Method for Producing a Composition Containing at Least one Metal Amino Acid Compound and Composition Obtainable by Means of a Method of this Kind

Abstract

The invention relates to a method for producing a composition containing at least one metal amino acid compound, in which method —a basic compound of a divalent metal is first reacted together with an alpha amino acid in a molar relationship of one to at least two in water during heating of up to 60° C. to 100° C., —a reaction equilibrium is awaited, —the reaction solution is then mixed with a water-soluble salt of the same divalent metal at a quantity such that the molar total quantity of the divalent metal from the basic compound of the metal and the metal salt does not exceed the molar quantity of the alpha amino acid, —the metal salt is allowed to completely dissolve, —the reaction solution is then dried thereby obtaining a solid composition.

Claims

1.-14. (canceled)

15. A method for preparing a composition comprising at least one metal-amino acid compound, the method comprising: carrying out a reaction of a basic compound of a divalent metal with an alpha-amino acid in a molar ratio of 1 to at least 2 in water while heating to 60° C. to 100° C.; waiting until the reaction has reached an equilibrium; adding to a reaction solution of the reaction a water-soluble metal salt of the divalent metal in an amount such that a molar total amount of the divalent metal of the basic compound of the divalent metal and of the metal salt of the divalent metal does not exceed a molar amount of the alpha-amino acid; waiting until the water-soluble metal salt of the divalent metal has completely dissolved; drying the reaction solution to obtain the composition as a solid.

16. The method according to claim 15, further comprising the step of selecting the basic compound of the divalent metal from the group consisting of a hydroxide, a carbonate, a hydroxide carbonate, and an oxide.

17. The method according to claim 15, further comprising the step of selecting the divalent metal from the group consisting of copper, manganese, zinc, and iron.

18. The method according to claim 15, wherein an anion of the water-soluble metal salt of the divalent metal is sulfate.

19. The method according to claim 15, wherein the alpha-amino acid is a naturally occurring, proteinogenic amino acid.

20. The method according to claim 15, wherein the alpha-amino acid is glycine.

21. The method according to claim 15, wherein drying of the reaction solution is carried out by one or more methods selected from the group consisting of fluid-bed drying in a spray granulator; oven drying; vacuum drying; and spray drying.

22. The method according to claim 21, wherein fluid-bed drying in a spray granulator is carried out at a product temperature of 70 to 130° C.

23. A composition comprising at least one metal-amino acid compound, the composition obtained by the method of claim 15.

24. The composition according to claim 23, wherein the basic compound of the divalent metal is a copper compound, wherein the alpha-amino acid is glycine, and wherein the water-soluble metal salt of the divalent metal is a copper sulfate, wherein the composition is characterized through an X-ray diffractogram obtained by Cu-Kα.sub.1 irradiation at room temperature and comprising characteristic reflections at 11.99, 13.37, 19.39, 20.03, 21.60, 22.55, 23.09, 28.37, 29.81, 30.63 and 31.23° at 2θ.

25. The composition according to claim 23, wherein the basic compound of the divalent metal is a copper compound, wherein the alpha-amino acid is glycine, and wherein the water-soluble metal salt of the divalent metal is a copper sulfate, wherein the composition is characterized through an X-ray diffractogram obtained by Cu-Kα.sub.1 irradiation at room temperature and comprising characteristic reflections at 10.54, 11.83, 13.27, 15.95, 16.42, 19.10, 20.27, 22.34, 23.83, 27.52, 28.12, 29.23, 31.59 and 33.39° at 2θ.

26. The composition according to claim 23, wherein the basic compound of the divalent metal is a copper compound, wherein the alpha-amino acid is glycine, and wherein the water-soluble metal salt of the divalent metal is a copper sulfate, wherein the composition is characterized through an X-ray diffractogram obtained by Cu-Kα.sub.1 irradiation at room temperature and comprising characteristic reflections at 10.29, 11.67, 13.27, 14.84, 16.32, 19.15, 20.23, 22.29, 23.76, 27.47, 28.01, 29.12, 31.47 and 33.42° at 2θ.

27. The composition according to claim 23, wherein the basic compound of the divalent metal is a zinc compound, wherein the alpha-amino acid is glycine, and wherein the water-soluble metal salt of the divalent metal is a zinc sulfate, wherein the composition is characterized through an X-ray diffractogram obtained by Cu-Kα.sub.1 irradiation at room temperature and comprising characteristic reflections at 7.58, 10.21, 11.67, 15.14, 16.08, 17.53, 18.39, 18.81, 20.54, 20.81, 21.27 and 21.72° at 2θ.

28. A method of enriching an animal feed with divalent metals of high bioavailability by adding a composition comprising at least one metal-amino acid compound to the animal feed, the composition obtained by the method of claim 15.

29. An animal feed comprising a composition comprising at least one metal-amino acid compound, the composition obtained by the method of claim 15.

Description

EXAMPLE 1

[0020] 418 g of basic copper carbonate (Cu.sub.2CO.sub.3(OH).sub.2H.sub.2O) is added, with stirring, to 4.5 kg of water. 600 g of glycine (NH.sub.2CH.sub.2COOH) is then added, with stirring, and the suspension is boiled for 40 minutes. This results in the dissolution of the turquoise-green basic copper carbonate, with evolution of gas and the formation of a dark blue solution with a precipitate of the same colour. 624 g of copper sulfate pentahydrate (CuSO.sub.4.5H.sub.2O) is then added, with stirring, to the hot reaction and the mixture is boiled for a further 10 minutes. A dark blue clear solution forms, which was dried into a granulate by spray granulation in a fluid bed using a Glatt GPCG 3.1 dryer operated with the following parameters:

TABLE-US-00001 Air inflow 140-150° C. Air inflow rate: 50-90 m.sup.3/h Air outflow  75-85° C. Product 90-110° C.

[0021] The dark blue crystalline and granular composition (FIG. 1) had a copper content of approx. 308 g/kg, a nitrogen content of approx. 83 g/kg and a surface water content of approx. 54 g/kg. It is characterized by an X-ray powder diffractogram (FIG. 2) that for Cu-Kα1 irradiation at room temperature has particularly characteristic reflections at 11.99, 13.37, 19.39, 20.03, 21.60, 22.55, 23.09, 28.37, 29.81, 30.63 and 31.23° at 2θ.

EXAMPLE 2

[0022] 17 kg of basic copper carbonate (Cu.sub.2CO.sub.3(OH).sub.2H.sub.2O) is added, with stirring, to 150 kg of water. 24.3 kg of glycine (NH.sub.2CH.sub.2COOH) is then added, with stirring, and the suspension is boiled for 30 minutes. This results in the dissolution of the turquoise-green basic copper carbonate, with evolution of gas and the formation of a dark blue solution with a precipitate of the same colour. 25.25 kg of copper sulfate pentahydrate (CuSO.sub.4.5H.sub.2O) is then added, with stirring, to the hot reaction and the mixture is boiled for a further 15 minutes. A dark blue clear solution forms, which was dried into a granulate by spray granulation in a fluid bed using a Glatt ACT 400 dryer operated with the following parameters:

TABLE-US-00002 Air inflow 180-220° C. Air inflow rate: 1000-1200 m.sup.3/h temperature: Air outflow  90-105° C. Product 95-110° C. temperature: temperature:

[0023] The dark blue crystalline and granular composition had a copper content of approx. 312 g/kg, a nitrogen content of approx. 84 g/kg and a surface water content of approx. 12.2 g/kg. It is characterized by an X-ray powder diffractogram that for Cu-Kα.sub.1 irradiation at room temperature has particularly characteristic reflections at 10.29, 11.67, 13.27, 14.84, 16.32, 19.15, 20.23, 22.29, 23.76, 27.47, 28.01, 29.12, 31.47 and 33.42 at 2θ.

EXAMPLE 3

[0024] 680 kg of basic copper carbonate (Cu.sub.2CO.sub.3(OH).sub.2H.sub.2O) is added, with stirring, to 4000 kg of water. 972 kg of glycine (NH.sub.2CH.sub.2COOH) is then added, with stirring, and the suspension is boiled for 30 minutes. This results in the dissolution of the turquoise-green basic copper carbonate, with evolution of gas and the formation of a dark blue solution with a precipitate of the same colour. 1010 kg of copper sulfate pentahydrate (CuSO.sub.4.5H.sub.2O) is then added, with stirring, to the hot reaction and the mixture is boiled for a further 15 minutes. A dark blue clear solution forms, which was dried into a granulate by spray granulation in a fluid bed using a Glatt AGT 2200 dryer operated with the following parameters:

TABLE-US-00003 Air inflow 170-190° C. Air inflow rate: 40 000-45 000 m.sup.3/h temperature: Air outflow  65-90° C. Product 70-95° C. temperature: temperature:

[0025] The dark blue crystalline and granular composition had a copper content of approx. 306 g/kg, a nitrogen content of approx. 84.6 g/kg and a surface water content of approx. 32 g/kg. It is characterized by an X-ray powder diffractogram that for Cu-Kα1 irradiation at room temperature has particularly characteristic reflections at 10.54, 11.83, 13.27, 15.95, 16.42, 19.10, 20.27, 22.34, 23.83, 27.52, 28.12, 29.23, 31.59, 33.39 at 2θ.

[0026] The measurements were in each case carried out using a STADI P powder diffractometer from Stoe & Cie, Darmstadt, in Guinier geometry between films as a flat preparation. The radiation source used was a Cu anode (40 kV, 20 mA) with Cu-Kai irradiation (1.54059 angstroms) generated using a Johann-type germanium monochromator. The detector used was an Imageplate IP-PSD from Stoe & Cie.

[0027] None of the compositions mentioned above or compounds obtained from such a composition are present in the relevant crystal structure databases such as the Cambridge Structural Database (CSD).

[0028] The following reaction cascade with steps A) and B) is in each case assumed, it not being known exactly which end products or end product composition are formed:

A) Reaction of Glycine with Basic Copper Carbonate [CuCO.sub.3.Cu(OH).sub.2]:

##STR00004##

[0029] where H.sub.2CO.sub.3H.sub.2O+CO.sub.2←

2)

##STR00005##

B) Presumed Further Reactions:

[0030] ##STR00006##

EXAMPLE 4

[0031] 268 g of basic zinc carbonate (Zn.sub.2CO.sub.3(OH).sub.2H.sub.2O) is added, with stirring, to 2 kg of water. 336 g of glycine (NH.sub.2CH.sub.2COOH) is then added, with stirring, and the suspension is boiled for 40 minutes. This results in the dissolution of the white basic zinc carbonate, with evolution of gas and the formation again of a white suspension. 401 g of zinc sulfate monohydrate (ZnSO.sub.4.1H.sub.2O) is then added, with stirring, to the hot reaction and the mixture is boiled for a further 10 minutes. A light grey clear solution forms, which was dried into a white granulate by spray granulation in a fluid bed using a Glatt AGT 400 dryer operated with the following parameters:

TABLE-US-00004 Air inflow 190-220° C. Air inflow rate: 1000-1300 m.sup.3/h temperature: Air outflow 110-125° C. Product 110-130° C. temperature: temperature:

[0032] The white crystalline composition has a zinc content of approx. 308 g/kg, a nitrogen content of approx. 69 g/kg and a surface water content of less than 5 g/kg. It is characterized by an X-ray powder diffractogram that for Cu-Kα.sub.1 irradiation at room temperature has particularly characteristic reflections at 7.58, 10.21, 11.67, 15.14, 16.08, 17.53, 18.39, 18.81, 20.54, 20.81, 21.27 and 21.72 at 2θ (FIG. 3).

[0033] There is likewise no composition or compound of this kind present in the relevant crystal structure databases such as the Cambridge Structural Database (CSD). The reaction is here presumed to proceed via a cascade analogous to the reaction cascade described above with basic copper carbonate.