LU81236A1 - PROCESS AND PLANT FOR THE MANUFACTURE OF PELLET FERTILIZERS - Google Patents

Description

V. * 7,. 501 2.-ΠΪ5 ον

. GRAKD-DUCHE DE LUXEMBOURG

....... 3 5 Λ du · Lu. '. M .................... MÂ.0 Minister, 5¾¾¾ of the Economy National and Movennes Classes

Book title: ........................................ h ȕ-% j psr -m3; j Industrial Property Service

~ LUXEMBOURG

jÙd / 1 &, v —J ----------------- Application for Patent of invention, t U. ”............... .................................................. ....

I. Request

The Belgian anonyiiie society called: rSociété de Pr ay on. ", P department., (1) .ÎJlit, ...... Belgium, ..... represented ..... D a r ... Mg n sie u r ... C har 1 e s ..... München, ...............

.cens eil en patentes à L uxeubgurg, api ssant ... en c np.l J. ts de, 2) 3.ΆΆ data ire ................... .................................................. .................................................. .................................................. ..................................................

remove ........ this ........... badly new ...... 1500. soi xarits-dix-nguf ............................................ ......... (3) at ...... 1 ..? .. hours, at the Ministry of National Economy and the Middle Classes, in Luxembourg: 1. this request for the obtaining a patent for an invention concerning: “Process and in s ta 11 a ticn pour 1 a fgbri cat Ion ... d1 s nq.r§.j. s .........., -4) .. granulated ", ......

declares, assuming responsibility for this declaration, that the inventor (s) is (are): .Mgdi .u.r: ΐΧΜΜ.ί 17. h. "111 Il IJl'SJL · .. ..ly at ii.lA.1. Dyprle., ..... !! - JB f5) ..1.11.31.5 ...... iclpipu ..? .. .................................................. .................................................. .................................................. .................................................. ..........

2. the delegation to move. dated, from ........ 1. it —.'.... t.T. on .1 ..ÛL..1 i..T ...: .... T .................

f a *% r Us S. Is description in language______________________________; —1 ........................... this rcnvenron in two exenepiai-es; 4 .......... 1 ................... drawing boards, in two copies; 5. the auittance of the taxes paid to the Bureau de -'Enreriserement in Luxembourg,

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îolîicite the delin umnre hard: patent c'uueuuue fear the cb .'- a: described and lerrémnté in las a.- ·. ··. · -s e ‘* * mm; i sustsenflormâas. - avee ε-ourr-sr-ant de vc-tie cxuvrxuaa a .... u.uû .... ..... y. ; s.

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Read the aforesaid patent ducuxmtmu ε been ùuru: ru Γl: r. '. SMre de IxEeoconvs Z'rü.uua and these Medium Classes, Service de la Prmviuâ Industrielle at uvxmrrovrg. dated: D - -5 '.

U .x -. „. „/" Br. Le Imbire

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| DESCRIPTIVE MEMORY

i! · Filed in support of a request for Γ d.

|: PATENT D1 INVERTION

i on behalf of the public limited company known as "Société de Prayon" for: "Process and installation for the manufacture of granular fertilizers".

: Inventor: Armand DAVISTER.

The present invention relates to a process for the manufacture of granulated fertilizers, in particular ternary fertilizers.

1 There are essentially two distinct manufacturing processes and this granulation of ternary fertilizers, a process -next! which starts with powdery raw materials sema — rances: r-. î— f - es 1 1 -¾ - ---- m —-> · - * s c? "'- * r * t ^" 1 n. in "rv * 1 · λ · - Iras se r.nn Ί 1 ^; t ς

Tja Γ3 L Co. ’ii. ΟΠ G f Θ ^ CTiT B i. S ‘ΟθίΓ ^ -α ^ 1 * ~ 5u 00 -10 10Γ * O S

| Solid semi-finished takes place by dosing and mixing of these materials _ ^ _J .'T r J-. _ ^ t 4 ^ ^ r „„ 4. ^ -J f <r - _ __ _ ^ ... _ _ ^ // '/ / • /' y - 2 - i i f! water or generally acidic liquids, to allow a; - agglomeration of this pulverulent material and thus form! j ï - granules.

I Generally a supply of water vapor is provided to heat the mass to be granulated and partially solubilize 5; j salts, so as to thus form a binder between the grains to be agglomerated into granules.

| * The semi-finished products used as raw material for the manufacture of ternary fertilizers are generally the following: i - ammonium nitrate and urea,! - simple and concentrated superphosphates, [. - binary phospho-nitrogen compounds, such as phosphates m on o - and b .i amm on i eu es, - potassium chlorides and sulfates, 1 - other compounds containing addition elements (for example: Mg, S) and trace elements, j - composites containing one or more of these cited elements I- i! upper.

i i \ - case Natural phosphates.

i I. * Water can be replaced, following the formulas fsrtili r an-; your envi s "o ée s," read or less "" • v-.p 'a -. =, 7 ent uar an acid sulft.ui -, que, pnesonorrru e and / or natr.vmue ou.t teut r your car with tau c ~ .tut j of the aforementioned semi-finished products. Anhydrous artnoiuiac had some other bones is because this case sluggish towards the tero.s of the grar.rlo on to neutralize the eu: yielding acidity.

I -This mixing operation and this granulation can be erased am tans known devices, such eue famüuur, plate ^.

The - 3 - i i |,! ί \ i

After granulation, the product is dried in an oven and, after cooling, screened in a sieving device. Products that are too fine and products that are too large, after grinding, are recycled to granulation.

The other process, according to which one starts from porridge, is rather written in an integrated unit where the manufacture of ternary fertilizers is directly linked to the dissolution of this phosphate, j for example by nitric, sulfuric attack, phosphoric or l]; mixed.

According to this process, one or the other solid semifinished material is incorporated into the slurry, from which part of the lime nitrate produced has been optionally removed, and this slurry is granulated by mixing with cases produced by return from it. a sieving device, for example one of the granulation apparatuses mentioned above in connection with the granulation process for solid materials.

j; · The method of granulation by slurry present, compared to granulation this solids are as defined above, various advantages.

Thus, because ebne η; span if one of the fertilizers in one can react between them more quickly euanu fear to come to an end this reaction. This is not the case for a fertilizer where the reactions continue in the finished short which,, / /

In addition, the formation of granules from a slurry being effected by coating several successive layers of slurry, gives the granules better mechanical strength and, therefore, a lower risk of solidification.

Finally, since a mixture is normally more homogeneous than a mixture of solid products, the granules formed from a * mixture are also more homogeneous in fertilizing elements than a simple mixture of solid products.

'. An important drawback, however, of the slurry granulation method is that it must necessarily take place in a factory where a phosphate attack is carried out with nitric, phosphoric and / or sulfuric acid.

| An essential drink of the ores ^ rig ^ ^ ve ^ tioc ^ st ce j present a new process this manufacture of granular fertilizers ij combines the advantages of the two known processes described i I so mv air em en t -cs ε su s.

| Λ csc: ü -'- ~ '2t, the process according to the invention conrorsnd the hot reaction of an ammonium niurate solution, j - / c ui ^ - = _ \ ee aa in ^ ns a substance uivérulen-! ·, ”this containing one or more iron elements it Ή jumps, such as au'au il ΙΓΐ0.ΐ.Γΐ3 VSi3 0 33 3 * '" λ cr "r - -.-.- Λ -r * ·, - * j ^ ^ r ^ * | Λ o - · ^ (i!

It "“ - .r - - 3 w1 ^: *? B. Tü cJ.t- f.33 33 3 3 ^ ~ nc * ό ^ * 1303 ÿS 3 - -. Z? 33 i | p..o, i ^ _iOiZOi2s, such as iss pnosphates mono- and biantmoniçp-Ίθ s, te 5!, v--; c "rt .._ sa ul. buntes - = pore ssioir. and natural phosphates, di i mariers a ror: er rte pulp or boiled, and aranulati-οη ce ceti! / / i /./! /./ i "i - - 1 - pulp or boiled by mixing the latter with a | pulverulent fertilizer formed in particular by fine return product from sieving of the granules.

The invention further relates to an installation for the miss implementing the above method.

This installation is characterized by the fact that it comprises at least one heated reactor and provided with an agitator, in which, on the one hand, the suspension of the snbstan- are carried out! these aforementioned powders in a hot solution of ammonium nitrate and / or urea and, on the other hand, the reaction between this solution and these powdery substances.

The invention finally also relates to the granulated ternary fertilizer obtained by this process or by the use of [this installation for manufacturing granulated fertilizers.

; Other details and peculiarity of the invention come out! will draw from the cescritvzion given above as an example! | non-limiting this several particular embodiments! to the process for manufacturing granulated fertilizer according to the invention; and of a particular form of a granulation installation according to the invention.

i - Ο ί of potassium and natural phosphates, well known in the i manufacture of fertilizers, and then subjecting the pulp or boiled product thus obtained to granulation by mixing the latter i with a pulverulent fertilizer formed in particular by product ! end of return from sieving of the granules.

In some cases, this ammonium and / or urea nitrate can be added to the solution as a phos- i solution. ammonium phage.

I The amount of ammonium phosphate solution is

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j · feed less than 20%, and preferably less than 10%, of the total amount of fertilizer obtained.

The solution of ammonium nitrate and / or urea i i contains very little water, this quantity of scanned water of pre-I.

rance of between 4 and 15% by weight of the solution.

The solution is reacted with the above substances; \ s at I a temperature between 75 and 100 ° C and preferably ink I * 'j! 80 and 90 ° C, so as to maintain good fluidity with the mixture.

i! To obtain a yield this granulauion as impeccable as possible, and according to Iss reusable formulas to produce. it governs the amount by weight of the solution arouses pa ~ tnpgvru î; to the quantity of powdery substance reacted in a mannered manner! ! to obtain a few pulps or boiled contsnant entered Θτ · i the total amount of boiled or pulp.

• t | In addition, we adjust the water content in the final boiled ferment between 4 and 7% compared to the quantity tozars! -iis or de or read. This will reduce the s sorting and minimum 1 ^; "'. / 7> - 7 -! I I Simultaneous adjustment of the solids or ligux content and of the water content is ensured, in addition to the dosage of the quantity and title of the urea solution or nitrate, by the addition of marketable phosphoric acid to 50 - 52¾ P205 and anhydrous ammonia to the slurry. The amount of ammonia is such that the molar ratio NH3 / H3PQ4 is between 1.35 and | 1 , 40 so as to keep the maximum solubility in this solution] v of ammonia phosphate thus formed.

To reduce the acidity of the slurry before granulation, for example as a result of the introduction of phosphoric acid, I ammonia is introduced into the slurry before the granule- I .....

I tion, as a neutralizing agent> -Xon.

The quantity of fine fertilizer recycled and mixed with the palpa | or boiled during granulation is generally understood! between 1 and 3 times the amount of porridge and even between 1 and 2 times this amount.

-after the granulation, the product obtained is subjected to a drying, eventuell followed by cooling, and to a calibrated, oar sx émois oar tamisa re. The fine fertilizer concealed sm-; . > said used during the granulation tion preferably comes from j *

This installation essentially includes a tank in J

i of urea, a series of hoppers 2, 3 and 4 containing powdery solid raw materials formed for example by superphosphates, binary phospho-nitrogenous compounds, chlorides or potassium sulphate, etc.

The main part of the installation comprises at least j a pulp or slurry reactor where the solid raw materials from hoppers 2, 3 and 4 are suspended i in a hot solution of ammonium nitrate and / or urea pro; ji I coming from tank 1.

I. In the embodiment shown in the figure, two! <j pulp reactors. 5 and 6 mounted in series have been provided, i arrow 7 shows the supply of the solution from tank 1 to the first reactor 5, while arrow S shows the supply of solid raw materials to this same reactor 5.

The brought of the solution can p.s. be carried out by a known t will go isolated to cost; -Yes ---------'— * - ----! | saturated water vapor, the supply of pulverulent material can take place by means of a sir.pla conveyor belt moving below these trsmies, itself, such as a coding t ~ I.. _ ^ - - r. _.-.- ή-c; --V. -u te- a troue, non recrre- ^ r- I νθ2 ^ ΓΓ < 3ΐΧ2 ^ “ΰ2 03 22 ^ - - - - —----- - e l- · 1 'e K ^ ΐ téa à la îioure. Their granulometry follows these materials 1' ''“ 'i possibly dry and cro " its before J. eu rm <—l ~ ov-C —3— - These reactors, having a determined volume, are provided if / “of agitators 9 and 10 ai this s ser heating pads 11 and 12. l-nsi, q ^ · * T ^ j “I f ..„, / U -. “I-, ^ i ~, -p. C '”' ·" * "T" [p ^! · By bringing the solution into contact, coming from tank 1, and - 'J - ο maintained at the temperature necessary to create good fluidity and also a mixture homogeneous as possible allowing reactions to be carried out under ideal conditions.

In addition to a homogeneous mixture, between the solution, coming from tank 1, and the solid matter, coming from hoppers 2 to 4, in these heated reactors 5 and 6, a certain evaporation of water allowing, for example if starting from a relatively dilute solution, bring the title of the porridge obtained to the value required for the subsequent operations.

j .If necessary, one can add to one of the reactors, eg to the j j reactor 5, as indicated by arrow 26, a certain quantity i | phosphoric acid.

] t i! The reactor 6 is successively followed by a granulator j j 15, such as a drum granulator, a dryer 16 and a | cooler 17.

j The granulated products leaving the cooler fall into a sieving device 18 where a calibration of the granules; takes place, for example by means of two superimposed sieves 19 and 20.

j The particles retained between the sieves 19 and 20 will then have i j the predetermined particle size and consequently constitute the granulated production fertilizer which can be sent to j v, a conditioning device, as indicated by arrow 21.

j I Large particles that do not break through | i ““ j the sieve 19 are sent to a grinder 22, while the

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\ fine particles passing through the sieve 20 are collected in | a hopper 23. These fine particles and the crushed particles are then directed, as indicated by arrow 24, towards] the inlet of the granulator 15, so as to constitute the fertilizer | back intended to be mixed with the porridge as a support / 5 - /! - 10 - during a good granulation yield, part of the granulated fertilizer forming the finished product may have to be recycled, as * indicated by arrows 21a.

The arrow 25 indicates a possible introduction, into the granulator 15, of ammonia as neutralizing agent from a storage tank 28.

! A similar introduction can also take place in reactors 5 and 6, as indicated by arrow 27.

] In granulator 15, the slurry therefore coats the par- | fine sheets recycled according to arrow 24 until constituted,! | by forming several successive layers of porridge, j! relatively hard granules of a certain size. The dimensions of the granules depend, among other things, on the duration of stay in the granulator, the composition and the viscosity of the slurry, etc. These working conditions are generally determined experimentally so that the quantity of powdery product to be recycled can be governed in an approximate manner according to arrow 24 to the granulator 15.

The object of the invention will be illustrated further by a few practical examples of the manufacture of a ternary fertilizer according to the process of the invention by means of the above-mentioned installation.

! Example 1: Manufacture of a ternary fertilizer 17-17-17 based on j | of ammonium nitrate solution.

I 415 kg of hot 90% ammonium nitrate solution

J

| and at a temperature of 85 ° C was fed to the two

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j reactors in series 5 and 6 where it has been mixed with the materials. / j · - 11 - following first pulverulent from hoppers 2, 3 and * 4: 307 kg of phospho-nitrogenous binary compounds containing 11% "» of ammoniacal nitrogen and 49% of P2 ° 5 '15 kg of bicalcium phosphate at 43% of and 282 kg of 60.5% potassium chloride; of K20 1 As indicated by arrow 26, we added to the reactor! '5, in addition, 15 kg of liquid phosphoric acid at 54% p2 ° 5 *! * Thus; a pulp containing 56% solid matter * was obtained, but containing only 4.8% water.

In reactors 5 and 6 the temperature was maintained at around 80 ° C.

] In these reactors, especially the sux- reactions occur | between the suspended products; -KC1 + ΝΕΛΝ0_ - * KNO + EH. Cl.

4 3 3 4 J - KC1 + ammonium phosphate -> potassium phosphate- j j! sium + ΓΗ cl.

4] Thanks to these reactions, we obtain the constitution of potassium nitrate and phosphate products and airano- chloride; niac which are more favorable to good behavior and resistance! | mechanics of the granules obtained and with fertilizing properties] * * 1 ‘of the final ternary fertilizer.

The residence time of the products in the reactors was 2 to 40 minutes.

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] The pulp thus produced was then fed to the granulation apparatus 15, the latter also being feed / i /, | fj / - 12 in recycled products in an essentially pulverulent state.

This recycled amount was between .1.7 'and · 2rl times the total amount of slurry from reactor 6.

3 kg of ammonia were introduced into the granulator 15 / as a neutralizing agent. This has been indicated by arrow 25.

1.037 kg of granulated fertilizer were thus obtained corresponding to the quantity of products reacted.

By drying and evaporating 37 kg of water, 1,000 kg of product was obtained at 1.3% humidity and titrating as such 17% total nitrogen, of which 6.5% nitric nitrogen and 10, 5% ammoniacal nitrogen, 17% phosphoric anhydride and 17% of Example 2: Manufacture of ternary fertilizer 15-22-12 based on a urea solution.

258 kg of a hot 90% urea solution at a temperature of 11 ° C was fed to the two reactors in series 5 and 6 where it was mixed with the following powdery raw materials from hoppers 2, 3 and 4 : 263 kg of phospho-nitrogen binary compounds containing 11% ammoniacal nitrogen and 49% PO, 224 kg of simple superphosphate at 19% P 0_ and 198 kg “'potassium chloride at 60.5% K ^ O.

As indicated by arrow 26, 590 kg of 54% P 2 O phosphoric acid was added to the reactor, as well as 15 kg of amz-3 o moniac as indicated by arrow 27.

Thus, a pulp containing 65% solid matter but containing only 5.8% water was obtained. In reactors 5 and 6, the temperature was maintained at 90 ° C.

Besides the partial ammoniation of phophoric acid, there is ί - “* KCl + ammonium phosphates -> potassium phosphate + I- nh4ci.

This reaction makes it possible to obtain more favo-rable products with good behavior and mechanical resistance of the granules obtained.

The residence time of the products in the reactors was of the order of 55 minutes.

The pulp thus produced was then supplied to the granulation apparatus 15, the latter also being supplied with recycled products.

This recycled amount was between 2.4 and 2.9 times the amount of slurry from reactor 6. 4 kg of ammonia were introduced into the granulator 15,; as a neutralizing agent. This was indicated by t; arrow 25.

j 1.052 kg of corresponding granular fertilizer were thus obtained.

S

i j danh to the quantity of products reacted.

| j By drying and evaporating 52 kg of water, 1 1,000 kg of product was obtained at 0.8% humidity and titrating on such that i Γ I 15% total nitrogen, 22% phosphoric anhydride and 17% K ^ O.

| From the description given above it therefore follows .1 \ ύ * | j that the process according to the invention can be applied in j ’a conventional mixing workshop for dirty raw materials

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to powdered snow, by means of the introduction of pulp reactors and i! d‘'une storage tank of a hot solution of nitrate of am-; monium or urea and thus enjoy the flexibility of exploitation and the wide variety of possible formulas of fertilizers I, j ternary specific to such a mixing workshop. / i / ü! - 14 - ί

Furthermore, the fact of starting from hot liquids and containing little water has the consequence that a direct solidification of the successive coating layers is obtained by simple cooling. This has the important effect of a very large increase in the granulation yield and in the capacity of a given specific granulation apparatus and of a dryer of given size and calorific capacity with respect to; »Known methods.

It is understood that the invention is not limited to the embodiments described and that many variants! can be envisaged without departing from the scope of this patent.

i | This is how the process can advantageously be

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{applied for the production of fertilizers of all compositions, /: in particular binary fertilizers. f \ f / \ // i / \ / i ’i î i i x]

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Claims (16)

1.- A method of manufacturing granulated fertilizer, characterized in that it comprises reacting, under heat, a solution of ammonium nitrate and / or urea with at least one substance for% drous containing one or more fertilizing elements, such as at least one of the powdery substances chosen from the group formed by simple and concentrated superphosphates ·,. binary phospho-nitrogen compounds, such as mono- and biammonium phosphates! ques, potassium chlorides and sulphates and natural phosphates, so as to form a pulp or boiled, and the granulation of this pulp or boiled by the mixture of the latter with a pulverulent fertilizer formed in particular by fine return product from a sieve of granules. 2.- Method according to claim 1, characterized in that cru'c uses a hot solution at 85 to 96% by weight of nitrate * ammonium • and / or. a hot solution at 85 to 95% by weight of urea 3, - Process according to either of Claims 1 and 2, characterized in that the solution and the abovementioned substances are reacted at a temperature between 70 ° C and 103 ° C and preferably between 80 ° C and 90 ° C. 4.- Method according to either of Claims 1 to 3, characterized in that the quantity by weight of the above-mentioned solution is adjusted relative to the quantity of pulp substances! s virulent reactions in order to obtain a pulp or porridge containing between 50 and 70% of solid rantiêres compared to the total amount of this porridge or pulp. 5. Method according to any one of claims / J / I 1 to 4, characterized in that the quantity by weight fi / \ '] + is adjusted: j - 16 - f. 4! V the above-mentioned solution relative to the quantity of pulverulent substances reacted so as to obtain a pulp or slurry containing between 4 to 10%, and preferably between 4 <and 7% of water relative to the quantity total porridge or: pulp. 6.- Method according to any one of the claims? 1 to 5, characterized in that liquid phosphoric acid is added to the slurry to adjust the content of P2 ° 5 ^ ans l1®11-fertilizer obtained. '; · Ϊ́ J 7. Method according to any one of claims - J! 1 to 6, characterized in that liquid ammonia or gaseous ammonia is introduced as neutralizing agent ,. î .1 7 i i j i î 8. Method according to any one of claims 1 j I to 7, characterized in that a part of the water contained J j is evaporated in the pulp or boiled before granulation. AT } 9. Method according to any one of claims 1 to j 8, characterized in that the pulp or pellet is granulated with a J- * J; amount of recycled fine fertilizer between one and three times i the amount of porridge. 10. Method according to any one of claims>] 1 1 to 9, characterized in that the product, obtained after granulation, is subjected to drying and sizing, eg by sieving, tj and in that it is recycled at least part of the materials removed \ during sizing, possibly after grinding, towards / granulation, so as to constitute at least part of * the above-mentioned recvclosed fertilizer intended to be mixed with the pulp or boiled, the calibrated product forming the granulated production fertilizer. 11. Method for manufacturing granulated fertilizer as described above, more particularly in the appended examples. 12. Installation for the manufacture of fertilizer according to any one of the preceding claims, characterized in that it comprises at least one heated reactor and provided with an agitator, in which the suspension of the pulp substances is carried out - verulent above mentioned in a hot solution of urea ammonium nitrate and / or phosphate c. * ammonium and the reaction between them 13. Installation according to claim 12, characterized in that it comprises at least two reactors in series. • | 14. Installation according to either of claims A j 12 and 13, characterized in that the reactors are provided with j S heating coils. 15. Installation according to any of the claims | 12 to 14, characterized in that it comprises, downstream of the reactor, | | successively a granulator, a dryer and a device for | j sieving. 1 =, 16.- Plant for the manufacture of fertilizers as described above and shown in the accompanying drawings. I * 17. Fertilizer obtained by the process or by means of the installation described above or shown in the attached drawing. î I -; _A ...........- j> 14 1 ...... ”! ... S ...... 1 - ¾ KTîAAJ Λ y? , v ïï / à