DK147652B - PROCEDURE FOR THE PREPARATION OF A CARBAMID-CONTAINED FEED CONCENTRATE FOR DRUGS - Google Patents

Description

in 147652

The present invention relates to a process for the preparation of a free-flowing particulate concentrate for ruminants containing nitrogen as carbamide, sulfur as magnesium sulfate and phosphorus and trace minerals as inorganic compounds, in particular salts which are soluble in rumen liquid.

In order to obtain protein nutrition, ruminants can utilize simple nitrogenous compounds such as urea (carbamide), ammonia and ammonium salts because they have a bacterial flora that can build up bacterial protein of these substances and this bacterial protein can be digested by the ruminant later in the gastrointestinal tract. This ratio is of great importance in cattle farming, where carbamide is increasingly used, for example with cut straw, in concentrate feed instead of soybean meal or other oilcakes.

If carbamide is to provide a substantial part of the ruminant's protein supply, it must necessarily be balanced with a number of mineral nutrients necessary for the metabolism of the bacteria and therefore for their ability to convert the nitrogen of carbamide into protein. The bacterial protein contains direct phosphorus and sulfur, and a number of trace minerals are needed to maintain the metabolism of the bacteria so that they can build up the bacterial protein. The minerals that should be added in addition to P and S are Fe, Zn, Cu,

Mn and Co. The compounds should be soluble in rumen fluid, which in practice means that they should be water-soluble, since the bacteria can only absorb dissolved nutrients.

In the rumen, carbamide is rapidly cleaved to ammonia, the rumen fluid containing a urease. Large amounts of ammonia are harmful to the animal, so it is important that the bacteria quickly absorb this ammonia and convert it into bacterial protein. A prerequisite for this is that all the nutrients needed for the bacterial metabolism are present simultaneously with the urea / ammonia and essentially in the physiologically correct quantity ratio for the bacterial flora; this quantity ratio is well known.

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Since the different nutrients necessary for the bacteria should be present at the same time, in practice they must also be administered simultaneously, for example with the ruminant feed or with the animal's drinking water. The animal should thus, in a very different way, take a feed concentrate which is a mixture of carbamide and certain mineral nutrients.

However, it has been found that simple mixtures of these substances present great difficulties, especially with regard to keeping the mixture at a constant composition, so that the animals are always given the uniform compound mixture which is a prerequisite for optimal utilization of the carb amide.

The commodities which can be used to produce such simple mixtures are of very different particle sizes and in part densities, and it is therefore difficult to maintain a uniform mixture of them during transport and during mixing with other feed components, for example straw. Carbamide is mostly traded as so-called prills, ie. approximately spherical particles of 1-3 mm diameter. Since micro minerals such as compounds of Fe, Mn and Cu are only included in compound feed in amounts of the order of 19-50 ppm each, they will naturally appear in fine grain form to be distributed in the feed at all.

Thus, a mixture of carbamide and such finely powdered constituents will readily be separated during transport, including by mixing with coarse feed components.

The separation problem cannot be solved by grinding the carbamide into particle size powders approximately like the micro-minerals, thereby losing the carbamide's properties as a free-flowing material, and furthermore, it cannot be stored in silo or in a loose state otherwise without great risk of baking. Even if successful mixing of the carbamide with the other substances is achieved, the separation tendency is high, and is increased by the conventional methods of transport in bulk in tankers. Internally at companies, for example where the concentrate feed with carbamide is to be mixed into cut straw or other coarse feed, the transport to the mixing unit is often carried out by pneumatic route and the mixing itself is also often carried out by blow-in.

By these methods the separation tendency is large.

For several reasons, including in addition, due to the hygroscopicity of the carbamide, it is difficult to obtain a uniform admixture in the roughage; the content of carbamide in the finished feed mixture for direct use can easily fluctuate by 10% or more, so that there is a risk that some cows will have too low ration carbamide and thus protein, which will be very detrimental for eg their milk yield; while other cows get too much carbamide and thus protein, which is uneconomical.

German Patent Specification No. 2141003 discloses a grain supplementary feed for ruminants consisting of carbamide or other nitrogenous non-protein material, phosphate,

NaCl, anhydrous Na 2 SO 4, double carbonate of Ca and Mg, sulfur and trace elements. It is stated to be storage stable and prepared by mixing the components, including 2-15% NaCl, at 55-70 ° C with a sufficient amount of water to form a sprayable and liquid mass which is then granulated in a known manner, preferably spray drying. , at no specified temperature. The mixture does not contain magnesium sulfate. It is not stated whether the finished product is also storage stable at higher temperatures and the amount of energy needed for water evaporation during the spray drying will be prohibitively costly.

In the German patent it is stated as an advantage that the presence of Mg as double carbonate with calcium prevents conversion to magnesium sulfate, since this substance would significantly increase the hygroscopicity of the product. In the present invention, this hygroscopicity is avoided by the use of calcined Kieserite, and water is not used in the preparation, thus avoiding the prohibitive costs of its evaporation.

U.S. Patent No. 4283423 discloses a process for preparing a feed concentrate containing carbamide in granular, substantially free-flowing form by, after dry mixing of carbamide with at least ca. 10% calcium sulfate hemihydrate or anhydrite compacts this mixture at 71-107 ° C and then crushes the product to the desired particle size. The document does not mention the addition of magnesium sulfate in any form, the preparation described is not a granulation process and it is merely generally stated that the product is stock stable, not at higher temperatures.

Due to the described problems of mixing carbamide with other feed components, it is an obvious desire to granulate the carbamide together with the other mentioned nutrients. However, it has not been possible until now to find someone at once satisfactory and economically acceptable granulation method.

In the manufacture of granules, a granulating liquid containing a binder is typically used. The granulating liquid may be an organic solvent, but on the one hand it will in itself cost the product to a prohibitive extent and on the other hand it will be difficult to remove it to the extent necessary. The granulating liquid may also be water and in that case typically starch or other polymeric compounds such as carboxymethyl cellulose or a salt thereof or polyvinylpyrrolidone. However, the profit margin for cattle keeping is so small that a feed concentrate based on carbamide and micronutrients as described cannot bear the cost of the binder and subsequent drying of the granulate.

However, it has now been found that magnesium sulphate and carbamide together have properties which enable usable to obtain a useful granule of constant composition and free flowing properties as required by a granulation method which requires only simple heating without the addition of granulating liquid.

If the common commodity magnesium sulfate heptahydrate is used together with carbamide, an appropriate phosphate and suitable micro minerals, a granulate of all the components can be formed by simple heating to approx. 40 ° C. Upon heating, the mixture becomes somewhat sticky, gets a consistency reminiscent of cloves, and the grains blend together to a mass of consistency like slightly moist brown sugar ("powdered sugar"). Upon cooling, this character fades and the mixture TA7652 turns into a free-flowing granule while preserving the agglomerated particles substantially intact and with a very small amount of fine particles; the mixture should be kept in motion until the cooling process is complete.

However, it has been found that such a mixture is not stock resistant. It has a pronounced tendency to bake together to form larger aggregates at room temperature over 1-3 months and appreciably faster at higher temperatures, e.g., 30-40 ° C. Such higher temperatures can occur on hot summer days in temperate climates, and can easily occur in subtropical and tropical regions.

However, it has been surprisingly found that this baking tendency at relatively low temperatures can be avoided by using, instead of the heptahydrate, anhydrous magnesium sulphate obtained by calcining Kieserite (which is MgSO 2 O 2, i.e. a monohydrate) together with an antisetting agent. since the heating temperature of the granulation must then be somewhat higher.

Accordingly, the method of the invention is peculiar to the characterizing part of claim 1.

It has been found that after cooling, the granules present are free flowing and completely uniform with no appreciable amount of fine particles and therefore have no separation tendency. It is stable at temperatures up to 60 ° C for long periods and can withstand wind sieving, pneumatic transport and other normally occurring treatments without undergoing change.

It is necessary to heat the mixture to approx.

80 ° C to obtain the necessary agglomeration of the particles of the individual components. If, on the other hand, a maximum temperature of 86-95 ° C is exceeded during the granulation, the mixture becomes so sticky and adherent that it "burns" to the sides of the mixing vessel. If you get close to the maximum temperature, the granulate becomes absolutely uniform and does not separate at all, for example by wind sifting.

As anhydrous magnesium sulfate, calcined Kieserite, the most common type of anhydrous magnesium sulfate, is used and contains approx. 98% MgSO4.

As carbamide can be used ordinary technical carb amide, usually like the above prills, but there is nothing to prevent the use of other forms.

In the composition, any phosphorus compound which is at least partially soluble in water (or rumen fluid) and which can be utilized by the bacteria of the rumen can be used, provided that it does not contain elements harmful to the bacteria or the host animal. Preferably, a water-soluble phosphate salt with a suitable cation is used, preferably one which supplies one or more of the substances useful for the bacteria in addition to phosphorus.

However, since most phosphates are highly soluble, the present invention utilizes particularly convenient monoammonium phosphate, which is partly soluble and partly has the advantage of contributing to the nitrogen supply of the rumen bacteria. If this phosphate is used, the amount of carbamide must be adjusted according to its presence, so that the balancing of the nitrogen available for the bacteria with the mineral nutrient components takes into account the nitrogen content of the phosphate.

Of the mineral nutrients, Mg and S will be present in sufficient quantity by virtue of the presence of the calcined silica. As for trace minerals, it has been found that Fe, Zn,

Cu, Mn and Co are present. Since they must be present in soluble form, they will always be added as salts, usually as sulphates with or without crystal water; most often it is preferred to use these salts as their usual forms, ie. as for the zinc sulphate with 7 moles of crystal water, for the rest without. The trace oxidation (valence) of the trace metals seems insignificant.

A desired ratio of nitrogen (N), phosphorus (P) and sulfur (S) is the ratio N: P: S 10: 2: 1, but some variation is possible taking into account the feed that is otherwise used.

An appropriate composition of the nutrients, apart from the anti-baking agent and the micronutrients, is 22-40%, preferably approx. 30% nitrogen, 3-9% and preferably approx. 6% phosphorus and 1-6%, preferably approx. 3% sulfur, the percentages being weight% of the N-, P- and S-containing nutrients in the feed concentrate.

Such a ratio can be obtained with a mixture containing 57% carbamide, 24% monoammonium phosphate, 10% calcined Kieserite, 4% micromineral mixture (with the composition 25% iron sulphate, 25% zinc sulphate, 5% copper sulphate, 20% manganese sulphate, 23% sodium chloride and 2% cobalt sulfate), 0.02% vitamin A / D, 0.1% vitamin E, and 4.88% anti-caking agent; all percentages are weight percent. This mixture contains 28.8% nitrogen, 5.7% phosphorus and 2.6% sulfur or, based solely on the content of carbamide, monoammonium phosphate and calcined Kieserite 31.6% nitrogen, 6.3% phosphorus and 2.8 % sulfur, corresponding to a ratio of 10: 2: 0.9.

As an anti-caking agent, any of the usual anti-caking agents used as food additives can be used, provided that it is harmless to the rumen flora. An anti-caking agent which contributes to the mineral nutrition of the female flora may well be used, but since the preparation of the preparation is cheapest by using standard mixtures of trace minerals, and since a composition such as the above is a standard mixture, it is most appropriate if anti-caking. -the agent is inert to the mineral nutritional needs of the rumen flora. On the other hand, it is irrelevant whether the anti-caking agent can contribute to the carcinogenic nutrition of the rumen flora.

In itself, the anti-caking agent could well contribute to the nitrogen nutrients of the microorganisms, provided that the other components of the mixture are adapted accordingly.

Examples of suitable anti-caking agents include in particular calcium aluminum silicates, tribasic calcium phosphate (in which case the amount of monoammonium phosphate must be adjusted accordingly), calcium silicate and sodium aluminum silicate. Particularly conveniently, according to the invention, the anti-caking agent may be substantially insoluble in water and rumen liquid, and as examples of such agents may be mentioned various forms of silica, for example in the form of a suitable form of diatomaceous earth.

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Perlite is particularly preferred as an anti-caking agent.

Depending on the grain size, the amount of anti-caking agent may vary within a relatively wide range, for example between 1 and 10% by weight of the entire feed concentrate weight. In general, according to the invention, it has been found that an amount of approx. 5% of the total concentrate weight is appropriate.

It has been found that at least a portion of the anti-caking baking agent, at least ca. 20% of the total weight of the anti-caking agent should be added to the mixture of the other ingredients before or at the latest during heating to approx.

80 ° C, while the residue may be added while maintaining the mixture at this temperature, but should be present before cooling occurs. Conveniently, it proceeds as set out in claim 2. It is also possible to add the entire amount of anti-caking agent before or during the heating.

It is most convenient to do the cooling relatively quickly, at least until the temperature is below approx. 60 ° C, to definitely avoid baking.

The method according to the invention will now be described in more detail by an exemplary embodiment.

Example 580 g of carbamide, 240 g of monoammonium phosphate, 100 g of calcined Kieserite, 40 g of micromineral mixture (consisting of 25% iron sulphate, 23% zinc sulphate, 5% copper sulphate, 20% manganese sulphate, 2% cobalt sulphate and 25% sodium chloride) and 10 g ("Dicalite" ®438) was placed in a plow shovel mixer ("Lodige", type M) and mixed thoroughly while heating to approx. 82 ° C until the mixture had become cohesive; it took approx. 15 minutes. Then an additional 40 g of perlite ("Dicalite" ® 438) was added and after mixing for a few minutes the mixture was drained in hot state and cooled on trays.

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The grain size distribution was determined by sieve analysis:> 2000µ 4.90 g 4.6%> 1250µ 25.62 g 24.0%> 800µ 64.26 g 60.1%> 600µ 96.40 g 90.2%> 500µ 103.00 g 96.4%> 300µ 106.55 g 99.7%> 200µ 106.84 g 99.9%> 100µ 106.89 g 100.0%> 0µ 106.90 g 100.0%

To assess the usefulness of the product, it was placed in a heat cabinet at 60 ° C for two days, thereby showing no lumping or baking tendency.

In comparison, a similar product was prepared and of the same composition, but in such a way that the entire amount of perlite acting as a special anti-caking agent was added after the mixture had reached the temperature of approx. 82 ° C and had become cohesive. After cooling, this product showed a slight clumping tendency when placed in a heat cabinet at 62 ° C. The grain size distribution was approximately as indicated above.

For further comparison, similarly prepared - with total addition of perlite after reaching the maximum temperature and the mixture becoming cohesive - a similar preparation whose composition differed only from the previous two by replacing the 100 g calcined silica with 200 g MgSO ^, 71 ^ 0th Here it was heated only to 45 ° C, as the mixture became easily cohesive already at that temperature. When attempting to store the cooled product in a heat cabinet at 60 ° C, it showed strong lumping tendency. The grain size distribution was approximately as above.

For comparison, a product was also prepared as the former, but using uncalcined Kieserite (MgSO 4 O) instead of calcined Kieserite, and otherwise in the same way. The uncalcined silica is very heavy-soluble, and the mixture did not form granules under the forward position, but remained a mixture powder which did not exhibit baking tendency.

Finally, for comparison, a product which deviated from the former was prepared by containing no anti-caking agent at all, but in which the magnesium sulfate as prescribed by the invention was used as calcined Kieserite. This product showed strong baking tendency. The grain size distribution was approximately as above.

In the method according to the invention, a granulate can be prepared for use as a supplementary feed for ruminants and which is stable for a long time, even in hot climates, and which can withstand robust transport conditions, for example in tanker or by pneumatic route. The product maintains constant composition and can be injected into roughage, for example, cut straw or hay and distributed evenly in it without any separation tendency. The product can therefore be manufactured industrially and mixed into the final feed on individual farms.