 bis 1,5 mm anfallen. Pa^s» 7,7% wasserlösliches P₂O₅, 2,1% freie Säurelayer apparatus is particularly advantageous.The mixing, opening up as a multi-chamber fluidized bed apparatus and granulating process takes place after just a few steps: it consists of a horizontal container, which is finished, and the hot, reactive one, something else in the offset against each other, directly on the moist mass is then a multi-chamber vortex sieve bottom seated partition walls are used. io layer apparatus, as it has already been described above. Air into which the air was written is fed through the sieve bottom from below, into which the material chamber is blown; above the sieve bottom and is cooled. After passing through these multi-chamber the individual partition walls there is a fluidized bed apparatus, the evenly ge-blade waves, which constantly turn over the material whirled up by the blown air with a grain size between 0.75 and 15 and 2 mm, it is already so free-flowing that it is transported from one chamber section to the next, neither placed directly in storage, put in silos or the. After leaving this multi-chamber vortex, bags can be filled directly.
The composition of the phosphate-cooled material obtained in a grain size from 0.15 to fertilizer is 28.5% total P ₂ O ₅ , 14.6% 4 mm, with about 90% in one Granules of 20 _{citric acid-soluble P 2} O ₅ , 8.2% citrate-soluble 0.5 to 1.5 mm. Pa ^ s »7.7% water soluble P ₂ O ₅ , 2.1% free acid

Das Rohphosphat kann auch gemeinsam mit und 1,8% Wasser.The rock phosphate can also be combined with and 1.8% water.

Schädlingsbekämpfungsmitteln, wie DDT, mit weite- Auch bei diesem Produkt zeigt sich, daß nach einerPesticides, such as DDT, with wide- Also with this product it is shown that after one

ren Makro- oder Mikronährstoffen verarbeitet wer- Lagerung von mehreren Stunden der Gehalt an freierThese macro- or micronutrients are processed storage of several hours of the content of free

den, soweit diese Zusätze unter den gegebenen Be- 25 Säure und Wasser weiter zurückgeht, und zwar nachto the extent that these additions continue to decrease under the given conditions of acid and water, namely by

dingungen beständig sind. Gegebenenfalls führt man einer Lagerzeit von 5 Stunden auf 1,3 bzw. 1,5%.conditions are stable. If necessary, a storage time of 5 hours leads to 1.3 or 1.5%.

die Behandlung in einem Mehrkammer-Mischer _B . . „treatment in a multi-chamber mixer _B. . "

durch, wie beschrieben. ü e 1 s ρ 1 e i .5through as described. ü e 1 s ρ 1 e i .5

. In einem durch zwei Stauwände aufgeteilten und Beispiel 1 _{30 son}ü_{t aus} ^rei Abteilungen bestehenden, kontinuier-Ungemahlenes 75er Marokkophosphat wird durch lieh nach dem Schleuder- und Wirbelverfahren arbeiein 3-mm-Sieb abgesiebt. Es bleiben dabei 2,5 % an tenden Mischer werden in der ersten Kammer, bei über 3 mm großen Phosphatteilchen auf dem Sieb der die Stauwand bis etwa zur halben Höhe des zurück; sie werden durch einen einfachen Brechvor- Innenraumes reicht, pro Minute 44 kg eines Marokkogang zerkleinert und dadurch in die zur Durchfüh- 35 phosphates (32% P₂O₅), das durch Absieben durch rung des Verfahrens geeignete Korngröße gebracht. ein 1 72-mm-Sieb von den gröberen Anteilen befreit 5 kg dieses Rohphosphates werden in einem nach worden ist, mit 25 kg Chlorkali (56% K₂O) unter Zudem Schleuder- und Wirbelverfahren arbeitenden, satz von 3% = 2,07 kg Wasser und 25% = 17,25 kg kleinen Mischer innerhalb von 10 Sekunden mit 96%iger Schwefelsäure, beides bezogen auf das Ge-655 ml Schwefelsäure vom spezifischen Gewicht 1,84 40 misch Rohphosphat + Kali, innig vermischt. Die dainnig vermischt und das dabei sofort entstandene bei erhaltene Reaktionsmasse wird in der zweiten Granulat noch etwa 10 Sekunden nach Beendigung durch die beiden Stauwände gebildeten mittleren des Mischvorganges im Mischer weiterbehandelt. Kammer mit 31kg Harnstoff innig vermischt und Die dabei erhaltenen, reaktionsheißen Granalien dieses Produkt in der dritten durch die zweite Stauwerden sofort einem Wirbelschichtkühler zugeführt 45 wand und die Mischerwand gebildeten Kammer durch und in diesem etwa 25 Sekunden einer Luftkühlung Zugabe von etwas Ammoniak durch eine in den unterworfen. Sie verlassen den Wirbelschichtkühler Boden dieser Kammer versenkte Düse geringfügig weitgehend gekühlt und besitzen eine Korngröße von nachammonisiert, um eventuell anhaftende freie Säure 0,5 bis 3,5mm. Die Analyse ergibt: 28,2% Gesamt- zubinden.. In a split by two walls and storage Example 1 _{30 son} ü ^ rei consisting _of departments, kontinuier-Unground _t 75er Morocco phosphate is sieved through borrowed after the spinning and whirling process arbeiein 3-mm screen. There are 2.5% of the mixer in the first chamber, with phosphate particles over 3 mm in size on the sieve of the retaining wall up to about half the height of the back; They are passed through a simple internal crushing area, 44 kg of a Moroccan gang per minute are crushed and thereby converted into the phosphate (32% P ₂ O ₅ ) that is suitable for the grain size by sieving through the process. A 1,72 mm sieve is freed from the coarser fractions. 5 kg of this rock phosphate are removed in one go, with 25 kg of potassium chloride (56% K ₂ O) using a centrifugal and vortex process, a rate of 3% = 2.07 kg water and 25% = 17.25 kg small mixer within 10 seconds with 96% sulfuric acid, both based on the Ge-655 ml sulfuric acid with a specific gravity of 1.84 40 mixed rock phosphate + potash, intimately mixed. The dainnig mixed and the resulting reaction mass immediately obtained is further treated in the second granulate about 10 seconds after the end of the middle of the mixing process formed by the two retaining walls in the mixer. Chamber with 31kg urea is intimately mixed and the resulting, hot reaction granules of this product in the third through the second accumulation are immediately fed to a fluidized bed cooler 45 wall and the mixer wall formed through the chamber and in this about 25 seconds of air cooling adding some ammonia through an in the subject. You leave the fluidized bed cooler bottom of this chamber, the sunken nozzle is slightly largely cooled and have a grain size of post-ammoniated to prevent any adhering free acid from 0.5 to 3.5 mm. The analysis shows: 28.2% total binding.

P₂O₅, 15,1% citronensäurelösliches P₂O₅, 8,4% 50 Die so erhaltene, reaktionsheiße Masse gelangtP ₂ O ₅ , 15.1% citric acid-soluble P ₂ O ₅ , 8.4% 50 The reaction-hot mass obtained in this way arrives

citratlösliches P₂O₅, 8,1% wasserlösliches P₂O₅ sowie nach Verlassen des Mischers wieder unmittelbar incitrate-soluble P ₂ O ₅ , 8.1% water-soluble P ₂ O ₅ and immediately after leaving the mixer again in

anfangs noch einen Gehalt an freier Säure von 1,2% eine Mehrkammer-Wirbelschicht-Apparatur und wirdinitially still a free acid content of 1.2% a multi-chamber fluidized bed apparatus and is

und einen Wassergehalt von 1,5 %. dort abgekühlt bzw. getrocknet.and a water content of 1.5%. there cooled or dried.

Das so erhaltene Produkt läßt man jetzt noch Nach Verlassen dieser Vorrichtung erhält man ein 1 Stunde ablagern, wobei der Gehalt an freier Säure 55 etwa 1 bis 3 mm großes Granulat der Zusammenauf unter 1%, der Wassergehalt auf nahezu 1% ab- Setzung 14% N, 14% P₂O₅ und 14% K₂O bei einem sinkt. Die Granalien liegen nunmehr bereits in einer Wassergehalt von 0,7 %.The product obtained in this way is now left to settle after leaving this device for 1 hour, the content of free acid 55 granules about 1 to 3 mm in size amounting to less than 1%, the water content to almost 1%, 14% N, 14% P ₂ O ₅ and 14% K ₂ O at one drops. The granules now have a water content of 0.7%.

rieselfähigen Form vor, so daß sie ohne weiteres ver- Das erhaltene Produkt ist abriebfest, riesel-, streupackt werden können, und verpackungsfähig. Es kann daher sofort einge-_Ώ ... 6υ lagert oder in Säcke verpackt werden, wobei es vor-Beispiel 2 teilhaft ist, Säcke mit Polyäthylen- oder Bitumen-Vorgebrochenes Pebblephosphat mit 34,5 % P₂O₅ Einlage zu verwenden, mit Rücksicht auf die durch wird durch ein Sieb von allen über 2 mm großen den Harnstoffzusatz bedingte Hygroskopizität.free-flowing form, so that they can easily be The product obtained is abrasion-resistant, free-flowing, litter-packed, and packable. Therefore, it can immediately einge- _Ώ ... 6υ stored or packed in sacks, whereby it is part way before Example 2, bags with polyethylene or bitumen pre-crushed Pebble phosphate 34.5% P ₂ O ₅ to use insert with Consideration of the hygroscopicity caused by the addition of urea through a sieve of anything over 2 mm in size.

Claims

are not available. In addition, the

Claim: bene fine grinding unnecessary.

It is also possible to add all rock phosphates

Method of making a granulated use, not just preferably soft-earthed, such as

Phosphate fertilizer by treating un- 5 them according to the German Au:; Legeschrift 1125 454

ground rock phosphate with mineral acid come primarily into consideration. One can also

one after the centrifugal and vortex principle with hard phosphates, z. B. Pebble, work, and it

working mixer, thereby identified, is required in the extreme case, the parts that

draws that by sieving over coarser than 3 mm, one can briefly break off. It can

3 mm large particles of freed rock phosphate with i ° also poorly digestible phosphates, such as KoIa

about 15 to 35 weight percent concentrated phosphate, can be processed in the same manner.

Sulfuric acid and / or phosphoric acid and / or Furthermore, it has been found that it is not necessary

Treated nitric acid, after which the obtained is borrowed, the vortex curtain apparatus according to patent

Product is cooled and dried. 1 036 876 to use, but that it is in principle

15 is possible to use any apparatus that can be used according to

the same scheme works. Is preferred

a multi-chamber fluidized bed apparatus,

The invention relates to a method for the manufacture, which will be described in detail later,
Finally, and that is another significant treatment of unground rock phosphate with advances, it has been found that it is not essential to the mineral acid in an after centrifugal and the final product on the mixer operating in Section I of the vortex principle . named grinding fineness according to the German Auslege-In German Auslegeschrift 1 125 454 a script 1 125 454 is to be brought, and it was found in the process for the production of finely powdered phosphate opposite that a non-ground, grading agent described, the product graded according to the following steps 25 a surprisingly good plant work: possesses physiological effectiveness. Practical tests based on the centrifugal or vortex principle have shown that a mixer that is no longer working will give rock phosphate with a ground end product according to the present invention grain size of a maximum of 1 mm with such amounts of manure considerably better yields than a fine mineral acid treated so that there is an approximately 30 milled partial digestion according to the German Auslegeschrift 50% iiger. , 1 125 454 of the same composition.

In the second stage, the reaction-warm According to the present invention, both digestion product in a phosphoric acid fertilizer charged with cooling air and also multi-nutrient vortex curtain apparatus can be produced in a known manner in fertilizers. In the case of the cooled and dried. In the third stage, the now dry substances can also be added unground salts - product is set to a grinding fineness of 90% passage, from which the over 3 mm pass through a DIN sieve 40 to 100% passage through proportions have been separated by sieving.
Sieve DIN 100 finely ground. Since the mixing with these salts and the object of the present invention is the 40 addition of the sulfuric acid not in every case the same method described in a number of points is possible in a number of points - for example, would be advantageous to modify and thereby a granular nature of ammonium nitrate by the addition To gain fertilizers. nitrogen oxides escape from sulfuric acid - it has been found that granulated phosphate is expedient, in these cases initially only the raw fertilizer! by treating unground phosphate with sulfuric acid in the mixer that works after the rock phosphate with mineral acid in a mixer that works according to the centrifugal and vortex principle.

can be obtained by sieving this is possible if the mixer is built in

Rock phosphate freed over 3 mm particles of a retaining wall is designed in such a way that sulfuric acid

with about 15 to 35 percent by weight of concentrated 5 ° and rock phosphate are initially vennisched for themselves

Sulfuric acid and / or phosphoric acid and / or and then, after crossing the barrier, im

Treated nitric acid, after which the obtained pro- other part of the mixer with the other salts,

product is cooled and dried, which may also be added in the form of melts

According to the German Auslegeschrift 1 125 454 it can be given, mixed and finished

known, powdery to fine-grained rock phosphate is granulated with 55.

such amounts of mineral acid, the maximum one Instead of sulfuric acid, one can also use phosphorus

Effect 50% partial digestion, treat or phosphoric acid or nitric acid or mixtures of these

to mix intimately. Use acids, depending on the fertilizer

So this is a short-term one wants to generate.

Mixing process and no granulation, as this after 6 ° Is also an additional ammonization of the

the present proceedings. If the granulation is desired, this can also be done in the

but it is of the joy of granulating and that its mixer takes place when it consists of three through stowage walls *;

. on the other hand, there is again a sufficient content of separate parts, with im

Water and free acid dependent, but then also in the last section the ammonization by introducing

of the sufficient duration of the granulation of ammonia or ammoniacal

initiating movement in the ammonium nitrate solution used for this in the granulate, if necessary

Apparatus. Conditions and measures can therefore be carried out with the addition of further sulfuric acid,

like this one in the German Auslegeschrift 1 125 454 In any case, this is removed from the mixer