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FR2529187A2 - Prepn. of di:calcium phosphate for feedstuffs - by direct reaction of phosphoric acid and chalk - Google Patents

Prepn. of di:calcium phosphate for feedstuffs - by direct reaction of phosphoric acid and chalk Download PDF

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Publication number
FR2529187A2
FR2529187A2 FR8211174A FR8211174A FR2529187A2 FR 2529187 A2 FR2529187 A2 FR 2529187A2 FR 8211174 A FR8211174 A FR 8211174A FR 8211174 A FR8211174 A FR 8211174A FR 2529187 A2 FR2529187 A2 FR 2529187A2
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Prior art keywords
phosphoric acid
phosphate
soluble
lime
dry
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FR8211174A
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French (fr)
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FR2529187B2 (en
Inventor
Antonio Baslini
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BASLINI IND CHIM
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BASLINI IND CHIM
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Priority to FR828211174A priority Critical patent/FR2529187B2/en
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Publication of FR2529187B2 publication Critical patent/FR2529187B2/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/32Phosphates of magnesium, calcium, strontium, or barium
    • C01B25/322Preparation by neutralisation of orthophosphoric acid
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K20/00Accessory food factors for animal feeding-stuffs
    • A23K20/20Inorganic substances, e.g. oligoelements
    • A23K20/26Compounds containing phosphorus

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Animal Husbandry (AREA)
  • Zoology (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Fertilizers (AREA)

Abstract

Bicalcium phosphate dihydrate suitable for food use is prepared by reaction between 60-75% H3PO4 and calcium oxide to give a dry, flowable powdered mixture of bicalcium phosphate and monocalcium phosphate having a P2O5 content above 50%, at least 50% of which is soluble in water the rest being soluble in ammonium citrate. The phosphoric acid is applied to the lime at a rate of 500-2500 litres/hour continuously or discontinuously. The CaO content of the lime is 80-100% by weight and its particle size is such that 90% of the granules pass a 5000 mesh/sq. cm sieve and 100% passes a 1000 mesh/sq. cm sieve. The product is more soluble and better assimilated by animals than is that prepared by the parent patent FR76.16485. A further advantage is that the product is not deliquescent and may be stored in the atmosphere without special precautions.

Description

Le brevet principal concerne un procédé pour la production de phosphate bicalcique pour usage dans les mangeailles selon lequel on fait réagir l'acide phosphorique à haute concentration directement avec de l'oxyde de calcium finement moulu. The main patent relates to a process for the production of bicalcium phosphate for use in feeds, in which phosphoric acid is reacted in high concentration directly with finely ground calcium oxide.

Le brevet principal crée une disposition particu lière par laquelle il est possible d'obtenir du phosphate bicalcique bihydrate à L'étant sec, c'est-à-dire contenant pratiquement la seule eau de cristallisation, en faisant réagir directement l'acide phosphorique et l'oxyde de calcin sous des conditions convenables. Le procédé selon le brevet principal est réalisé essentiellement dans un seul stade de production, puisqu'il suffit d'assurer le développement exothermique de la réaction pour l'obtention d'un produit sec, tandis que la haute réactivité de l'oxyde de calcium avec l'acide phosphorique donne lieu à un produit final qui est exempt de toute particule de chaux libre ou englobée; des stades supplémen tares de travail de purifaction ou de séchage ne sont donc pas nécessaires. The main patent creates a special arrangement by which it is possible to obtain bicalcium phosphate bihydrate in the dry state, that is to say containing practically only the water of crystallization, by reacting directly the phosphoric acid and cullet oxide under suitable conditions. The process according to the main patent is carried out essentially in a single production stage, since it suffices to ensure the exothermic development of the reaction to obtain a dry product, while the high reactivity of calcium oxide with phosphoric acid gives rise to a final product which is free of any particles of free or enclosed lime; additional stages of purifaction or drying work are therefore not necessary.

Conformément au brevet principal, le procédé pour la production de phosphate bicalcique bihydrate, à utiliser dans les mangeailles par réaction directe de l'acide phosphorique sur la chaux, est caractérisé en ce qu'on fait réagir dans un seul stade par charges successives, en profitant du chauffage créé par la réaction exothermique, de l'acide phosphorique à une concentration comprise entre 50 et 75 % de
H3 P04 et de l'oxyde de calcium en poudre jusqu'à l'obtention d'un produit final en poudre, sec et coulant.
According to the main patent, the process for the production of bicalcium phosphate bihydrate, to be used in mangeailles by direct reaction of phosphoric acid on lime, is characterized in that one reacts in a single stage by successive charges, taking advantage of the heating created by the exothermic reaction, phosphoric acid at a concentration between 50 and 75% of
H3 P04 and calcium oxide powder until a final powdery, dry and flowing product is obtained.

La présente addition crée un perfectionnement par lequel l'invention, objet du brevet principal, devient applicable à la production d'un melange homog3ne en poudre, sec et coulant de phosphate bicalcique et de phosphate monocalcique contenant une quantité plus importante de P205, QÇ une forme plus soluble et mieux as3lmilable par le bétail que celle selon la demande de brevet antérieur.  The present addition creates an improvement by which the invention, subject of the main patent, becomes applicable to the production of a homogeneous powder, dry and flowing mixture of bicalcium phosphate and monocalcium phosphate containing a greater amount of P205, QÇ a form more soluble and better as3lmilable by cattle than that according to the prior patent application.

La disposition suivant l'addition est caractérisée en ce qu'on fait réagir dans un seul stade de acide phos phorique à une concentration comprise entre 60 et 75 % de
H3P04 et de l'oxyde de calcium jusqu'à l'obtention d'un mélange homogène en poudre, sec et coulant, de phosphate bicalcique et de phosphate monocalcique , dont la concentration en
P205 est supérieure à 50 % et la solubilité dans l'eau est également supérieure à 50 %, le reste étant soluble dans le citrate d'amonium.
The arrangement following the addition is characterized in that one reacts in a single stage of phos phoric acid at a concentration of between 60 and 75% of
H3PO4 and calcium oxide until a homogeneous dry, flowing powder mixture of bicalcium phosphate and monocalcium phosphate is obtained, the concentration of
P205 is more than 50% and the solubility in water is also more than 50%, the rest being soluble in ammonium citrate.

Dans le brevet principal on a décrit la préparation de phosphate bicalcique bihydraté et sec par réaction de la chaux avec de l'acide phosphorique concentré à 50-60% en poids ou jusqu'à 70% en présence de carbonate de calcium. On obtient ainsi du phosphate bicalcique en poudre sèche contenant toutefois encore une certaine quantité de phosphate tricalcique (neutre), ce qui conduit à une diminution de la teneur en phosphore (jamais supérieure à 19%) et à une moindre solubilité. In the main patent, the preparation of bicalcium phosphate, hydrated and dry, has been described by reaction of lime with concentrated phosphoric acid at 50-60% by weight or up to 70% in the presence of calcium carbonate. Bicalcium phosphate in dry powder is thus obtained, however still containing a certain amount of (neutral) tricalcium phosphate, which leads to a reduction in the phosphorus content (never greater than 19%) and to a lower solubility.

On a maintenant trouvé que si l'on fait réagir directement de l'acide phosphorique à une concentration comprise entre 60% et 75% sur de la chaux en poudre très fine, on obtient un mélange de phosphates bicalcique et monocalcique en poudre sèche et coulante complètement soluble dans l'eau ou dans le citrate d'ammonium. Cela prouve qu'il n'y a plus de phosphate tricalcique, tandis que la teneur en phosphore s'élève à 22% environ. Un avantage supplémentaire consiste dans le fait que la poudre obtenue, bien qu'elle contienne du phosphate monocalcique, n'est pas déliquescente et peut être conservée à l'air libre sans précautions particulières. It has now been found that if phosphoric acid is reacted directly at a concentration of between 60% and 75% on very fine powdered lime, a mixture of bicalcium and monocalcium phosphates in dry and flowing powder is obtained. completely soluble in water or in ammonium citrate. This proves that there is no longer any tricalcium phosphate, while the phosphorus content is around 22%. An additional advantage consists in the fact that the powder obtained, although it contains monocalcium phosphate, is not deliquescent and can be stored in the open air without special precautions.

L'acide phosphorique employé pour la réaction, à une concentration comprise entre 60% et 75% en poids, est ajouté dans un réacteur muni d'un opérateur à ruban double à une quantité donnée de chaux avec une vitesse comprise entre 500 et 2500 litres/heure. L'addition peut être continue ou discontinue. I1 est également possible d'ajouter, à une quantité donnée de chaux alternativement ou en même temps, de l'acide phosphorique et de la chaux de manière continue ou discontinue. The phosphoric acid used for the reaction, at a concentration of between 60% and 75% by weight, is added to a reactor equipped with a double ribbon operator at a given quantity of lime with a speed of between 500 and 2500 liters /hour. The addition can be continuous or discontinuous. It is also possible to add, to a given quantity of lime alternatively or at the same time, phosphoric acid and lime continuously or discontinuously.

Les quantités, vitesses d'addition, temps de réaction, etc. sont fixés de manière à obtenir un produit sec et coulant avec un contenu en P205 supérieur aux 50E
Les paramètres ci-dessus dépendent de la concentration de l'acide phosphorique, de la réactivité de la chaux et de la quantité de chaleur que le système peut céder
Le titre en CaO de la chaux est compris entre 80% et 100% en poids, tandis que sa granulométrie est telle que 909 des granules passent à travers un sas au tamis de 5000 mailles/cm2 et 100% à travers un sas de 1000 mailles/cm2.
The quantities, addition rates, reaction times, etc. are fixed so as to obtain a dry and flowing product with a P205 content greater than 50E
The above parameters depend on the concentration of phosphoric acid, the reactivity of the lime and the amount of heat that the system can release
The CaO title of the lime is between 80% and 100% by weight, while its particle size is such that 909 of the granules pass through a sieve sieve of 5000 meshes / cm2 and 100% through a sas of 1000 meshes / cm2.

Les exemples suivants illustrent plus particulière- ment l'invention sans nullement la limiter. The following examples illustrate the invention more particularly without in any way limiting it.

Exemple 1. 2800 kg de chaux à 94E de CaO moulue de manière que 908 des granules passent à travers le sas de 5000 mailles/cm sont chargés dans un réacteur avec opérateur à double ruban. 8600 kg d'acide phosphorique épuré ayant un titre de 72% en H3PO4 sont ajoutés à travers des atomiseurs à une vitesse de 1950 litres/heure. Example 1. 2800 kg of lime with 94E of CaO ground so that 908 of the granules pass through the airlock of 5000 meshes / cm are loaded into a reactor with double ribbon operator. 8600 kg of purified phosphoric acid having a titer of 72% of H3PO4 are added through atomizers at a speed of 1950 liters / hour.

A la fin de l'addition d'acide phosphorique on laisse réagir pendant 60 minutes. At the end of the addition of phosphoric acid, it is left to react for 60 minutes.

On obtient ainsi 8850 kg de phosphate mono-bicalcique sec et coulant contenant 50,67% de P205 total et 28,18% de soluble dans l'eau. 8850 kg of dry and flowing mono-bicalcium phosphate are thus obtained, containing 50.67% of total P205 and 28.18% of water-soluble.

Exemple 2. 500 kg de chaux à 94% de CaO sont chargés dans un réacteur à double ruban. Example 2. 500 kg of lime with 94% CaO are loaded into a double ribbon reactor.

A l'aide d'atomiseurs on ajoute 13000 kg d'acide phosphorique à 70% de H3P04 à une vitesse de 1600 litres/ heure. Using atomizers, 13,000 kg of phosphoric acid containing 70% H3PO4 are added at a speed of 1600 liters / hour.

En même temps que l'addition d'acide phosphorique on commence à ajouter 3650 kg de chaux à une vitesse de 800 kg/heure.  At the same time as the addition of phosphoric acid one begins to add 3650 kg of lime at a speed of 800 kg / hour.

On laisse enfin réagir pendant 60 minutes. Finally allowed to react for 60 minutes.

On obtient 13070 kg de phosphate mono-bicalcique contenant 50,438 de P205 total et 28,9% de P205 soluble dans liteau, le reste étant soluble dans le citrate d'ammonium.  13070 kg of mono-bicalcium phosphate are obtained containing 50.438 of total P205 and 28.9% of P205 soluble in batten, the remainder being soluble in ammonium citrate.

Claims (3)

REVENDICATIONS 1 - Procédé pour la production de phosphate bicalcique bihydrate à utiliser dans les mangeailles par réaction directe de l'acide phosphorique sur la chaux selon la revendication 1 du brevet principal, caractérisé en ce qu'on fait réagir dans un seul stade de l'acide phosphoriqueà une concentration comprise entre 60 et 75% de H3POd et de l'oxyde de calcium jusqu'à l'obtention d'un mélange homogène en poudre, sec et coulant, de phosphate bicalcique et de phosphate monocalcique, dont la concentration en P205 est supérieure à 50% et la solubilité dans l'eau est également supérieure à 50%, le reste étant soluble dans le citrate d'ammonium. 1 - Process for the production of bicalcium phosphate bihydrate to be used in mangeailles by direct reaction of phosphoric acid on lime according to claim 1 of the main patent, characterized in that it reacts in a single stage of the acid phosphoric at a concentration between 60 and 75% of H3POd and calcium oxide until a homogeneous powder, dry and flowing mixture of bicalcium phosphate and monocalcium phosphate, the concentration of P205 is obtained greater than 50% and the solubility in water is also greater than 50%, the remainder being soluble in ammonium citrate. 2 - Procédé selon la revendication 1, caractérisé en ce que l'acide phosphorique est ajouté à travers des atomiseurs à une vitesse comprise entre 500 et 2500 litresiheure.  2 - Process according to claim 1, characterized in that the phosphoric acid is added through atomizers at a speed between 500 and 2500 liters / hour. 3 Mélange homogène de phosphate monocalcique et phosphate bicalcique en poudre sèche et coulante obtenu par le procédé selon l'une des revendications 1 ou 2.  3 Homogeneous mixture of monocalcium phosphate and bicalcium phosphate in dry and flowing powder obtained by the process according to one of claims 1 or 2.
FR828211174A 1976-02-10 1982-06-25 PROCESS FOR THE PRODUCTION OF BICALCIC PHOSPHATE FOR USE IN FEEDERS FROM PHOSPHORIC ACID AND LIME Expired - Lifetime FR2529187B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
FR828211174A FR2529187B2 (en) 1976-02-10 1982-06-25 PROCESS FOR THE PRODUCTION OF BICALCIC PHOSPHATE FOR USE IN FEEDERS FROM PHOSPHORIC ACID AND LIME

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Application Number Priority Date Filing Date Title
IT2003476 1976-02-10
FR828211174A FR2529187B2 (en) 1976-02-10 1982-06-25 PROCESS FOR THE PRODUCTION OF BICALCIC PHOSPHATE FOR USE IN FEEDERS FROM PHOSPHORIC ACID AND LIME

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FR2529187A2 true FR2529187A2 (en) 1983-12-30
FR2529187B2 FR2529187B2 (en) 1990-06-08

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2149828C1 (en) * 1999-07-01 2000-05-27 Общество с ограниченной ответственностью "Эковита" Method of synthesis of food dicalcium phosphate
US7273521B1 (en) * 2006-04-28 2007-09-25 J.M. Huber Corporation Method of producing granulated calcium carbonate/calcium phosphate composite materials with very high calcium to phosphate mole ratios

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3391992A (en) * 1964-06-04 1968-07-09 Swift & Co Feed grade dicalcium phosphate

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3391992A (en) * 1964-06-04 1968-07-09 Swift & Co Feed grade dicalcium phosphate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2149828C1 (en) * 1999-07-01 2000-05-27 Общество с ограниченной ответственностью "Эковита" Method of synthesis of food dicalcium phosphate
US7273521B1 (en) * 2006-04-28 2007-09-25 J.M. Huber Corporation Method of producing granulated calcium carbonate/calcium phosphate composite materials with very high calcium to phosphate mole ratios

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FR2529187B2 (en) 1990-06-08

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