DE3017878A1 - AGENTS AGAINST CLUMPING IN SEWING AGENTS AND ITS USE - Google Patents

Description

The invention relates to an agent against the formation of lumps in fertilizers, a method for prevention the formation of lumps in fertilizers through the use of the agents mentioned or at least their components and finally those obtained with the aid of this process and with the use of said means Fertilizer.

15 The object of the invention is to provide a means

to create, with which it is possible to produce fertilizers that do not cause clumping, degranulation and tend to form dust.

0 This object is now achieved by the means according to the invention against the formation of lumps in fertilizers, which is characterized in that it is at least an ester of an oxyalkyl derivative or an alkoxylated derivative and at least one hydrophobic Ver-5 contains bond, the ester of the oxyalkyl derivative

an ester is off

- an aromatic or aliphatic, saturated or unsaturated polyacid, preferably polycarboxylic acid, and preferably a short polyacid

3 0 or polycarboxylic acid and

- one condensed with water, a primary, secondary or tertiary diol or a diphenol Ethylene oxide, propylene oxide or butylene oxide, the condensate of ethylene oxide and water being preferred

35 and where the molecular weight of the condensate is below

10,000, preferably between 100 and 4000 and still more preferably between 3,00 and 4,000.

0300A7 / 085 6

Said ester of the oxyalkyl derivative can also be an ester of an aliphatic, saturated or unsaturated one Monoacid, preferably monocarboxylic acid.

According to a preferred embodiment, the invention the hydrophobic compound is selected from the group of compounds that

- Aliphatic ^ or aromatic acids and preferably Carboxylic acids with 6 to 3 0 carbon atoms, preferably 10 to 22 carbon atoms,

- Amides of the above acids with ammonia, with polyfunctional amines of the polyalkylene polyamine type, with hydrazine or with aromatic amines, and

- Vegetable or animal fats 20 includes.

According to a further preferred embodiment of the invention, said agent also contains one mineral or inorganic filler.

Another preferred embodiment of the invention according to the agent is with an effective amount of an oil, a solvent, a fuel and / or optionally a surfactant

3 0 formulated so that it is meltable or sprayable and stable in storage.

According to a further embodiment of the invention, the mineral or inorganic filler optionally used is a filler selected from the group comprising talc, chalk, clay, infusor earth and similar products of this type. "■ '

0300A7 / 0856

The method according to the invention for preventing the formation of lumps in fertilizers is characterized in that that the fertilizer granules or the fertilizer granules are preferably removed at the outlet the production device either with the agent according to the invention or successively with the ester

10 of the oxyalkyl derivative, the hydrophobic compound and the mineral filler, which represent the constituents of the. Agent, enveloped, with the entire amount based on the ester and hydrophobic compound used, 0.05 to 5 kg / t, preferably 0.1 to 2 kg / t

to the mass of the fertilizer.

The fertilizer according to the invention is characterized by that the particles forming it have a coating which, with the aid of the Ver-20 according to the invention Fahrens has been formed and which consists of the agent according to the invention.

In addition to the embodiments mentioned, the invention relates to further embodiments that simultaneously are preferably used and of which in more detail below with reference to the examples, the preferred Embodiments of the teaching according to the invention represent, the talk will be.

The fertilizers against the formation of clumps according to the invention The fertilizers of the NPK type and the fertilizers are particularly effective Ammonium nitrate type fertilizers.

To treat these fertilizers one subjects the

granules or granules formed therefrom, preferably at the outlet of the manufacturing plant, a casing with at least one ester of the oxyalkyl derivative and

030047/0856 "

at least one hydrophobic compound, as defined in more detail below. These two Components used for the coating can be applied simultaneously or in succession.

The agent according to the invention is advantageously used a mineral or inorganic filler to prevent clumping.

The total amount of the ester and the hydrophobic compound, which are used according to the invention, based on the fertilizer mass, is 0.05 to 5 kg / t and preferably 0.1 to 2 kg / t.

The ratios of ester to hydrophobic compound depend on various parameters, such as the type

20 of the fertilizer to be treated, the surface condition of fertilizer particles or granules that Humidity of the fertilizer, the storage conditions and especially the humidity, the molecular weight of the ester and the type of hydrophobic compound

manure.

In practice, make up the total of esters and hydrophobic compound the proportion of the ester 15 bis 85%, preferably 30 to 70%, and the proportion "of the hydrophobic compound 85 to 15%, preferably 70 to 30% off. . ■

For example, one part by weight of the ester is used for 2 parts by weight of the hydrophobic compound for treating an NPK type fertilizer with a moisture content of 0.5% when the granules

030047/0856

this fertilizer have a good surface condition 5.

The amount of mineral filler used is from 0 to 60%, preferably from 20 to 55% based on the whole.

The entire agent consisting of the ester, the hydrophobic compound and optionally the mineral filler consists, can with oils, solvents, a fuel and / or optionally surface-active

15 means are formulated or mixed to make it

to make meltable or sprayable and storage-stable.

The preparation produced in this way comprises 90 to 100% of the agent from the ester, the hydrophobic Compound and any mineral filler used.

The ester is used as the ester of the oxyalkyl derivative or of the alkoxylated derivative

- an aromatic or aliphatic, saturated or unsaturated polyacid, preferably polycarboxylic acid, more preferably from a short or short-chain polyacid and preferably polycarboxylic acid,

3 0 and

- one condensed with water, a primary, secondary or tertiary diol or a diphenol Ethylene oxide, propylene oxide or butylene oxide, the condensate of ethylene oxide and water being preferred and wherein the molecular weight of the condensate is below 10,000 and preferably between 100 and 4,000 lies. More preferred is the molecular weight

030047/0856

of the condensate between 300 and 4000. 5

The above-mentioned polyacids or polycarboxylic acids are selected from the group consisting of adipic acid, Azelaic acid, citraconic acid, citric acid, glutaric acid, itaconic acid, pimelic acid, sebacic acid and Suberic acid, this list is not exhaustive and does not limit the invention target.

The short polyacids particularly preferred according to the invention or polycarboxylic acids are maleic acid, fumaric acid, phthalic acid, malonic acid, succinic acid and Oxalic acid, this list also not being exhaustive and the invention is also not intended to limit it.

The ester of the oxyalkyl derivative used according to the invention or the alkoxylated derivative can furthermore be an ester of an aliphatic, saturated or unsaturated Monoacid or preferably monocarboxylic acid

be off. of acetic acid, propionic acid, butyric acid, Valeric acid, caprylic acid, capric acid, pelargonic acid, lauric acid, palmitic acid, oleic acid, linoleic acid, Linolenic acid, ricinoleic acid, acrylic acid and methacrylic acid comprehensive group, including this enumeration is not exhaustive and is also not intended to limit the invention.

The hydrophobic compounds used according to the invention are selected from the group of compounds /. the

- aliphatic or aromatic acids, preferably

030047/0856

Carboxylic acids, with 6 to 30, preferably 10 to 22 carbon atoms,

- The amides of the acids mentioned with ammonia, polyfunctional Amines of the type of polyalkylenepolyamines, hydrazine and aromatic amines and

- vegetable and animal fats

includes. As aromatic or aliphatic acids, which preferably have 10 to 22 carbon atoms, you can use capric acid, undecylic acid, lauric acid, palmlatinic acid, stearic acid, oleic acid, linoleic acid, Name linolenic acid and ricinoleic acid, this list not being exhaustive and the invention not intended to restrict.

The above-mentioned polyfunctional amines are, for example, ethylenediamine, diethylenetriamine, triethylenetetramine, Tetraethylene pentamine, hexamethylene diamine and hydroxyethylethylene diamine. The said aromatic Amines are, for example, aniline and its derivatives.

Vegetable or animal fats include tallow, wax and paraffins.

The optionally in the agent according to the invention incorporated mineral filler can, for example, consist of talc, chalk, clay and infusor earth, this list, too, is not exhaustive and is not intended to restrict the invention.

For the preparation of the above-mentioned esters of the oxyalkyl-3 5 derivatives can be used

- either react the acid with the oxyalkyl derivative in the presence of a catalyst, whereby the ge

030047/0856

- 14 -.

water formed is removed by distillation and / or optionally by azeotropic distillation _r

- or react the anhydride of the acid with the oxyalkyl derivative.

In the latter case, the acid formed reacts with the remaining alcohol residues with elimination of Water, so that the ester obtained contains neither free acid nor free oxyalkyl derivative.

The preferred esters mentioned above, which are obtained by reacting a diacid with a polyethylene glycol, have molecular weights which depend on the ratio R between the number of molecules of the diacid and the number of molecules of the polyethylene glycol depend, the molecular weight being a consequence of the ongoing polymerization approaches infinity when this ratio assumes the value 1. This relationship can be between 0.5 and 1, with particularly effective compounds at ratios from 0.5 to 0.8 receives.

In particular, one can for the preparation of an ester of the type in question, which has a ratio of 0.5, using an apparatus with. a stirrer, a thermometer and a vacuum distillation system, 1 mol of an acid anhydride, 2 mol of an oxyalkylated dialcohol and 0.01 mol of p-toluenesulfonic acid as a catalyst to react. The reaction medium is heated to 120 to 130 ^° C., working in a vacuum of 6.7 mbar (5 mm Hg) in order to remove the water formed in the course of the reaction. In order to facilitate the removal of this water, one can also use a volatile solvent which, with water, forms an az-eotropic

030047/0858

Mixture forms.
5

The reaction time used varies from 2 to 6 hours depending on the molecular weight the dialcohol used.

After completion of the reaction, which is carried out by thin-layer chromatography can follow the reaction medium depending on the melting point of the obtained Polyester either cooled or poured out while still warm.

The thin-layer chromatographic analysis must show the absence of dialcohol. If still Dialcohol is present, an additional amount of the catalyst is added and heating continues until to the disappearance of dialcohol.

Depending on their molecular weight, the products obtained are in the form of viscous liquids, pasty masses or friable solids.

For the production of esters with other proportions of the components, which are between 0.5 and 1, one works in the same way, apart from the proportions in which the starting materials are used begins.

To clarify the above general explanations, a numerical example of the Her-35 is given below position of one of the esters in question, namely a polyethylene glycol maleate, its ratio from number of moles of diacid to number of moles of polyethylene

030047/0856

glycol is 0.66.
5

For the preparation of this compound is charged, the reaction apparatus described above with 180 parts by weight of a light gasoline having a boiling point of 80 ⁰ C, which forms with water an azeotropic mixture, 905 parts by weight of polyethylene glycol having a molecular weight of 600, 99 parts by weight maleic anhydride and 14 parts by weight sulfuric acid as Versterungskatalysator. The mixture was heated to reflux and distilled azeotropic mixture of gasoline and water at about 80 ⁰ C from.

The gasoline is recycled and the distillation continues until 18 parts of water are obtained has collected, which takes about 6 hours, which indicates the end of the reaction.

The light naphtha is then stripped, without the temperature exceeding in the resultant mass 100 ⁰ C.

This mass is in the form of a medium viscosity oil that can be easily poured at this temperature can. They can either be used as such in the process according to the invention, or they can use them for the production of the agent 0 according to the invention against the formation of lumps. .

In the former case it is either in the molten state or in the form of a dispersion in a solvent onto the fertilizer granules sprayed _s exiting the apparatus used in their manufacture to give this treatment preference

030 047/0856

wisely caused before the application of the hydrophobic compound, in the case of this ester and with regard to the fertilizers for which it is particularly suitable, i.e. the fertilizers of the
NPK type and ammonium nitrate type, preferably a fatty acid and in particular stearic acid.

In the second case, that is, used to form a useful anti-clumping agent the ester as it comes from the manufacturing

tion emerges, that is, one carries in 1000 parts

of the hot oil 2000 parts of a previously melted hydrophobic compound, for example commercially available, technical stearic acid. The mixture is then homogenized for 15 minutes and then

0 poured onto a cylinder cooled ^{to 5 ° C.} The resulting plates with a thickness of 3 to 10 mm are then crushed into flakes in order to form particles, the largest dimension of which is 1 to 2 mm
to 2 to 3 mm.

In this case, no mineral filler is provided.

According to a further embodiment, this is replaced 30 polyethylene glycol with a molecular weight of 600 by a polyethylene glycol with a molecular weight from 1500. One works in the same reaction device, in this case in the presence of 180 parts by weight of the above gasoline 35 works, but 42 parts by weight of maleic anhydride and 8 parts by weight of heavyelic acid to 958 parts by weight

Q30047 / 0856

parts of polyethylene glycol with a molecular weight von 1500 (PEG 1500) used. The reaction is complete after 7.7 parts by weight have been obtained by distillation Has removed water, which is achieved after about 6 hours.

1000 parts by weight of the ester are obtained, which is in the Heat is in the form of an oil.

The agent according to the invention against the formation of lumps is prepared by introducing 2000 parts by weight of previously melted stearic acid and 1500 parts by weight of talc into this oil. Homogenizing the mixture for 15 minutes at 100 ⁰ C and poured in the present form of a homogeneous, fluid dispersion composition on a cooled cylinder, the door temperature is 5 ⁰ C. The layer obtained in this way is comminuted with a thickness of 3 to 10 mm to form flakes, the largest dimension of which is between 1 and 3 mm.

The product obtained in this manner in the form von.Schuppen can be used as such by aufstreut it to the fertilizer, which emerges from its manufacturing apparatus and its granules have a temperature of at least 85 ⁰ C. The flakes then melt on the granules and surround them in the form of a protective layer that prevents them from forming lumps.

It is still possible to spray the product in the form of flakes after using it in particular diluents, such as heavy fuel oil or mineral oils, which may be surface-active

030047/0856

Contained funds, has added. The spraying then takes place at a temperature of 6 0 to 8 0 ⁰ C.

For storage can be agents of the invention against the formation of lumps to preparations in a heavy fuel oil or a mineral oil, the dispersing agent for organic media, such as polycarboxylic acid, zinc naphthenate, which is optionally combined with Calciumalkylarylsulfonaten, and _/ containing alkyd resins, process.

As a numerical example, an advantageous preparation based on the agent mentioned may be mentioned, which contains polyethylene glycol with a molecular weight of 600 (PEG 600). As in the example above prepare a mixture of 200 parts of the maleate

20 of PEG 600, 400 parts of stearic acid, 300 parts

Talc and 5 parts of zinc naphthenate. The mixture is homogenized for 15 minutes at 100 ^° C., cooled and processed into flakes in the manner described above.

The flakes obtained in this way can be heat-dispersed in a heavy fuel oil or an oil to obtain a dispersion which is stable and can be easily atomized.

As already indicated, according to the invention, various Treat types of fertilizers, especially the NPK type fertilizers and the ammonium nitrate fertilizers.

The following are a number of examples in view

030047/0856
BATH ORIGINAL

on beneficial means as well as those with certain Fertilizer types given results obtained.

In these examples the fertilizers are identified by three digits for the constituent NPK, for example by the sequence of digits 17-17-17 or three times 17. It should be remembered that the values in the order given for the nitrogen content as a percentage ^ of the nitrogen, represent the phosphorus content as a percentage of phosphoric anhydride (P ₂ Oc-) and the potassium content, expressed as a percentage of potassium oxide (K ₂ O). These fertilizers, also known as fertilizer complexes, may contain traces of trace elements.

In the case of ammonium nitrate fertilizers, they are identified by their nitrogen content, which is called percentage nitrogen content, based on the fertilizer, is given.

With regard to the method according to the invention The results obtained with the agent according to the invention can be derived from the behavior of the treated fertilizers read off which behavior can be assessed with the help of two examination methods.

30 The first of these investigation methods is based on a compaction investigation and gives the degree of mass increase of the sample (dalsT). To carry out this For examination, a sample of the treated fertilizer is brought into a cylindrical shape with a diameter

35 by 3.5 cm and a height of 5 cm. Then you practice on the treated granules with the help of a piston, the diameter of which is slightly smaller than that of the cylinder

030047/0856

or, to avoid friction, a pressure of 0.981 bar (1 kg / cm ² ). The samples formed in this way and kept under a pressure of 0.981 bar (1 kg / cm ² ) are placed in a container in which various temperature and humidity conditions can be maintained. The investigation shows that a treatment period of 4 to 5 days is sufficient to evaluate the samples.

After this time has elapsed, the metal cylinder is opened at its circumference and the breaking strength is determined of the fertilizer block in a pressure measuring device (dynamometer). When the sample is taken disintegrates from the mold, this corresponds to an excellent action of the agent against the formation of lumps. In general, the lower the effect against lump formation, the greater the effect Breakage of the samples is the value read on the pressure gauge.

The degree of mass increase of the sample is expressed as a percentage ratio of the fractional value of the examined Sample determined at the fractional value of the control sample.

The second test is the so-called sagging test. For this examination, 10 kg of the treated-0 are stored th fertilizer in a pressure-resistant polyethylene bag. The sack is weighed down for 2 months twenty times its weight. Then you open the sack and examine the sample against one untreated control sample.

In each sack, the lumps of the agglomerated are weighed

030047/0856

Granules and determines the degree of lump formation via the ratio of the weight of the lumps of the examined Sample to the weight of the lump of the untreated Control sample. One can also subjectively rate the hardness of the lumps.

The result of anti-clumping The lower this percentage, the better the treatment.

A wide variety of illustrative examples of the invention have been made based on these research methods Examples carried out.

For each example the following is given:

- regarding the composition of the funds, the relationship between the two the various constituents and in particular the ratio R of the ester;

- with regard to the application of the remedy to the Fertilizers, the type of treatment selected and the Temperature conditions;

- with regard to the fertilizer, the type and formulation of the fertilizer and its moisture content;
and

- with regard to the behavior of the treated fertilizers, the results obtained from the compaction study, the percentage of lump formation and the results obtained in the sagging test.

These details are for all examples in the following Table compiled. .. ·. "-

030047/0856

Tabel

O CaJ O O -O

-Ν » O OO en

at Together Tempe Damp I. 0.37 Tempe Kind of Be Amount of ester Amount of Amount of Minera Ver Clump A I. spat settlement rature tig rature plot (Weight o / oo) hydrophobic Solution with lischer you- pen- bag No. of of speed the and ratio R link tel filler management bil- test Manure Manure of On- (based on (Weight o / oo, (Weight o / oo (Weight o / o test manure (Loading by means of with Manure inertial the amount of based on related to: based (Dan) (%) obedient tel with loading Fertilizer) the crowd the crowd on the to do- (° C) tel 0.37 hand- of manure of manure Mass of gene) (%) lung by means of) by means of) Manure (° C) by means of 15-15-15 60 80 spray 0.2 o / oo 0.2 o / oo D, 15 o / oo 0.5 o / oo 7.2 16 1 Polyester phtha- Stearic acid [solution with talc 0.37 lat re tel + PEG 400 (0.5) D, 5 o / oo Heavy 0.37 edible oil 2 Il 60 80 If 0.2 o / oo poly 0.2 o / oo 3.1 o / oo lo 0.35 o / oo 8.1 18th estermaleat stearin solvent talc 0.6 PEG 600 (0.5) acid + 0.7 o / oo Heavy Heating oil 3 η 60 80 Il 0.3 o / oo poly 0.3 o / oo . o / oo 0 5 11 estermaleat stearin Heavy PEG 600 (0.66) acid Heating oil 4th untreated 46 100 delte con troll test 5 17-17-17 60 80 spray 0.156 o / oo poly 0.333 o / oo . o / oo 0 3.5 11 estermaleat stearin Heavy PEG 1600 (0.66) acid Heating oil

J J

CD

OO OO

at Together • Tempe Damp Tempe Kind of Be Tabel Amount of Amount of Minera Ver Clump I.
N) A game settlement rature tig rature plot (Continuation) hydrophobic Solution with lischer you- pen- I. bag No. of of speed the Amount of ester link tel filler management bil- test Manure " Manure of On- (Weight o / oo) (Weight o / oo, (Weight o / oo, (Weight o / oc test manure (Loading by means of with Manure inertial and ratio R based on based on based (Dan) (%) obedient tel with loading (based on the crowd the crowd on the to do- (° C) tel hand- the amount of of manure of manure Mass of gene) (%) lung Fertilizer) by means of) by means of) Manure (° C) by means of 6th 17-17-17 60 0.6 80 spray 0.333 o / oo 1 o / oo stearin Heavy 0 3.9 13th 0.166 polyester acid Heating oil ο maleate CO 7th Il 60 0.6 80. Il PEG 600 (0.66) 0.4 o / oo 1 o / oo 3.3 o / oo 3.0 10 O stearin Heavy talc O 0.2 o / oo poly acid Heating oil 8th H 60 0.6 ■ 'so Il estermaleat 0.266 o / oo 1 o / oo D, 2 o / oo 5 16 PEG 1500 (0.66) stearin Heavy talc O
OO 0.133 o / oo poly acid Heating oil OI 9 Il 60 0.6 80 Il estermaleat, 0.3 o / oo 1 o / oo 0 4 ' 13th O) PEG 600 (0.66) Octadecyl Heavy 0.3 o / oo poly amine Heating oil 1.0 (I. 0.6 untreated estermaleat 31 100 delte- PEG 1500 (0> 66), troll test U 15-15-, 15 60 0 _r 52 80 spray 0.4 o / oo o / oo 0 1.4 8th rie hydrogenated Heavy selfä 0.2 o / oo poly tallow heating oil hig estermaleat PEG §00 (0.66)

Tabel

(Continuation)

to σ CD

co cn CD

At- Together Tempe Damp Tempe Kind of Be Amount of ester Amount of Amount of Minera Ver Clump A Spie; settlement rature tig rature plot (Weight o / oo) hydrophobic Solution with lischer you- pen- bag No. of of speed the and ratio R link tel filler management bil- test Manure Manure of On- (drawn on (Weight o / oo, (Weight o / oo, (Weight o / oc test manure (Loading by means of with Manure inertial the amount of based on based on based (Dan) (%) obedient tel with loading Fertilizers) the crowd the crowd on the to do- (° C) tel hand- of manure of manure Mass of gene) (%) lung by means of) by means of) Manure (° C) by means of 12th 15-15-15 60 0.52 80 spray 0.166 o / oo poly 0.333 o / oo 1 o / oo 0 1.6 9 trickle estermaleat hydrogenated Heavy able to PEC 600 (0.66) tallow Heating oil 13th Il 60 0.52 80 M. 0.2 o / oo poly 0.3 o / oo 1 o / oo 0 2.1 12th Il estermaleat Stearylamide Heavy PEG 600 (0.66) from diethy Heating oil lentriamine 14th Il 60 0.52 80 Il 0.2 o / oo poly 0.25 o / oo 1 o / oo 0 1.8 10 It estermaleat Stearylamide Heavy PEG 600 (0.66) from diethy Heating oil lentriamine 15th 0.52 untreated 17.8 100 90% delte con Klum troll test pen, hard 16 17-17-17 110 0.47 Wrapping 0.2 o / oo poly 0.2 o / oo 0 0.5 o / oo 2 7th trickle estermaleat Stearic acid talc : uh PEG 600 (0.66)

ι CJt

-CO O

OO OO

Table (continued)

σ oo cn

at Together Tempe Damp Tempe Kind of Be Amount of ester Amount of Amount of Minera Ver Klurn- l ·.,
A game settlement rature ¹ tig rature plot (Wt. 'O / oo) hydrophobic Solution with lischer you pen- bag No. of of speed the and ratio R link tel filler tion s- bil- test Manure Manure of On- (based on (Weight o / oo, (Weight o / oo, (W / o / oG test manure (Loading by means of with Manure inertial the amount of based on based on based (Dan) (%) obedient tel with loading Fertilizer) the crowd the crowd on the to do- (° C) tel hand- of manure of manure Mass of gene) (%) lung by means of) by means of) Manure (° C) by means of 17th 17-17 ^ 17 110 0.47 Wrapping 0.2 o / oo Pöly 0.2 o / oo 0 0.35 o / oo 1.9 7th trickle e ste rphthalate Stearic acid talc able to PEG 400 (0.5) 18th Il 110 .0.47 If 0.2 ό / οο poly- 0.3 o / oo 0 0 3.1 11 Il estermaleat Stearic acid PEG 600 (0.66) 19th Il 110 0.47 .. 0.3 o / oo poly 0.4 o / oo 0 0.30 o / oo 2.2 8th Il estermäleat stearin talc PEG 1500 (0.66) acid 20th Il 110 0.47 Il 0.15 o / öö poly- 0.375 o / oo 0 0 4.1 15th Il estermaleat paraffin PEG 15Ö0 (0.66) wax + 0.075 o / oo stearin acid 21 M. 0.47 unhandled 27.2 100 100% delte con Klum troll test pen, hard

Tabel

Together Tempe Damp Tempe Kind of Be (Continuation) Amount of Amount of Minera Ver Klum I. ) at settlement rature tig rature plot Amount of ester hydrophobic Solution with lischer you pen- A trickle. spat; of of speed the (Weight o / oo) link tel filler tung s bil- bag able to No. Manure Manure of On- and ratio R (Weight o / oo (Weight o / oo (Weight o / o test manure test but by means of with Manure inertial (based on based on related to based (Dan) (%) (Loading ver tel with loading the amount of the crowd. the crowd on the whether- seals (° C) tel hand- Fertilizer) of manure of manure Mass of to do- 00% (%) lung by means of) by means of) Manure gene) Klum (° C) by means of pen 17-17-17 60 0.71 .. 80 spray 0.3 o / oo 1 o / oo 0 1.7 8.5 22nd 0.3 o / oo poly stearin Heavy trickle estermaleat acid Heating oil able to Polyethylene glycol II 60 0.71 80 ti col 600 (0.5) 0.2 o / oo 1 o / oo 0 3.6 13th 23 0.4 o / oo poly stearin Heavy It estermaleat acid Heating oil Polyethylene Il 60 0.71 80 It glycol 600 (0.5) 0.3 ö / oo 1 o / oo 0 4.1 20th 24 0.3 o / oo poly Octadecyl Heavy estermaleat amine Heating oil Polyethylene glycol col 600 (0.5) M. 0.71 untreated 0 0 20th 100 25th te control 0 sample 17-17-17 60 0.75 80 spray 0.2 o / oo . o / oo 0 -6.2 15.5 26th 0.4 o / oo poly stearin Heavy ester succinate acid Heating oil PEG 600 (0.5)

Tabel

28 - at Together Π Tempe Damp Tempe t 80 Kind of Be Amount of ester Amount of Amount of Minera 0 0 0 Ver Klum A game settlement rature tig rature plot (Weight o / oo) hydrophobic Solution with lischer you- pen ^ bag No. of of speed the and ratio R link tel filler management bil test Manure Il Manure of On- . 80 (based on (Weight o / oo, (Weight o / oo, (Weight o / oc test manure (Loading by means of with Manure inertial the amount of based on based on based (Dan) (%) obedient tel with loading Fertilizer) the crowd the crowd on the to do- .17-17-17 (° C) tel hand- 80 of manure of manure Mass of gene) (%) lung by means of) by means of) Manure (° C) by means of 27 17-17-17 ii 60 0.75 80 spray 0.4 o / oo poly 0.2 o / oo 1 o / oo 0 3.5 8th * ester phthalate stearin Heavy PEG 600 (0.5) acid Heating oil 28 11 60 0.75 80 11 0.4 o / oo poly 0.2 o / oo 1 o / oo 0 3.6 8th ester adipate stearin Heavy PEG 600 (0.5) acid Heating oil 29 0.75 untreated 45 100 te control sample 30th 60 0.5 spray 0.4 o / oo poly 0.2 o / oo 1 o / oo 6.8 34 trickle estermalonate stearin Heavy able to PEG 600 (0.5) acid Heating oil 31 60 ■ 0.5 11 0.3 o / oo poly 0.3 o / oo 1 o / oo 2.6 10 Il estermalonate stearin Heavy PEG 600 (0.5) acid Heating oil 32 60 0.5 11 0.2 o / oo poly 0.4 o / oo 1 o / oo 3 11.5 I. estermalonate stearin Heavy PEG 600 (0.5) acid Heating oil

Tabel

Together Tempe Damp Tempe _r 80 Kind of Be (Continuation) Amount of Amount of Minera Ver Clump 29 - at settlement rature tig rature plot Amount of ester hydrophobic Solution with lischer you- pen- A game of of speed the (Weight o / oo) link tel filler management bil- bag No. Manure Fertilizer of on 80 and ratio R (Weight o / oo, (Weight o / oo (Weight o / oc test manure test by means of with'- Manure carrying (based on based on based on based (Dan) (%) (Loading tel with be the amount of the crowd the crowd on the obedient (° C) tel hand 80 Fertilizer) of manure of manure Mass of to do- (%) lung by means of) by means of) Manure gene) (° C) by means of 17-17-17 60 0.5 80 spray 0.3 o / oo 1 o / oo 0 5.2 20th 33 0.3 o / oo poly Octadecyl Heavy rie estermaleat amine Heating oil selfä PEG 600 (0.5) hig but ver 0.5 untreated 26th 100 density V 34 delte con 100% troll test Lump 17-17-17 60 0.64 spray 0.2 o / oo 1 o / oo 0 6th 20th hard 35 0.4 o / oo poly stearin Heavy estermaleat acid Heating oil ti 60 0.64 Il PEG 600 (0.66) 0.3 o / oo 1 o / oo 0 4th 13th 36 0.3 o / oo poly stearin Heavy estermaleat acid Heating oil Il 60 0.64 H PEG 600 (0.66) 0.4 o / oo o / oo 0 2.2 7th 37 0.2 o / oo poly stearin heavy estermaleat acid leizöl 11 0.64 untreated PEG 600 (0.66) 30.2 100 38 te control sample

Tabel
(Continuation)

O CaJ O CD

O CO cn sr »

at
game
No. Together
settlement
of
Manure
by means of Tempe
rature
of
Manure
with
tel
(° C) Damp
tig
speed
of
Manure
with
tel
(%) Tempe
rature
the
On-
inertial
loading
hand-
lung
(° c) Kind of Be
plot Amount of ester
(Weight o / oo)
and ratio R
(based on
the amount of
Fertilizer) Amount of
hydrophobic
link
(Weight o / oo,
based on
the crowd
of manure
by means of) Amount of
Solution with
tel
(Weight o / oo,
based on
the crowd
of manure
by means of) Minera
lischer
filler
(Weight o / oc
based
on the
Mass of
Manure
by means of 0 Ver
you
tion s-
test
(Dan) Clump
pen-
bil-
manure
(%) A
bag
test
(Loading
whether-
to do-
gene) I. 39 ammonium
nitrate
3.9%
nitrogen 25th 0.15 90 spray 0.2 o / oo poly
estermaleat
PEG 600 (0.66) 0.4 o / oo
stearin
acid 0 0 0 0.5 3 40 Il 25th 0.15 80 spray 0.166 o / oo poly
estermaleat
PEG 1500 (0.66) 0.333 o / oo
stearin
acid 0 0 1.4 9 41 Il 25th
25th 0.15 untreated
te Kohtroll
prdbe 15.8 100 42 ammonium
nitrate
26th%.
nitrogen 25th 0.5, 80 spray 0.2 o / oo poly
estermaleat
PEG 600 (0.66) 0.4 o / oo
stearin
acid 1 o / oo
Heavy
Heating oil 3.5 12, < 43 Il 0.5
0.5 spray
untreated
te control
sample 0.2 o / oo poly
estermaleat
PEG 1500 (0.66) 0.4 o / ob
stearin
acid 1 o / oo
Heavy
Heating oil 3.1 11 44 Il 28.2 100

oo

From the table above it can be seen that the inventive Means and the claimed method have considerable advantages, in particular Provide fertilizers that do not clump or destroy the granules or granules and tend to form dust.

0300A7 / 0856

Claims (17)

Patent attorneys Dipl.-Ing. H. ^ eickmann, Dipl.-Phys. Dr. K. Ftncke Dipl.-Ing. F. A. Weickmann, Dipl.-Chem. B. Huber Dr. Ing.H. LisKA 3017878 8000 MUNICH 86, DEN '"^; . - ;.' ■ PO Box 860 820 MÖHLSTRASSE 22, CALL NUMBER 98 39 21/22 HtM / ei Case: 0192 80 05 COMPAGNIE FRANCAISE DE PRODÜITS INDUSTRIELS 28, Boulevard Camelinat 92233 Gennevilliers, France Agent against the formation of lumps in fertilizers and its use PATENT CLAIMS Agent against the formation of lumps in fertilizers, characterized in that there is at least contains an ester of an oxyalkyl derivative and at least one hydrophobic compound, the ester of the Oxyalkyl derivative one - an aromatic or aliphatic, saturated or unsaturated polyacid, preferably a short poly- Q30047 / 0858 acid, and.
- one with water, a primary, secondary. or a tertiary diol or a diphenol condensed Ethylene oxide, propylene oxide or butylene oxide, preferably a condensate of water and ethylene oxide, the molecular weight of the condensate being below 10,000 and preferably between 100 and 4000 lies, is. 2. Agent against the formation of lumps in fertilizers, thereby marked z. eich η et that it contains at least one ester of an oxyalkyl derivative and at least one hydrophobic compound, the ester of the oxyalkyl derivative being the one - an aliphatic, saturated or unsaturated monoacid and - an ethylene oxide, propylene oxide or butylene oxide condensed with water, a primary, secondary or tertiary diol or a diphenol, preferably a condensate of water and ethylene oxide, the molecular weight of the condensate being below 10,000 and preferably between 100 and 4,000,
is. 3. Means according to one of claims 1 or 2, characterized in that the Molecular weight of the condensate between 300 and. 4000 lies. '- - 4. Means according to one of claims 1 to 3, »characterized in that it contains a mineral filler. 030047/0856 5. Agent according to one of claims 1 to 4, d a characterized in that it by formulating with an effective amount of an oil, a solvent, a fuel and / or optionally a surfactant has been made meltable or sprayable and storage-stable. 6. Agent according to one of claims 1 to 5, d a d-urch characterized in that the hydrophobic compound selected from the group 15 is that - aliphatic or aromatic acids with 6 to 30, preferably 10 to 22 carbon atoms, - the amides of the acids mentioned with ammonia, polyfunctional amines of the polyalkylene type 2 0 polyamines, hydrazine and aromatic amines and - includes vegetable or animal fats. 7. Agent according to one of claims 4 to 6, d a 25, characterized in that it contains, as mineral filler, a filler selected from the group consisting of talc, Chalk, clay, infusor earth and the like. 8. Agent according to one of claims 1 to 7, characterized in that the Combination of the ester and the hydrophobic compound and the ester in an amount of 15 to 85% preferably from 30 to 70% and the hydrophobic compound in an amount from 85 to 15% and preferably contains from 70 to 30%. 9. Agent according to one of claims 4 to 8, there- 030047/0856 characterized by that it is based on the mineral filler in an amount of from 0 to 60%, preferably from 20 to 55% on the combination ,, contains. 10. Agent according to one of claims 1 and 3, d a through marked that the polyacids from adipic acid, azelaic acid, citraconic acid, citric acid, glutaric acid, itaconic acid, Pimelic acid, sebacic acid and suberic acid are selected. 15th 11. Agent according to one of claims 1 and 3, characterized in that the short polyacids from maleic acid, fumaric acid, phthalic acid, malonic acid, succinic acid and Oxalic acid comprehensive group are selected. 12. Means according to one of claims 2 and 3, characterized in that the aliphatic, saturated or unsaturated mono - 25 acid from acetic acid, propionic acid, butyric acid, valeric acid, caprylic acid, capric acid, pelargonic acid, Lauric acid, palmitic acid, oleic acid, linoleic acid, linolenic acid, ricinoleic acid, and acrylic acid Methacrylic acid comprehensive group is selected. . 13. Means according to claim 6, "'characterized that the aromatic or aliphatic acids having 10 to 22 carbon atoms are selected from the group consisting of capric acid, undecylic acid, lauric acid, palmitic acid, Stearic acid, oleic acid, linoleic acid, linolenic acid, ricinoleic acid that includes the polyfunctional Amines from the ethylenediamine, diethylenetriamine, TrI- 030047/0856 ethylene tetramine, tetraethylene pentamine, hexamethylene-5 diamine and hydroxyethyl ethylenediamine are selected, that the aromatic amines include aniline and its derivatives and that the vegetable and animal fats include tallow, waxes and paraffins.
10 14. Agent according to one of claims 1 to 13, characterized in that it as a hydrophobic compound stearic acid, as an ester of the oxyalkyl derivative a representative of 15 group, the polyester phthalate PEG 40 0, polyester maleate PEG 600, polyester maleate PEG 1500, polyester succinate PEG 600, polyester phthalate PEG 600, Polyester adipate PEG 600 and polyester salonate PEG 600 includes, and optionally talc as a mineral see contains filler. 15. Method of preventing clumping in Fertilizers, characterized in that the fertilizer grain 25 surfaces, preferably when leaving the manufacturing device, enveloped with an agent according to claims 1 to 14. 16. Method of Preventing Lump Formation in Fertilizers, characterized in that the fertilizer granules, preferably on leaving the production device, sequentially or simultaneously with the components of an agent according to a 35 of claims 1 to 14, wherein the total amount of the ester and the hydrophobic compound 0.05 to 5 kg / t, preferably 0.1 to 2 kg / t, 030047/0856 attracted to the bulk of the fertilizer, amounts to. 17. Fertilizers, characterized in that that the particles forming it have a coating which, with the aid of a process has been formed according to claims 15 or 16 and from a means according to a of claims 1 to 14 exists. 030047/0856