DE3235523A1 - FERTILIZER COMPOSITIONS, METHOD FOR THE PRODUCTION THEREOF AND METHOD FOR THE USE THEREOF - Google Patents

Description

Fertilizer compositions, processes for their preparation and methods of using them

General state of the art

The invention relates to a new fertilizer product in compound Granulate form, a process for its production and a process for its use. In particular the invention relates to a granular fertilizer product in which the grains have a strength, size and weight own that for a mechanical distribution and

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Application on or in the ground are suitable. These new fertilizer granules result in a new one. Combination of fine particles: A nitrogen source in Macroparticle form, such as melamine, along with a Binder such as urea, which binds the nitrogen starting material present in macroparticles in granular form is suitable.

Ammonia, ammonium nitrate, and urea are the most common used raw materials for nitrogen, but all of these nitrogen fertilizer products are readily soluble in water. For this reason, they are subject to leaching and their use causes rapid release of nitrogen. Since this fact repeated applications to maintain a growth or requiring a single application with higher washout losses, many developments have been made that To slow down the release of nitrogen from the fertilizer products. Generally, such products sacrifice the nitrogen for control purposes beyond the availability of nitrogen.

Melamine and its hydrolysis products, ammeline, ammelide and cyanuric acid have been viewed as possible sources of nitrogen for incorporation in fertilizer compositions or for use as a nitrogen source per se. Melamine has a nitrogen content of 66.6 yes. If it could be used as a fertilizer material it would yield a large proportion of nitrogen per unit weight used. However, at the present time it is more expensive than urea. In addition, it is commercial

manufactured melamine only as a fine crystalline Powder available. It is made in the form of very fine crystals because this is for the present commercial end users of melamine are required, e.g. the production of melamine-formaldehyde resins and the production of fire retardant paints.

A typical sieve analysis for a commercially available one Melamine, done with United States standard mesh screen, is as follows:

Sieve analysis percentages obtained

40 mesh
40 - 50 mesh 50 - 60 mesh 60 - 80 mesh 80 - 100 mesh 100 - 200 mesh 200 - 325 mesh over 325 mesh

Mesh = number of stitches per inch linear

The commercially produced small melamine crystals are made Desired by resin manufacturers because small crystals dissolve more easily and larger particles when they are present would require a longer process time; therefore, the larger particles are less desirable. In the field of the fire retardant paint market, the melamine crystals are dispersed in the paint where the small ones used continuously Particle sizes a smoother structure in the dried

0 - 0.1 0 - 0.1 0 - 0.3 0 .5 - 5.0 1 .0 - 5.0 13 - 30th 13 - 30th 40 - 60

Color appear as larger particles.

The fine particle sizes of the commercially available Melamine products make melamine appear as a product, which is not very suitable for agricultural use cases. In addition, the fine particles make it large of the currently commercially produced melamine impractical for use as a fertilizer material. the fine particles were when they hit the surface of the Applied to the ground, can be blown away even in low winds. For an application from the For example, air from an airplane or a helicopter, drifting would be a serious problem and would cause uneven application. at When applied by mechanical dispensers, the fine particles would tend to bridge and develop this way clog transport and distribution facilities. These difficulties in handling commercially available melamine solids would make any application on a larger scale in agriculture than impractical oppose.

Description of the invention

In one aspect of this invention, it is based on one Fertilizers in granular form. The fertilizer granules have a strength, sizes and weights that are suitable for one mechanical distribution are suitable for use on and in the ground. The preferred size range is is between about one millimeter and about 10 millimeters and is the most preferred size range

between 3 mm and 5 mm.

These fertilizer granules have a nitrogen feedstock of macro-particle size and a binder. The nitrogen source is characterized by fine particle size of not larger than about 10 mesh, by poor solubility in pH 7 water at 2O ⁰ C, and by a long same conversion in the soil to a form in which they are useful for growth of plant life in the soil is. The nitrogen starting material is selected from a group of materials consisting of melamine, ammeline, ammelide, cyanuric acid, mixtures thereof, their inorganic salts, their organic salts and mixtures thereof. The binder is present in an amount which is at least sufficient to bind the fine crystals or powder particles of the nitrogen feedstock together to form granules which have the desired strength. It is preferably a readily soluble material which, after the granules have been dispersed in the soil, releases the nitrogen source particles to allow the particles to act on the particles by water and microorganisms. The binder is selected so that it is compatible with the soil and any residues of the binder will either be inert, biodegradable, soil improver or be of nutritional value to the plants.

The binder is selected from the group of materials that include urea, ammonium sulfate, potassium sulfate, ammonium nitrate ,, ammonium phosphate, potassium nitrate, potassium chloride, ammonium chloride, potassium dihydrogen phosphate, lignin sulfonate,

Currently

Urea formaldehyde resin, melamine formaldehyde resin, starch » Composed of latex and mixtures thereof.

According to a preferred embodiment of the invention, the granules contain up to 80% parts by weight of the nitrogen starting material present in macro-particle size and at least 20 % parts by weight of the agent.

According to an even more preferred embodiment of the invention, the granules contain from 60 to 80 % parts by weight of melamine and from 20 to 40 % parts by weight of urea. According to another preferred embodiment of the invention, the granules contain 67 to 80 % parts by weight of melamine and 20 to 33 % parts of urea. In a most preferred embodiment of the invention, the granules comprise about 67 parts by weight of melamine and about 33 parts by weight of urea.

Another object of this invention relates to a Granules made by a process that includes an annealing step for increased strength of the granulate and these for use as a raw material for nitrogen for fertilizer applications to make suitable. This process involves mixing a nitrogen source in Macro part size that comes from the group of the above materials is selected with an effective amount of a suitable binder to bind the nitrogen source particles in granules that have sizes and weights that make them suitable for mechanical use are. The mixture is then applied with a jet of water

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brought into contact with an aqueous solution of the binder. The moistened mixture is agglomerated, dried and calcined. According to a preferred embodiment of the invention, the method requires a drying temperature of less than 93 ⁰ C and an annealing temperature between 135 ⁰ C and 149 ⁰ C according to a most preferred embodiment of the invention, this granulate of a mixture of 50 to 80 parts by weight of melamine and 50 prepared up to 20 parts by weight of urea.

Another object of this invention is to provide a fertilizer in prill form (granules produced by spray crystallization) directed. This prill is prepared by mixing an effective amount of molten binder obtained from the Group of the above binder materials has been selected, with fine powder particles of a macro-size Nitrogen starting material selected from the above group became. Drops of this mixture are then cooled to form prills. According to a preferred embodiment According to the invention, these prills have from 40 to 65 parts by weight of melamine as the nitrogen source and from 35 to 60 parts by weight of urea binders. According to another preferred embodiment of the invention this prill has 50 to 60 parts by weight of melamine and 40 to 50 parts by weight of urea.

Another aspect of this invention includes a method of making a fertilizer product in US Pat granular form which is suitable as a source of nitrogen for fertilizer purposes. This procedure includes mixing a nitrogen source in

Macro particle size selected from the above group and an effective amount of a binder selected from the group above. The procedure involves a Contacting the misehing with a jet of water or an aqueous solution of the binder, agglomerating the wetted mixture to form agglomerates and drying the agglomerates. The agglomerates are screened to produce agglomerates of product that are sized in a range of preferably 1 mm to 10 mm. Oversized particles can be crushed to this size and finer ones can be recirculated.

According to a preferred embodiment, the method requires mixing 50 to 80 parts by weight of melamine with 50 to 20 parts by weight of urea binder. After a most preferred embodiment includes this Method of mixing about 67 parts by weight of melamine with about 33 parts by weight of urea.

According to another embodiment, this invention includes a process for the production of a granular agglomerate which is suitable for the use of a raw material for nitrogen for fertilizer applications, which includes a subsequent annealing step which follows in addition to the mixing, contacting, agglomeration and drying steps of the above process. According to a preferred embodiment, this invention includes an I rocknen the agglomerates at temperatures of less than 93 ⁰ C, and a glow of the dried agglomerates at a temperature between 135 ° C un 149 ° C. In another preferred embodiment, this method involves mixing 50 to 80 parts by weight of melamine and 50 to 20 parts by weight of urea. Usually will

a compressive strength of 1000 grams or more, where the annealing was carried out at a heating of 135 ° C to 149 ⁰ C on those prepared from melamine and urea granules.

In another aspect, this invention relates to a method of fertilizing plants containing a distribution of a granular product on the soil, which is a nitrogen source in macroparticulate form which is selected from the above group and an effective amount of a binder from the above. Group of binders has been selected.

In a preferred embodiment this includes Process a distribution of a granular product on the ground containing 80 parts by weight of the nitrogen starting material and comprises at least 20 parts by weight of binder. In a most preferred embodiment, this method involves dispensing a granular product containing up to 80 parts by weight of melamine and at least 20 parts by weight of urea

In another embodiment, this invention relates to a method for fertilizing plants, which involves dispensing on the ground a granular product that has a strength, size and has a weight suitable for mechanical dispensing and application obtained by mixing a effective amount of a binder selected from the above group of binders, and a Macroparticle-sized nitrogen feedstock that consists of

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selected from the group of the above nitrogen starting materials is formed. After the mixing step, the method includes contacting the mixture with a Water jet or an aqueous solution of a binder, agglomeration of the moistened mixture, to form agglomerates, drying the agglomerates and calcining the dried agglomerates. After a In the preferred embodiment, this process involves mixing melamine as the nitrogen source in macroparticle size with a urea binder. According to another preferred embodiment, this method includes fertilizing a cereal plant, of potatoes or rice.

In these methods of fertilizing plants is the total rate of application so that sufficient long-term nitrogen fertilization is added for an entire growing season A first advantage of this method and the use of the composite granular fertilizer, which made according to the invention is that the rate of application of the fertilizer is generally less than half of that is required is to get comparable results when ammonium sulfate as the only raw material for Nitrogen is used and applied as a solution via a sprinkler system with a sprinkler system will.

Another aspect of this invention relates to a method of providing a slow release of a Nitrogen fertilizer source on field soil as a food

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2?

source of resources for a plant by introducing and dividing into macro-particle form a nitrogen fertilizer raw material in the soil in the root zone, the starting material being poor in solubility in pH Water at 20 C is characterized, This slowly releasing nitrogen starting material can be melamine, ammeline, Ammelide, cyanaric acid, their organic or inorganic salts or mixtures thereof. After applying the solid form of the nitrogen starting material on the surface of the soil, a part of the soil is turned over to bring the fertilizer to the desired depth range to be introduced into the soil and distributed.

In another aspect, this invention relates to a method of using the slow release
Nitrogen raw material, as described above, in the form of a solid sludge in a sufficient amount of a liquid binder for the nitrogen raw material, which the application of the slowly releasing
Fertilizer particles and their distribution in the ground allowed.

Definitions:

The term "poorly water-soluble" relates to materials that are in water at 20 ° C, pH 7, to an extent of
Dissolve 5 grams per 100 grams or less; this means materials that form solutions of less than 5 % concentration.

The term "poor solubility" in pH 7 water at 20 C has the same meaning here.

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The term "readily water-soluble" refers to materials that dissolve in water at 20 C, pH 7, to the extent of 20 grams per 100 grams; this means materials that form solutions of 20 % or an even higher concentration.

Based on available information, the solubilities in water of 20 C, pH 7 are for various Materials useful in connection with this invention, in grams per 100 grams:

Table 1
Solubility values

material

Melamine ammeline ammelide cyanuric acid melamine nitrate ammonium nitrate Ammonium sulfate diammonium phosphate

Potassium Sulphate Potassium Sulphate urea

q / 100q

0.50 0.008

less than 0.008 0.27 0.85 192

75.4

131 (at 15 °) 51 .4 11 .1 119.3 (at 25 ° C)

Detailed description of the invention

Fertilizer products according to the present invention are in granular form, with sizes in the range of

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about 1 mm to 10 mm, preferably 3 mm to 5 mm. They are manufactured in such a way that they can be poured easily, are a seemingly desirable specific gravity and are substantially free from dust. The granules are manufactured in such a way that they are suitable for mechanical distribution and application on or in the ground are suitable with modern tools.

Granular fertilizer products can in accordance with preferred embodiments of the invention in US Pat Be in the form of agglomerates or prills. The agglomerates can be made by any conventional technique by agglomerating the fertilizer products using poorly or poorly soluble nitrogen fertilizer starting materials of the present invention, followed by an annealing treatment to achieve sufficient compressive strength. In this way, the poorly or poorly soluble nitrogen starting material is made into an agglomerate selected from the group consisting of melamine, ammeline, ammelide, cyanuric acid, "mixtures thereof, their inorganic salts, their organic salts and mixtures thereof. These salts are preferably selected from the group the hydrochloride, hydroiodide, metaphosphate, nitrate, orthophosphate, orthophosphate dihydrate, polyphosphate, Potassium dihydrogen phosphate, bisulfate, and sulfite, and likewise Acetate, cyanurate, chloroacetate, formate, benzoate, fumarate, lactate, maleate and phthalate and mixtures thereof. These materials are characterized by poor or poor solubility in pH 7 water at 20 C and by a slow transformation in the soil into a form in which nitrogen is necessary for plant growth Soil is useful,

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These nitrogen feedstocks, as generally commercially available or as prepared, are in the form of very fine particles. In the case of melamine 2.B. the commercially available product typically has crystalline particles that are smaller than 10 mesh, US standard sieve size, and generally mostly smaller than 40 mesh. These very fine, powdery nitrogen raw materials are agglomerated through the use of a binder. In general, the binders form at least one percent by weight of the pulverulent particles, preferably at least two percent by weight of the pulverulent particles and even more preferably at least 5 % of the pulverulent particles. The binders can be selected from a very wide range of materials, but preferably they are selected so that they are compatible with the soil, so that it and any residues thereof are either inert, biodegradable, soil improver, or have some nutritional value to plants own.

The binder to be used should be sufficiently hard to cure or heat treat the granular Agglomerates give a compressive strength of at least 454 grams, as happened by tests at ten Selected agglomerates were determined, with sizes ranging from 3 to 4 mm, with the results were averaged. Preferably, however, the compressive strength is at least 680 grams, in particular Grams or higher. A compressive strength of approximately 454 Gram is conventional, commercial, prilled

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ti

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Similar to urea and of sufficient strength to be used in most commercial applications, such as area treatment equipment, spreading machines, planter stalk application equipment and distribution of airplanes and helicopters.

Between the preferred exemplary embodiments are those of the group comprising lignosulfonate and its salts, starch, Urea, urea-formaldehyde resins, melamine-formaldehyde resins and latice made from synthetic polymer materials. Such binders are most preferred which have a phytonutrient value, such as urea, Urea formaldehyde and melamine formaldehyde resins are.

According to a preferred agglomeration technique, this is Melamine powder with 5 to 25 percent by weight of powdery!) Urea blended to make a mixture. This mixture is then made up with water or a solution Urea sprayed in an agglomeration device such as on a rotating disk or in a rotating drum. In the case of a binder solution, the particles are coated. In case of a Water spray either dissolves the urea or it becomes damp and sticky; definitely it coats the powdered melamine particles in sufficient Dimensions to initiate agglomeration. The agglomerates are dried and cooled to form hard constituents to result in sizes generally in a range from about 1 mm to about 10 mm, and preferably 3 mm up to 5 mm. This composite has good compressive strength and is essentially dust-free.

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Any of the known agglomeration techniques can be used will. In this way all binders can be used in solution. If the binder is a material such as lignin sulfonate, urea formaldehyde resin or melamine formaldehyde resin solution form application will generally be most convenient. The binder can also be a material such as phenolic resin, which is in solution form is applied, but such a material, although it has excellent properties as a binder, can do not contribute any nutritional value and is therefore less desirable · The same considerations apply to synthetic polymer latice.

The fertilizer particles according to the invention can also be used in be made in the form of prills. In the prilling process (crystallization), melamine powder is melted Binder material, preferably urea, added to a slurry of melamine powder particles to form in the "molten urea. Drops of this molten slurry are produced by that they are dripped through a prilling tower, solidified in a known manner. Urea is the preferred material for the production of prills because of its nitrogen content and its easy solubility in water and also because melamine is somewhat soluble in molten urea, but so are other materials, such as sulfur and mixtures of materials could be used. In the production of urea bound prills is used it is preferred that the prilled product contain at least 33 weight percent urea. When there is less urea it is difficult to create a flowable suspension to create. The urea content of the prill can be up to

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$ 3

90 percent, so that the melamine content in one Range from 10 to 67 weight percent of size. The urea content is preferably between 35 and Percent by weight of the prills and the preferred range is between 40 and 50 percent by weight.

While preferred granular products are made by agglomeration and prilling, satisfactory ones can also be used Products can be manufactured using other techniques, such as injection techniques, pressing and granulating and Briquetting. For example, melamine powder or a powdered Melamine salt or the like. with a urea formaldehyde resin in powder form can be mixed to form a mixture. The mixture can be at an elevated temperature pressed to crosslink the resin and the resulting product can be granulated to form particles of the desired size, or the compressed, crosslinked mass can be converted into flake form. Sifting and recycling may be necessary to form granules of the desired sizes.

Easily soluble binders, such as urea and salts, such as ammonium nitrate allow a quick dissolution of the binding agents of the fertilizer granules in the soil, whereby the fine melamine or other fine particles are released. This can also be desirable, though the mixture not only melamine, but also easily soluble, having quick release nitrogen fertilizer material. If a slow release is desired, one of the binders that slowly releases the fertilizer power into the soil is commonly used, such as e.g., a urea-formaldehyde resin or a melamine-formaldehyde resin.

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Urea is a preferred binder for agglomerates or for the production of prills, because it is not only the production of fertilizer granules of sufficient Size, strength and weight allowed for convenient administration, but also because urea is easily soluble and in addition valuable and quickly released nutrient material in the soil adds. When used with a powdery nitrogen source, which is caused by a bad or is characterized by poor solubility and slow conversion in the soil to a usable form, the urea dissolves quickly and deposits the fine particles of the poorly soluble nitrogen source in the soil free for slow dissolution or biodegradation.

When an agglomerate is made from powdered melamine and a readily water soluble binder such as urea are preferred Amount ratios in the dried granular product obtained between 60 and 85 percent by weight of melamine and between 40 and 15 percent by weight urea, or more preferably between 67 and 80 percent by weight Melamine and between 33 and 20 percent by weight urea. Most preferred granules are about 67 Parts by weight of melamine and approximately 33 parts by weight of urea on.

In a preferred embodiment, from 85 to 99 parts by weight becomes that in macroparticulate form Nitrogen source combined with 1 to 15 parts by weight of a resinous binder selected from the group consisting of

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choose which lignosulfonate, urea-formaldehyde resin, Melamine-formaldehyde resin, latex or their mixtures contain. In an even more preferred embodiment, 95 parts by weight becomes melamine and 5 parts by weight of the specified resinous binders combined.

If an agglomerate is used, using an insoluble or only slightly soluble binder, such as starch, a derivatized starch, a modified starch, lignosulfonate, urea-formaldehyde, ormelamine-formaldehyde or one of the non-nutrient-containing Materials such as phenolic resin or a synthetic polymer in the form of a latex becomes a very slow release of nitrogen from the melamine particles (or particles of another poorly soluble Nitrogen source).

For the production of a single agglomerate Allowing administration per growing season, nitrogen fertilizer rapidly releasing materials, in general an ammonium salt or urea, advantageously used as the binder for the agglomerate. Examples of such salt-like binder materials are ammonium sulfate, potassium sulfate, ammonium phosphate, Diammonium phosphate, the potassium phosphate, ammonium nitrate, Potassium nitrate, potassium chloride and ammonium chloride. When a Binder material is used in the formation of an agglomerated composite, the proportion of such a salt-like binder material between 15 and 40 percent by weight of the agglomerate, and in particular between 20 and 33 percent by weight of the agglomerate.

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In addition, other materials can be incorporated into a granular fertilizer product as appropriate of the invention are made. Such materials can be micronutrients such as zinc, magnesium, Iron and boron>

One of the advantages of using granular Fertilizer compositions made in accordance with the present invention is that the rate of application in the form of nitrogen per unit area used can be much lower than it is is possible with conventional fertilizer practice. Because less active material is actually needed, it may be desirable to facilitate administration and, in some cases, an inert filler admit. Any of the known filler materials can be used, such as plaster of paris, Clay, sand, seashells, dolomite and limestone.

Another important advantage of using granular fertilizer products in accordance with of the present invention is that it is possible to give only a single administration per growing season due to the slow release characteristics. Furthermore, after the first administration, in the case of melamine-based fertilizer products, the release of nitrogen into the soil occurs over two growing seasons. As a result, in the second and subsequent growing cycles, even fewer administration rates may be desired for

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Results are made as it is for the first administration may be required.

Another effect of the invention is the unexpected and surprising finding that the supply of a majority or all of the nitrogen fertilizer requirements by a nitrogen fertilizer source according to the present invention Invention apparently leads to a more efficient production of agriculturally productive units per unit weight of nitrogen administered and per unit of growth area. One agricultural productive unit is a seed, fruit, flower, vegetable, plant fiber, tubers or the like .. Additionally leads the use according to the invention obviously to total yields for planting units that are comparable to those with the known standard fertilizer practice can be achieved, for which purpose, however, a much higher need for an administration of nitrogen fertilizers

require .

Generally speaking, the invention provides a method of increasing the effectiveness of usually easily dissolve, quick release stock fertilizers in creating productive units in agricultural crops / supplementing their action with the use of a slow release, poorly or poorly dissolving nitrogen fertilizer source. In this way a combination of about 10 to 50 % nitrogen in a common readily water soluble, quick release nitrogenous fertilizer can advantageously be combined with about 50 to 90 % slightly soluble materials such as the above.

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The agricultural crops expected from that they respond to the treatment according to the invention, include essentially all plants, but particularly this applies to plants where the fruit is harvested Unity is and not the whole plant. Such plants are e.g. food grain, feed grain, Legumes, fibers, root crops, citrus fruits, Tubers, oily units such as nuts, fruits and seeds, commercially available vegetables, commercially available melons, Tree fruits, grapevines, bush fruits and flowers. Food grain are e.g. wheat, rye and rice, fodder grain plants are e.g. field grain, oats, barley and sugar cane. Legumes are e.g. soybeans, peanuts, Beans and peas. Fiber plants include cotton, hemp and jute. Root plants are potatoes and sugar beets. Citrus fruits include oranges, mandarins, Grapefruits, lemons and limes. Tubers are potato. Oily plants include flax, saffron, sunflower, and castor beans. Commercially available Vegetables include pole, bush and Spring beans, beetroot, carrots, corn, cucumber, onions, green peas and tomatoes. Commercial melon plants include bump meions, honey melons, and watermelons. Tree fruit plants are apples, peaches, pears, Cherries and plums. Grapevines concern grapes. Bush fruits contain the different types of berries, especially raspberries and blackberries. Tree nut fruits include almonds, hazelnuts, pecans, and walnuts. However, this information is only an example.

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The invention is made with reference to the following Examples better understood. Throughout this application and in these examples, all references are to shares and percentages by weight and all references to temperatures are in degrees Celsius, except for is indicated differently.

Examples of the formation of granules useful in the process of the invention

In all of the following examples the melamine used is the commercial product of Melamine Chemicals, Incorporation, Donaldsonville, Louisiana. It is a fine white crystalline powder that exhibits sieve analysis as indicated above for the commercially available melamines. It is approximately 99.9 % pure, with specifications of a maximum moisture content of 0.1? E, maximum ash of 0.01 %, and a density of approximately 1.57 g / ml.

As pointed out in some of the examples below, a compressive strength of 454 grams or greater is preferred. Preferably, compressive strengths of 1362 grams or more are designed to facilitate administration. The bulk density of the granules should also be 40 lbs./ft ³ (0.64 g / cm ³ ) or more.

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The preferred combination of bulk density, compressive strength and particle size contributes to flexibility the administration. Usual compressive strengths of 1000 grams or more can be achieved when the glowbzw. Tetnperstufe of heating to 135 ° C to 149 ° C the melamine urea granules is exercised.

example 1

Melamine agglomerates with the use of a urea binder

Three batches of the composite granules were made, each containing different amounts of urea and melamine and with urea as a binder served. These batches of agglomerated granules were produced in a tub agglomerator with a diameter of approx. 22 cm. The urea was first ground and then mixed with the melamine powder | to make a homogeneous mixture to reach. The powder mixture was then fed to the vat agglomerator and with a near saturation Sprayed solution of urea and water. The solution added approximately 7 urea to the dried agglomerate to. The residue of the urea content was from the urea powder in the urea-melamine powder mixture removed.

¹ H.

Example 2 Annealed melamine granules

A batch of granules was prepared using 67 parts of melamine crystals and 33 parts of urea. The granules were produced on a disk pelletizer of approx. 45 cm. The urea was first ground, then mixed with the melamine to obtain a homogeneous mixture. This mixture was then placed in the pelletizer and sprayed with water. The granules were ^{dried at 94 °} C. for about 20 minutes and then subjected to a further heating stage in a laboratory oven at 149 ^° C. for three minutes. After cooling, the compressive strength and the dissolution in water were measured. These values are listed in Table I below.

Table 1

Compressive strength dissolution time in

water

Example 1 600 immediately

dried granules example 2

Annealed or tempered granules 2400 20 to 30 seconds

This example shows the / relationship between time and temperature in the annealing stage.

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Example 3 Annealed melamine granules

Melamine granules were prepared according to Example 2 and heated in separate Chragen at 104 ⁰ C 149 ⁰ C and 172 ⁰ C for different times. A standard laboratory oven was used. After cooling, the compressive strength was measured. The result is shown in Table II. The highest compressive strength appears at 172 ⁰ C at a öminütigen warming. The highest compressive strength appears at 149 ° C when heated for 11 minutes. Shorter drying and annealing times can be achieved in production if more powerful air dryers or ovens are used in place of the laboratory oven used in these examples.

Oven temperature

Table II Pressure Heating minutes in grams 560 20th 350 4th 881 5 978 6th 1333 7th 1290 θ 1530 9 1480 10 1780 11th 1300 12th 1640 13th 1445 14th 1530 15th 1454 20th 763 4th 1125 5 1340 6th 1200 7th 825 8th

149 ⁰ C 172 ° C

Example IV

Melamine agglomerated with urea powder; Water spray

A batch of agglomerated granules was prepared in a tub agglomerator according to Example I, with the exception that all of the urea was added as a powder and the spray applied in the tub consisted only of water. The resulting composites contained 80 % melamine and 20 % urea, and after sieving to 3-4 mm, a compressive strength of 953 g was found using the same test technique as in Example I.

Example V

Use of other binders to agglomerate melamine

Granular agglomerates were made with a pan agglomerator of about 40 cm using melamine with different Binders produced. In each case the binder was sprayed onto the melamine in liquid form. After drying, the compressive strength was determined as in Example I. The results are in the following Table III shown.

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Table III Observed compressive strengths

Agglomerated melamine with various binders

Binder compressive strength,

Grams of 3-4 mm agglomerates

Calcium Lignosulfonate 908

UCAR 368 Latex ¹ - 681

Me lamin formaldehyde resin 1544

■ \

Urea formaldehyde resin 454

Diammonium Phosphate (DAP) 91

Ammonium nitrate 150

Added at 30 - 50 % dry matter. The dried ones

Agglomerates had approximately 5 % binder.

"Essentially saturated solutions were used.

The dried agglomerates were approximately 93 % melamine

and 7 "ό salt.

Example VI

Melamine that has been agglomerated with other fertilizer materials

Melamine, ammonium phosphate and potassium chloride were mixed together in a weight ratio of 70:15:15. the

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The mixture was introduced into a tub agglomerator of approx. 40 cm and sprayed with a 30% solids content of lignin sulfonate solution. The dried, sieved granules had a compressive strength of 1000 g in the size range of 3 - 4 mm and a binder content of 3 S.

Example VII

Melamine in a matrix of solidified urea binder

Melamine and urea powder were in a ratio mixed from 63-37. The mixture was heated until a molten slurry was obtained. The mud was then poured onto a cold plate to form both thin and thick films. After cooling down the thin film was broken into flakes. The thick film of about 4 mm thick was made into granules Broken. The compressive strength of the 3 - 4 mm large granules was extraordinarily hobh, namely at 2500 g.

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Example VIII A pressed melamine-urea composite

A melamine-urea mixture was prepared as in Example VII. This mixture was then placed in a heated platen press at approximately 500 psi for 5 minutes at 138 ^° C. The resulting hot composite in the form of a sheet approximately 4 mm thick was then removed from the press and allowed to cool. The cooled layer was granulated and the resulting 3-4 mm granules of the composite had a compressive strength of 2500 g.

Example IX
Melamine urea from 60/40 prills

Melamine composite prills were made by heating 40 parts by weight of urea with 60 parts by weight of melamine. The heating was carried out in an aluminum pot using an electric heating tape. A sludge was formed at 135 ^{° C.} Holes were then made in the aluminum floor, allowing the sludge to drip out. A plastic sheet spread out on the floor caught the falling prills after they had dripped from the level of a fourth floor.

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The largest prill did not cool down before they hit and shattered. But the smaller prills were cooled and solidified and were collected for the measurement of compressive strength. Sufficiently good ones Strength results were achieved even though they were not measured. It would have a compressive strength expected, which would be similar to that of the granules from Example VII.

Example X

Melamine agglomerated with a latex binder

5 % Union Carbid UCAR 368 latex, 15 % water and 80 % melamine were mixed into a flowable suspension. ' A layer of the slurry was formed and then dried. An extremely hard composite resulted which could be granulated. The dried material contained 3 ° latex solids and 97 % melamine. The compressive strength of 3-4mm granules was 2180 g.

Example XI

Pressed composite of melamine and urea-formaldehyde

25 g urea, 70 g melamine and 15 ml of a 27% Formaldehyde solutions were mixed together and pressed at 149 ° C and 500 psi to form a thick layer. the The compressive strength of 3-4 mm granules was 680 g

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- κ-

Example XII Helamine Urea Agglomerates for Field Trials

For field tests, approx. 7250 kg of melamine / urea composite was produced using a pan agglomerator with a diameter of approx. 1.2 m. Various composites have been produced with melamine / urea ratios of 80/20, 75/25 and 67/33. Approximately 7 % of the composites were added with urea which was added in the form of an aqueous binder solution and the remaining urea was added as powdered urea which was mixed with the melamine powder before agglomeration. In the above examples, granular fertilizer products were made from commercially available fine crystals of melamine. Similar granular fertilizer products can be prepared in essentially the same manner from the hydrolysis products of melamine, for example ammeline, ammelide and cyanuric acid, and from salts thereof and from melamine. Among the salts, the reaction product of nitric acid and melamine is a preferred material

- 32 -

Example XIII

Grain tests using melamine urea agglomerates; Evaluation of different administration techniques

Test plots of approximately 1600 a (40 acres) of sandy until slightly loamy and muddy soil was treated with various amounts of melamine agglomerates to receive several different levels of nitrogen administered per 40 a (acre). Melamine-urea agglomerated Composites were used according to the example I and had 67 parts of melamine and 33 parts of urea binder; 75 parts melamine and 25 parts of urea binder; 80 parts of melamine and 20 parts of urea binder. The composites were successfully administered using a variety of techniques:

1. Distribution with a barber distributor;

2. Spread with a barber spreader and plow into the ground;

3. Airborne delivery by airplane;

4. Introduction into the soil during planting.

The results obtained are summarized in Table IV a below.

- 33 -

Table IVa Grain trials - effect of the method administered

Nitrogen melamine / administration number d. Average level of urea-rich ears / 100 number of d. Ears of wheat

lbs. /acre 75/25 technology plants per plant 140-150 75/25 (D 155 1 .55 140-150 75/25 (2) 147 1 .47 140-150 80/20 (3) 155 1 .55 150 Con (4) 153 1 .53 0 trolls UN-32 - 132 1 .32 400 * ** 129 1 .29 400 * 145 1 .45

* Standard fertilizing practice, multiple administrations during the growing season »

** A total of 400 lbs.N in the form of UN-32, administered in multiple administrations during the growing season to conform to standard fertilizing practice simulate.

All grain planting attempts listed in these examples, where a comparison has been made, were made within a week, if not substantial were carried out at the same time.

- 34 -

The grain growing in the plots, which was fertilized according to method 2, spread over the area and then plowed in, looked green and robustly healthy. That Grain growing in the plots, which was only fertilized surface-treated, method 1 and 3 yellow as well as green leaves, but it was greener than the grain, which after method 4, introduction after Plants that were fertilized, which looked yellow.

In an effort to estimate results, which ones are the first Ears of corn were counted in the same examples, with the following being available later during the year Inclusions were made: full ears of wheat were classified as one, small ears of wheat as 1/2, and outgrowths as zero counted. This count was shown in Table IVb as the effective ear counts.

In a further evaluation, the grain plants were harvested and weighed, and an ear count was carried out and ear weights were recorded from 2 Test areas. The first area was made with 75/25 melamine / urea agglomerates fertilized by spreading the area of the agglomerates, then they were introduced. the second tract was made according to local standard fertilizer practice with 400 lbs. N / acre fertilized. Standard fertilizer practice requires the administration of total 350 lbs. to 400 lbs. N per year and per acre. This is done in three separate stages.

- 35 -

Table IVb Grain Tests - Effect of the Administration Method

Nitrogen level (lbs./acre)

Melamine/ Appointment Effective number urea reaching of ears of wheat / 100 ** technology 75/25 (D 109.5 75/25 (2) 118 75/25 C3> 120.5 80/20 (4) 60 control - 40.5 UN-32 (D 124.5 * 145.5

Number of average plants / 100 ft. Effective number of ears per plant

cn cn ro co

140-150 140-150 140-150

400
400 * 109 126 115 134 95 128 159

* Standard fertilizer practice, multiple administrations during the growing season ** Whole ears are counted as 1, small ears as 1/2 and outgrowths as 0

1

0.94 ***

1

0.45

0.43

0.97

0.92

*** Ear sizes were also of interest:

at 150 lbs. N, administered as a 75/25 melamine / urea prill: 5-1 / 2 SFP: 4-1 / 2

cm diameter cm diameter

S3

First an early dose was with 200 lbs. N / acre performed like anhydrous ammonia. Second, 400 lbs./acre of 16-20-0 was given (based on Monoammonium phosphate). Third, UN-32, the urea and ammonium nitrate is generated by the irrigation sprinkler system administered. The results are summarized in Table V. All samples were in the pre-mature stage taken, i.e. when the grain was fully developed but still full of moisture and the characteristic Formation of the gap was still missing.

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Table V

Evaluation of the effect of the grain (pre-ripening stage)

CO N) CO

cn cn fs ^ co

fertilization

sample

Selection technique

Number of plants

weight

Number of ears of corn

weight

Ratio of ear weight to plant weight

Melamine / urea 75/25 2 Agglomerates, at 3,150 lbs. N / acre, distributed in area and brought in

75/25 agglomerates 4 at 235 lbs. N / acre, distributed over the area and brought in

75/25 agglomerates 5 at 150 lbs. N / acre, infused

Standard fertilizer - 1 practice, 350 - 400 2 lbs. N / acre 3

\ J ι In the sampling procedure
taken at open positions,
gave .

Sample _1 / sample J_ / Picked from a 50 ft row

Picked from a 50 ft row

Picked from a 50 ft row

10 39 lbs. 20th 18th .5 lbs. 0 .475 I. TO 35.5 20th 16 0 .45 58 122 59 47 .5 0 .39

64

122

134

73

67

49.5

47.5

Sample \ J 10 41 20th 14th Sample 1 / 10 41 20th 16 Withdrawal from 79 142 77 47 a 50 ft row

0.41

0.3-3

0.3h

0.40 ""

0.35 '

large plants have two ears of wheat, each one was from the ends of rows' where there is minimal interference from other grain crops

Claims (59)

Claims 1. Fertilizer product in granular form, wherein the granules have a strength, sizes and weights suitable for mechanical distribution and application on or in the soil, and wherein the granules have: a nitrogen source present in macro-particle size, which is caused by a poor Solubility in pH 7 water at 20 ⁰ C is characterized, this source being selected from a group which contains the following substances: melamine, ammeline, ammelide, cyanuric acid, mixtures thereof, their inorganic Salts, their organic salts and mixtures thereof, and at least an effective proportion by weight of the Fertilizer granules of a binder for said nitrogen source particles, which the nitrogen bind source particles into a granular form. 2. Granular fertilizer according to claim 1, wherein the macro-particle size nitrogen source by a fine particle size is indicated which is not greater than 10 mesh. 3. Granular fertilizer product according to claim 1, characterized in that the granules contain up to 80 parts by weight of the macroparticulate nitrogen source. 4. Granular fertilizer product according to claim 1, characterized in that the granules contain at least 20 parts by weight of a binder. 5. Granular fertilizer product according to claim 1, characterized in that the macroparticle size nitrogen source is melamine and the binder is selected from the group which is urea, ammonium sulfate, potassium sulfate, ammonium nitrate, ammonium phosphate, potassium nitrate, Potassium chloride, ammonium chloride, potassium dihydrogen phosphate, lignin sulfonate, urea-formaldehyde resin, Contains melamine formaldehyde resin, starch, latex and mixtures thereof. 6. Granular fertilizer product according to claim 3 or A, characterized in that the macro-particle size nitrogen source Is melamine and the binder is selected from the group consisting of urea, ammonium sulfate, potassium sulfate, Ammonium nitrate, ammonium phosphate, potassium nitrate, potassium chloride, ammonium chloride, potassium dihydrogen phosphate, Ligninsulfonate, urea-formaldehyde resin, melamine-formaldehyde resin, Contains starch, latex and mixtures thereof. 7. Granular fertilizer product according to claim 1, characterized in that the granules from 85 to 99 parts by weight of the macroparticle size present nitrogen source and from 1 to 15 parts by weight of a binder, the is selected from the group, the lignin sulfonate, Urea formaldehyde resin, melamine formaldehyde resin, Contains latex and mixtures thereof. 8. Granular fertilizer product according to claim 7, characterized in that the macro-particle size nitrogen source Melamine is. 9. Granular fertilizer product according to claim 1 or 5, characterized in that the granules have from 60 to 80 parts by weight of melamine and from 20 to 40 parts by weight of binder. 10. Granular fertilizer product according to claim 1 or 5, characterized by the fact that the granulate contains from 67 to 80 parts by weight of melamine and has from 20 to 33 parts by weight of urea. 11. Granular fertilizer product according to claim 1 or 5, characterized in that the granules from 60 to 80 parts by weight of melamine and has from 20 to 40 parts by weight of urea. 12. Granular fertilizer product according to claim 1 or 5, characterized in that the granules contain from 67 to 80 parts by weight of melamine and from 20 to 33 parts by weight of urea. 13. Fertilizer product in prill form, which is manufactured by: a) Mixing fine powder particles of a macro-particle size nitrogen source which is selected from the group which melamine, ammeline, ammelide, cyanuric acid, mixtures thereof, their inorganic salts ", their organic salts, and mixtures thereof, and an effective one Amount of molten binder, and b) quenching the drops of said mixtures to form prills. 14. Fertilizer product in prill form according to claim 13, characterized in that the binder is selected from the group consisting of urea, ammonium nitrate, potassium dihydrogen phosphate and mixtures thereof. 15. Fertilizer product in prill form according to claim 14, characterized in that the PrJ ₄ Il contains from 10 to 67 parts by weight of melamine. 16. Fertilizer product in prill form according to claim 14, characterized in that the prill contains from 35 to 60 parts by weight of urea. 17. Fertilizer product in prill form according to claim 16, characterized in that the prill contains from 40 to 50 parts by weight of urea. 18. A process for the manufacture of a fertilizer product in granular form suitable for use as a nitrogen source is suitable for fertilizer application and has the following steps: a) Mixing a macro-particle sized nitrogen source selected from the group is what melamine, ammeline, ammelide, cyanuric acid, mixtures thereof, their inorganic salts, their contains organic salts and mixtures thereof and an effective amount of a binder which is suitable is for binding said nitrogen source particles in granules of sizes and weights that make them suitable for mechanical administration, b) contacting this mixture with a Spray jet from water or an aqueous binder solution, c) agglomerating the moistened mixture to to form the agglomerates, and d) drying the agglomerates. 19. A method for producing a fertilizer product according to claim 18, characterized in that the binder is selected from the group which from urea, ammonium sulfate, potassium sulfate, ammonium nitrate, Ammonium phosphate, potassium nitrate, potassium chloride, ammonium chloride, potassium dihydrogen phosphate, lignin sulfonate, Urea-formaldehyde resin, melamine-formaldehyde resin, starch, latex and mixtures thereof. 20. The method according to claim 18, characterized in that the mixture contains from 85 to 99 parts by weight of the in Macroparticle size present nitrogen source and from 1 to 15 parts by weight of a binder has, which is selected from the group consisting of lignin sulfonate, urea-formaldehyde resin, MeIaminformaldehydharζ, Composed of latex and mixtures thereof. 21. The method according to claim 20, characterized in that the macro-particle size nitrogen source Melamine is. 22. The method according to claim 18, characterized in that the mixture contains from 60 to 80 parts by weight of melamine and contains 20 to 40 parts by weight of binder. 23. The method according to claim 19, characterized in that the mixture contains from 67 to 80 parts by weight of melamine and contains from 20 to 33 parts by weight of binder. 24. The method according to claim 19, characterized in that the mixture contains from 60 to 80 parts by weight of melamine and contains from 20 to 40 parts by weight of urea. 25. The method according to claim 19, characterized in that the mixture contains from 67 to 80 parts by weight of melamine and contains from 20 to 33 parts by weight of urea. 26. Process for the manufacture of a fertilizer product in prill form comprising the steps of: a) mixing fine powder particles of a macro-particle size present nitrogen source, which is selected from the group consisting of melamine, Ammeline, ammelide, cyanuric acid, mixtures thereof, their inorganic salts, their organic salts, and mixtures thereof and an effective amount of a molten binder, and b) quenching the drops of said mixture to form prills. 27. The method according to claim -26, gekennzecihnet that the binder urea ammonium nitrate or Mixtures thereof or potassium dihydrogen phosphate. 28. The method according to claim 26, characterized in that the mixture contains from 10 to 67 parts by weight of melamine contains. 29. The method according to claim 26, characterized in that the mixture contains from 35 to 60 parts by weight of urea. 30. Method of fertilizing plants, which includes an application of a granular product on or in the ground, which includes a macro-particle size present nitrogen source, which is selected from the group consisting of melamine, ammeline, Ammelide, cyanuric acid, mixtures thereof, their inorganic salts, their organic salts, and Mixtures consists of it and an effective amount a binder which is suitable for binding the nitrogen source particles in granules, are of sizes and weights that make them suitable for mechanical administration. 31. The method according to claim 30, characterized in that the binder is selected from the group which from urea, ammonium sulfate, potassium sulfate, ammonium nitrate, Ammonium phosphate, potassium nitrate, potassium chloride, ammonium chloride, potassium dihydrogen phosphate, Ligninsulfonate, urea-formaldehyde resin, melamine-formaldehyde resin, Is made up of starch, latex and mixtures thereof. 32. A method for fertilizing plants according to claim 31, characterized in that the granular product from 85 to 99 parts by weight of a macro-particle size nitrogen source and from 1 to 15 parts by weight of a binder, the binder being selected from Group is selected which consists of lignosulfonate, urea-formaldehyde resin, melamine-formaldehyde resin, Composed of latex and mixtures thereof. 33. The method according to claim 32, characterized in that the macroparticle size nitrogen source is melamine. 34. The method according to claim 30, characterized in that the granular product is up to 80 parts by weight of the macroparticulate nitrogen source and at least 20 parts by weight of the binder contains. - 10 - 35. The method according to claim 34, characterized in that the macro-particle sized nitrogen source is up to 80 parts by weight melamine and that Binder is up to 20 parts by weight of urea. 36. Method of fertilizing plants, which involves a distribution of a granular product on or in the soil includes, which has a strength, size and weight that makes it suitable for a mechanical Distribution and administration is appropriate, the granules being prepared in the following manner: a) Mixing a macro-particle sized nitrogen source selected from the group is made up of melamine, ammeline, ammelide, cyanuric acid, mixtures thereof, their organic salts and inorganic salts and mixtures thereof and an effective amount of a binder, which binds said nitrogen source particles in granules that have sizes and weights, which make them suitable for mechanical distribution and administration, b) bringing the mixture into contact with a spray jet of water or an aqueous binder solution, c) agglomerating the moistened mixture to the To form agglomerates, d) drying the agglomerates, and e) Annealing the dried agglomerates. - 11 - 37. The method according to claim 36, characterized in that the binder is selected from the group which from urea, ammonium nitrate, potassium dihydrogen phosphate and mixtures thereof. 38. A method for fertilizing plants according to claim 36, characterized in that the macroparticle size nitrogen source is melamine and the binder is urea 39. A method of fertilizing plants which comprises a distribution of a fertilizer product in prilled form or contained in the ground, characterized by the following steps: a) Mixing fine powder particles of a macro-particle size nitrogen source which is selected from the group consisting of melamine, ammeline, ammelide, cyanuric acid, mixtures thereof, their inorganic salts, their organic salts and mixtures thereof and one effective proportion of a molten binder and b) quenching the drops of said mixture to form prills. 40. The method according to claim 39, characterized in that the binder is urea, ammonium nitrate, potassium dihydrogen phosphate or mixtures thereof. - 12 - 41. The method according to claim. 39 characterized in that the mixture contains from 10 to 67 parts by weight of melamine contains. 42. The method according to claim 39, characterized in that the mixture contains from 36 to 60 parts by weight of urea binder contains. 43. The method according to claim 39, characterized in that the mixture contains from 40 to 50 parts by weight of urea binder. 44. A method of delivering a slow release source of fertilizer nitrogen to a field soil, as a nutrient source for a plant, which includes addition and distribution into the soil in the root region of a macro-particle size fertilizer nitrogen source characterized by poor solubility at pH 7 Water at 20 ⁰ C is characterized, the source being selected from the group consisting of melamine, ammeline, ammelide, cyanuric acid, mixtures thereof, their inorganic salts, their organic salts and mixtures consists of it. - 13 - 45. The method according to claim 44, characterized in that the slowly releasing fertilizer nitrogen source is applied in solid form to the surface of the field soil, and then at least part of the soil is turned over to provide the fertilizer nitrogen source to be brought into the soil in the desired depth range and distributed. 46. The method according to claim 44 or 45, characterized in that the fertilizer nitrogen source in the form of a Sludge of solids is administered in an effective amount of a liquid binder for the nitrogen source particles, which is an administration of the particles and their distribution allowed in the ground. 47. The method according to claim 44 or 45, characterized in that the fertilizer nitrogen source essentially is made of melamine. 48. The method according to claim 45, characterized in that the slowly escaping fertilizer nitrogen source Melamine is and is in the form of a solid sludge is administered, which is suspended in an effective amount of a liquid fertilizer which is a Allows administration of the solid particles and their distribution in the soil. - 14 - 49. Granular agglomerate suitable for use as a Nitrogen source is suitable for fertilizer purposes and is produced by a process that comprises the following steps: a) Mixing a macroparticle size Nitrogen source selected from the group consisting of melamine, ammeline, cyanuric acid, Mixtures thereof, their inorganic salts, their organic salts and mixtures thereof and an effective amount of a binder that for binding the nitrogen source particles in granules are suitable, of the sizes and weights which they are suitable for mechanical administration make suitable. b) bringing the mixture into contact with a spray jet from water or an aqueous binder solution, c) agglomerating the moistened mixture to the To form agglomerates, d) drying the agglomerates, and e) Annealing the dried agglomerates. 50. Granular agglomerate according to claim 49, characterized in that the binder is selected from the group consisting of urea, ammonium nitrate, potassium dihydrogen phosphate or mixtures thereof. 51. A granular agglomerate according to claim 49, characterized in that the binder is urea, the dry solids takes place at a temperature of less than 93 ⁰ C, and the annealing step includes heating at between 135 eine'Temperatur ⁰ C and 149 ° C . - 15 - 52. Granular agglomerate according to claim 49, characterized in that the macroparticle size nitrogen source is melamine and the binder is urea. 53. Granular agglomerate according to claim 49, characterized in that the mixture contains from 50 to 80 parts by weight and 20 to 50 parts by weight of binder. 54. A process for the manufacture of a fertilizer product in granular form suitable for use as a Nitrogen source suitable for fertilizer applications and includes the following steps: a) Mixture of a macro-particle size nitrogen source selected from the group is made up of melamine, ammeline, ammelide, cyanuric acid and mixtures thereof, their inorganic Salts, their organic salts and mixtures thereof, and an effective amount of one Binder suitable for binding the nitrogen source particles in granules, the Have sizes and weights that make them suitable for mechanical administration, b) bringing the mixture into contact with a spray jet of water or an aqueous binder solution, c) agglomerating the moistened mixture to form the agglomerates, d) drying the agglomerates, and d) Annealing the dried agglomerates. - 16 - 55. The method according to claim 54, characterized in that the binding agent urea, ammonium nitrate, potassium dihydrogen phosphate or mixtures thereof. 56. The method according to claim 54, characterized geke is used to mark, Tao, the binder is urea, that the drying stage at 93 ° C and that the annealing step at a temperature between 135 C and 149 ⁰ C ³ takes place. 57. The method according to claim 54, characterized in that the mixture contains from 50 to 80 parts by weight of melamine and from 20 to 50 parts by weight of binder. 58. The method according to claim 57, characterized in that the binder is urea. 59. A method for fertilizing plants according to claim 30, 35, 39 or 44, characterized in that the plant is grain, potatoes, rice or wheat.