Food or edible material: processes – compositions – and products – Products per se – or processes of preparing or treating... – Protein – amino acid – or yeast containing
Reexamination Certificate
1999-08-25
2001-09-11
Sayala, Chhaya D. (Department: 1761)
Food or edible material: processes, compositions, and products
Products per se, or processes of preparing or treating...
Protein, amino acid, or yeast containing
C426S069000, C426S807000
Reexamination Certificate
active
06287627
ABSTRACT:
FIELD OF THE INVENTION
The invention relates to a process for preparing a free-flowing, easy to handle animal feed supplement based on a methionine salt in which a granulated product is obtained starting from a methionine salt solution obtained in a conventional manner and the methioninate granular products obtained therefrom.
BACKGROUND OF THE INVENTION
Methionine and aqueous solutions of methionine salts, in particular sodium methioninate (DE 31 05 009 C), but also substitutes such as the methionine hydroxy analogue (MHA) are used all over the world as feed additives for rearing poultry, pigs and other economically useful animals and mainly promotes the production of animal protein. With regard to the increasing population of the world and increasing nutritional problems, methionine, as one of the essential amino acids in the animal growth process, and its different forms, and thus also its cost effective production, are very important. Solid or liquid forms may be preferred, depending on the requirements.
Commercially available sodium methioninate solution has a concentration of 40 wt. % methionine and its biological value corresponds to that of solid methionine, in contrast to the substitute MHA, compared on an equimolar basis. There are several suitable methods for preparing these types of sodium methioninate solutions, e.g.:
1. Dissolution of isolated methionine in caustic soda solution.
2. Alkaline hydrolysis of 5-(&bgr;-methylmercaptoethyl)-hydantoin with NaOH and/or Na
2
CO
3
.
3. Alkaline hydrolysis of methionine amide.
Although method 1 provides the purest product it is more costly and thus less economic than the production of methionine itself, due to an additional process step in comparison to production of the solid. In contrast, methods 2 and 3 are used at an earlier point in the production of methionine and thus there is no need to isolate the solid during the production of DL-methionine, depending on capacity.
The preparation of 5-(&bgr;-methylmercaptoethyl)-hydantoin is performed in a known manner by direct synthesis from the conventional starting materials methylmercapto-propionaldehyde (MMP) and hydrocyanic acid in the presence of ammonia and carbon dioxide. Methionine amide is prepared in a known manner by hydrolysis of methionine nitrile, which again is obtained by direct synthesis from the conventional starting materials MMP, hydrocyanic acid or ammonium cyanide and ammonia.
Depending on special requirements, it may be expedient to use a solid or a liquid form of the animal feed supplement.
The decision about which form to produce depends, inter alia, on the mixing apparatus which is available and the specific preferences of the particular manufacturer.
When preparing mixed feeds, the different feedstuffs and additives are initially present as separate components which, depending on their characteristics, are prepared by milling, shredding, drying or purifying. If the separate components have the characteristics required, the actual mixing process is performed in a mixing unit suitable for this process. Individual mixed batches differ, depending on the size of the unit. The essential amino acid methionine is used as a supplement for mixed feeds in concentrations of the order of magnitude of 0.01 to 1.0 wt. %. These amounts are added directly to the mixed feed by appropriate weighing and metering systems.
DE 31 05 009 describes the fact that aqueous solutions of sodium or potassium methioninate have the same methionine activity as solid methionine when used as an animal feed additive.
However, a result of the low-temperature stability of methioninate solutions, which has to be guaranteed by suppliers, it has hitherto been possible to supply only solutions with a concentration of up 40 wt. % of methioninate. Thus commercial products contain up to about 60 wt. % of water which leads to an approximately 2.5-fold increase in transport costs as compared with the transport of solid methionine. This has prevented liquid supplements based on methionine penetrating the market.
The use of crystalline sodium methioninate has not been considered due to the strongly hygroscopic nature of this compound.
However, it would be very useful to provide an additive for animal feeds which satisfies the following requirements:
1. It has precisely the same nutritive efficacy as solid crystalline methionine.
2. It can be converted into a liquid form at the desired concentration by the feedstuff mixer itself, without having to handle, for example, alkalis.
3. As little as possible “dead volume” in the form of water is carried during transport, so that the active substance content of the transported material is high.
4. The product can be adapted to the specific requirements of the individual users and optionally may also be used as a solid.
SUMMARY OF THE INVENTION
In view of these problems, the object of the invention is to provide a process such that the problems listed above can be solved by the product obtained. The invention also provides a new and improved solid methioninate product for animal feed supplements.
The invention provides a process for preparing a free-flowing, easy to handle animal feed supplement based on methionine, in which the starting material is an aqueous methionine salt solution (methioninate solution) generally obtained in a conventional manner, which is characterised in that the methionine salt solution is converted into a granular material in one or more stages.
This process may be performed continuously or batchwise.
The solutions are generally 10 to 70 wt. % strength, preferably 20 to 60 wt. % strength, in particular 25 to 45 wt. % strength, with respect to methionine.
Sodium and/or potassium methioninate solutions are preferably used, wherein the molar ratio of methionine to K or Na ions is preferably 1.1:1 to 1:1.1, preferably 1:1.
It has also been found to be advantageous to first treat the solutions to be sprayed and/or granulated with active carbon.
In one embodiment the methionine salt solution is spray dried in a spray apparatus with a centrifugal atomiser, wherein the temperature difference between the inlet temperature (120-200° C.) and the outlet temperature (60-100° C.) should be as large as possible. The powder obtained in this way is then converted into a granular material. This is achieved using a granulating plate, a granulating drum or a mixer. The granular mixture is preferably prepared in an Eirich mixer using an inserted, strongly shearing mixing device (cutter head insert).
The procedure in general is such that the spray dried powder is granulated in the mixing device together with a preferably saturated solution of the methionine salt.
The ratio by weight of powder to saturated solution, with respect to solid substance, is preferably in the range from 1:0.01 to 1:0.5.
The powder obtained by spray drying generally has a bulk density of 350 to 500 kg/m
3
, and a dust fraction of at least 1 to 5% (Dr. Groschopp's dust test).
The granular material has a bulk density of greater than 650 kg/m
3
, preferably greater than 700 kg/m
3
and a particle size distribution of 63 to 5000 &mgr;m, preferably 100 to 3000 &mgr;m, in particular 100 to 1400 &mgr;m, wherein about 90% has a particle size fraction >100 &mgr;m.
The proportion with a particle size <63 &mgr;m is generally at most 2%, preferably 1%, the Dr Groschopp's dust fraction is <1%, preferably <0.5%.
Another process variant for preparing the granular material according to the invention is granulation in a fluidised bed. In this case spraying the sodium methioninate solution and building up the feed additive granular material is performed in only one process step. The fluidised reactor being used may contain one or more crushing devices to regulate the particle size.
Here again preferably saturated methioninate solutions are used although less concentrated solutions may also be used.
The increase in weight in the fluidised bed under steady state conditions is compensated for by continuous withdrawal of the granular material. By means of a specific mode of operat
Binder Wolfram
Hasseberg Hans A.
Kniesel Heidemarie
Korfer Martin
Degussa - AG
Pillsbury & Winthrop LLP
Sayala Chhaya D.
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