DE1442857B - - Google Patents

Description

with an emulsifier and the effort required to evaporate the large amounts of water is very large and makes the process almost uneconomical.

Another method of making non-clumping salts, especially potassium chloride, describes the French patent specification 967 265. This method is intended to dry the centrifuged No need for salt, which was previously placed under watery salt porridge with the active ingredient against caking (Amine acetate) is added. So a treated salt is obtained, which today with 2 to 3 ° / o water content represents a reduced value of the goods, a circumstance which is precisely due to a downstream Drying cannot be helped, because according to this patent it is precisely this drying causes the salt crystals to grow back together.

Under these circumstances, the aim of the present invention is to be particularly economical Conditions a mixture of fatty acids and fatty amines as an anti-caking agent with the best effectiveness receive. The new anti-caking agents are also practically non-allergic and are more general Field of use.

The inventive method for the production of free-flowing fertilizers by adding a Mixture of fatty acids and fatty amines is characterized in that a mixture with a stoichiometric Excess of fatty acids is used. The new mixture thus shows besides the bound Part of free fatty acid, which promotes the anti-caking effect of the cationic and anionic components.

This increased anti-caking effect is not achieved with the known addition of a stoichiometric one Mixture of fatty acids and fatty amines.

The fatty acids or fatty amines used advantageously have a hydrocarbon radical from 8 to 22, in particular from 12 to 18 carbon atoms.

According to a further advantageous embodiment of the method according to the invention, the mixture is in molten state applied to the fertilizers. The chemical formula of anti-caking agents according to the invention reads as follows:

Rn · COOH, Rp NH ₂ + χ Rn COOH

45 attempt 1

1 part of the aforementioned fatty amine is melted with 3 parts also melted Saponification stearic acid mixed, which is composed as follows:

Lauric acid 2.4%

Myristic acid 1.4 ° / ₀

Palmitic 51.6 ° / ₀

Palmitooleinsäure 2.7 ° / ₀

Stearic acid 41.8%

In 360 g of mixture there are thus 90 g or 0.346 mol of amine and 270 g or 1.164 mol of saponification stearin, which means a stoichiometric excess of acid of 236 ° / ₀ , based on the amine.

Attempt 2

1 part of the aforementioned fatty amine is in a molten state with 3 parts of a fatty acid or a mixture of recuperation or circulating fatty acids mixed, consisting, for. B. from:

Neutral bodies (not saponified fats) 10 ° / ₀

Stearic acid and palmitic acid 30 ° / ₀

Oleic acid 59%

Impurities (including H ₂ O) 1% / ₀

In 360 g of mixture there are thus 90 g or 0.346 mol of amine and 270 g or 0.864 mol of circulating fatty acid, which means a stoichiometric excess of acid of 150 ° / ₀ , based on the amine.

Salt samples according to the invention were prepared with the reaction products of Experiments 1 and 2. The following were also produced as comparative tests:

Attempt 3

KCl treated with the fatty acid defined in Experiment 1 alone.

Attempt 4

where χ represents a positive number between 1 KCl treated alone with that under experiment 2

and 3, preferably 2, and Rn and Rp defined fatty acids.

Radicals with 8 to 22 carbon atoms, advantageous

Probably 12 to 18, with the part of experiment 5

Rn • COOH, Rp NH ₂

of the formula the chemical composition of the anti-agglomerating fatty amines and fatty acids represents.

For the preparation of the anti-caking agents according to the invention you can, for. B. natural, animal or use vegetable fatty acids, e.g. B. fatty acids from tallow, palm trees or palm oil, soy, copra and the like, also suitable synthetic fatty acids.

For the preparation of free-flowing potassium chloride attempts have been made with two mixtures of fatty acids and fatty amines whose fatty amine component consisting essentially of a mixture of 30 ° / o palmitylamine, is 30 ° / ₀ stearylamine and 40 ° / ₀ oleylamine.

KCl treated with the fatty amine from experiments 1 and 2 alone.

Trial 6
KCl untreated, as a calibration test.

The amount of added anti-caking agent was in all tests 0.36 ° / _00th

The salt samples treated as indicated and the untreated salt caused caking subject to effecting conditions. The samples were then examined and the degrees achieved in the maintenance of flowability. The average results of several such test series are compiled in the following table:

attempt

KCl + 0.36% ₀ KCl + 0.36 ° / ₀₀ KCl + 0.36 ° / ₀₀ KCl + 0.36% ₀ KCl + 0.36 ° / ₀₀ KCl a mixture a mixture fatty acid ■ fatty acid · ^! Fatty amine untreated of 3 parts of 3 parts ·· ■ '.' fatty acid fatty acid + 1 part + 1 part Fatty amine Fatty amine

100%

Achieved degree of effectiveness in preventing caking 96% I 92.6% j 85.2% | 100%

0%

free flowing

fluent under
a thin one
Surface hardening

Properties of the salt after trial

fluent under
a fixed one
Surface layer slightly baked together

free flowing

completely caked

The table shows that the two anti-caking agents according to the invention (experiments 1 and 2) are the same or have approximately the same effectiveness as the best of the known agents (experiment 5), this but with significantly improved economic efficiency.

Trial 7 and 8

In experiments 7 and 8, an anti-caking agent mixture is used, the amount of amine in which is the same as in corresponds to tests 1 and 2 used, d. H. 90 g or 0.346 mol for 1000 kg KCl. The acid content however, based on the amine, it is stoichiometric, i.e. 0.346MoI per 1000 kg KCl. This matches with 80.2 g of saponification stearic acid in experiment 7 and 108 g of circulating fatty acid in experiment 8. The corresponding Quantities in experiments 1 and 2 are each 270 g.

The degree of effectiveness achieved in the prevention of caking is in Experiment 1, 100%, 80.2% in Run 7, in experiment 2 96 ° / ₀ and 80% of attempts. While the product in experiments 1 and 2 is free-flowing or flowing with a thin surface hardening, in experiments 7 and 8 a slight agglomeration is observed.

This shows that with the same proportions of amine, the anti-caking effect and flowability are inadequate adjusts when the acid content is only stoichiometric, and that satisfactory properties can only be achieved with large excess of stoichiometric acid content.

In a second series of tests with a KCl with a different structure, the following were comparatively determined:

a) KCl + 0.36 ° / ₀₀ fatty acid of tallow (alone), anti-caking effect: 31.3 ° / _0th

b) KCl + 0.36 ° / ₀₀ fatty amine from tallow (alone), anti-caking effect: 63.5 ⁰ J ₀ .

c) KCl + 0.36 ° / ₀₀ of a mixture of 3 parts of fatty acid of tallow fatty amine with 1 part of tallow, anticaking effect: 98.1%.

In a third series of experiments, with a salt. (KCl) still another structure, and the same amount added (0.36% o) it was found:

a) KCl + fatty acid alone,
Anti-caking effect: 54.4%.

b) KCl + fatty amine alone,
Anti-caking effect: 65.4%.

c) KCl + mixture of 41
1 part fatty amine,
Anti-caking effect: 71.1%.

4 parts of fatty acid and

Claims (3)

1 2 applied products, cationic fatty amines in particular have been emphasized, agents which are very effective but also very expensive and which have the disadvantage of being physiologically allergic up to a certain point. There is also the use of anionic fatty 1. Process for the production of free-flowing acids known, which are much cheaper, but also a lot of fertilizers, especially free-flowing ones, are less effective than the fatty amines.
Potassium chloride, by adding a mixture. The German patent specification 1018 436 describes fatty acids and fatty amines, thereby io a process which consists in the fact that a mixture with baking to be protected, dry, fine-grained fertilizer, a stoichiometric excess of fatty acids means with moist Potash salt is used with the addition of a. Flotation agent, e.g. B. fatty amines, such as stearylamine, 2. The method according to claim 1, characterized in that palmitylamine, oleylamine or mixtures thereof in indicates that the fatty acids used should be mixed in amounts of 0.002 to 0.015%. This or fatty amines a hydrocarbon residue of process has the disadvantage that dry fertilizer-8 to 22, in particular from 12 to 18 carbon middle component and thus the mixture with have atoms. To load water. It also requires a 3. The method according to claim 1 and 2, characterized in additional mixing operation with their costs, wherein characterized in that the mixture in molten 20 remains at the discretion of the user, among the zenem state applied to the fertilizers different flotation agents the appropriate one is extracted, to choose. A similar procedure is already followed according to German patent specification 1 012 931, in which the production 25 non-baking fertilizers by mixing moist, flotation and still fertilizers with residues of flotation agents such as aliphatic Fettaminen, contaminated potash salt with rock phosphate is described. The fatty amines, however, that too 30 according to the aforementioned German patent specification 1 018 436 as an active ingredient for the production of non-baking Fertilizers can be used, are practically only slightly or not at all water-soluble. Their use in solution therefore requires either a The invention relates to a method for producing 35 extremely uneconomically high dilution or the provision of free-flowing fertilizers, in particular with the aid of dissolving neutralizing acids, their particular of free flowing potassium chloride, is not indifferent to choice; with the usual addition a mixture of fatty acids and fat consumption of hydrochloric or acetic acid is completely ineffective amines. and therefore making substances more expensive to use The handling of fertilizer salts is appropriate. known to be uncomfortable because the individual salt crystals. Procedures limited by the effects of pressure and changes in the action of ammonium chloride atmospheric conditions (humidity and according to German Patent 1 004 152, in which temperature) and the resulting active ingredients octadecylamine hydrochloride or octa alternately on the surface Any solvent and redecyl acetate that are in progress are used, that is, again baking together crystallization processes. Compounds that only exist in the cationic (amine), This caking of the salt is not counteracted in the anionic (hydrochloric acid or acetic acid) by adding small amounts of substances, some have an anti-caking effect,
which suppress this agglomeration by using a known method of manufacture lie down between the crystals. The crystals become 50 of a non-caking, free flowing either mechanically separated from each other mixed fertilizers are mixed fertilizers (NPK) (For example, by inert additives) or by being in a granulated or granular state with a treated with a thin, hydrophobic and insulating cationic amine (German Ausleger-Uberzug (e.g. by adding certain organic writing 1 075 642). However, this method has the Substances which have a particular affinity for the disadvantage that the fertilizer granulates first having treating salt) are provided. must be what a separate work step However, certain fatty amines used for this purpose have made it necessary. Furthermore, the must be used the disadvantageous property, under certain circumstances, physio-anti-caking agents which reduce the surface tension to act logically allergic. Contain substances and solvents, i.e. substances The present invention is based on studies 60 relating to the manufacture of the anti-caking agent used arose, which were intended, the disadvantages, which make them considerably more expensive. the use of the known simple or too-known to be used as an anti-caking agent Compound additives to prevent the also aqueous emulsions of pitches and mineral caking Own of salts, avoid using an oxide powder. Such an emulsion has a without a lower anti-caking effect, they take up a very high proportion of water and are added to the to have to, but if possible, a drying salt added (German Aushöhere To achieve profitability. legend 1 040 049). The disadvantage of this procedure Among those for the latter purpose is that that for the preparation of the emulsion