RU2351577C2 - Fertilisation compositions - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: invention refers to agriculture and concerns method for making fertilisation composition. Method includes the stages as follows: a) interaction of humified mineral chosen from the group including leonardite, lignite, xylolith and peat, in water with gluconic acid added to the specified mineral in amount ensuring reaction medium pH reduced to less than 2.5; and b) sequential addition to the mixture of alkaline reagent in amount ensuring pH reduced to the value corresponding to that of alkaline medium. Besides, the invention concerns liquid fertilisation compositions and granulated fertilisation compositions to be produced by declared method. Additionally, the invention concerns applications of granulated composition as fertiliser, particularly, for plant growth stimulation, application of granulated composition for higher fertility of arable soils or for cleaning of arable soils contaminated with chemical products and/or toxic metal ions. The invention also refers to applications of liquid composition for localised leaves irrigation and/or spraying fertilising.

EFFECT: invention allows for improved method for making liquid or solid fertiliser with enhanced properties and extended application.

20 cl, 4 ex

Description

This invention relates to a method for producing a fertilizer composition using fossils containing fossilized residues of organic matter (hereinafter referred to as “fossils”) with a high content of humic acids, in particular, Leonardite ore, and fertilizer compositions obtained in this way.

Leonardite is an oxidized form of lignite, which has been used for some time as a source of organic materials, in particular humic and fulvic acids, and which is intended to be used as an additive for soil treatment to regulate plant growth.

US Pat. No. 4,698,090 describes a method for producing a liquid composition that is used to control plant growth, where the Leonardite ore is reacted with an organic chelating agent in an aqueous medium at a temperature in the range of 77 ° C. to 107 ° C. The chelating agents used are ammonium salts or metal salts of hydroxy acids, in particular, such as gluconic, glucoheptonic, tartaric, tartronic acid, galactaric, glucaric, glutaric and glutamic acid, or glutamines, as well as synthetic organic chelating agents, such as EDTA.

At the end of the interaction, the method optionally includes adjusting the pH value by adding sodium or potassium hydroxide and separating the liquid phase, which is used as fertilizer.

US Pat. No. 4,786,307 describes a process for the preparation of liquid micronutrient compositions, wherein the Leonardite ore extraction product in water with a chelating agent, which consists of a hydroxy acid salt, is combined with a salt of a metal cation, which is a micronutrient, in the presence of hydroxy acid followed by the addition of anhydrous ammonia to the reaction mixture to adjust the pH to values in the range from 7.5 to 9.

This invention relates to an improved method for producing fertilizer in liquid or solid form, having improved properties and a wide scope.

In particular, the invention relates to a method for producing a fertilizer composition, which is characterized in that it comprises the steps of reacting a fossilized fossil with a high level of humification, which is selected from the group consisting of leonardite, lignite, xylolite (xylite) and peat, in water with gluconic acid and subsequent extraction of humic compounds by adding to the mixture an alkaline reagent, preferably potassium hydroxide or ammonium hydroxide, to achieve a pH value corresponding to an alkaline medium, preferably a pH value greater than 9.

The present invention also relates to a fertilizer composition, which can be obtained as described above; this fertilizer composition containing the reaction product of gluconic acid with humic and / or fulvic acids, which are contained in the fossil and which are extracted with ammonium or potassium hydroxide, will be further defined by the term “glucohumate complex”.

A preferred fossil with a high level of humification is Leonardite, preferably with a humic acid content of more than 80% (wt.). Further in the description, reference is made to the use of leonardite as a preferred material, but taking into account the fact that other fossil fuels mentioned above can be used.

In the first stage of the method according to this invention, finely ground Leonardite, for example, the particle sizes of which, as determined by sieving, are in the range from 50 to 300 μm, is mixed with water, preferably demineralized water or low-sodium spring water; the amount of leonardite relative to water is usually from 20% to 35% (wt.) and in any case is sufficient to obtain a mixture or suspension, which will be stable with stirring.

Then, with gentle stirring, technical grade gluconic acid (usually a 50% aqueous solution of gluconic acid in water) is added to the mixture of Leonardite and water, and the mixture is continued to mix slowly.

The first stage reaction in water in the presence of gluconic acid is preferably carried out while maintaining the temperature of the suspension at a level of less than 60 ° C, more preferably at a temperature in the range from 15 ° C to 30 ° C. The added amount of gluconic acid, expressed as a 50% (wt.) Solution of gluconic acid in water, is usually from 3% to 10% (wt.) Of the weight of leonardite or other fossil fuels used, so that the pH of the suspension is further acidified due to addition of gluconic acid is usually in the range of 2 to 3, preferably less than 2.5.

Stirring of the mixture thus obtained usually lasts from 2 to 4 hours, after which the mixture optionally remains stationary for about 6 to 12 hours at a temperature preferably in the range of 17 ° C to 30 ° C.

After this, an alkaline extractant is added to the mixture, preferably potassium or ammonium hydroxide, usually in an amount that provides a pH of more than 9, preferably more than 11. Typically, the amount of potassium hydroxide, expressed as 48-50% (wt.) Potassium hydroxide, is from 6% to 15% (wt.) the weight of Leonardite.

Stirring of the resulting mass then continues for 6 to 12 hours, followed by optionally storing in a stationary state for up to 24 hours.

In a first embodiment of the invention, the product thus obtained can be dried and granulated to obtain a granular product for use as a fertilizer.

Alternatively, filtration is carried out to separate the liquid phase, which can be used in such a state for localized fertilizer by irrigation.

In a preferred embodiment of the invention, the properties of the fertilizer composition thus obtained can be further improved by the addition of urea, and the resulting product will hereinafter be called urea glucohumate.

In one embodiment of the invention, urea can be added after completion of the reaction with potassium or ammonium hydroxide, which guarantees extraction of humic compounds (humic acids, fulvic acids and humic materials).

In this case, urea is added to the mass of the mixture in an amount of 10 to 60% by weight of the Leonardite used, and the mass is mixed for 3 to 6 hours to ensure the formation of a bond between the urea nitrogen atom and the organic mass. After this, the product enters the dryer and granulator. Alternatively, the mass thus obtained can be additionally diluted with water in an amount sufficient to obtain a suspension, which can be filtered to obtain the drug in liquid form for use by applying to leaves and localized fertilizer by irrigation.

Alternatively, urea can be added to the liquid phase obtained by filtering the reaction product with potassium or ammonium hydroxide.

In this case, the amount of urea is usually from 20% to 60%, preferably from 50 to 60% (wt.), The mass of the liquid phase.

The composition according to this invention may further include other macro- and micronutrients, which are preferably added to the mixture after mixing and completion of the reaction with ammonium or potassium hydroxide. In particular, micronutrients may include:

- phosphates (polyphosphates);

- potassium salts (carbonate, etc.);

- calcium salts (carbonate, phosphate, etc.);

- magnesium salts (carbonate, etc.).

Micronutrients may include:

- zinc compounds such as zinc oxide and organic zinc salts;

- iron salts;

- Manganese salts, copper salts, boron salts, molybdenum and cobalt compounds.

Typically, the amount of macro- and micronutrients is less than 15% (wt.) Of the fertilizer composition.

In addition, the composition may preferably include plant extracts, in particular such as extracts of castor oil and lupine seeds, usually in an amount of not more than 20% by weight of the composition, preferably in an amount in the range from 15 to 20% (wt.).

According to another distinguishing feature, this invention relates to granular absorption materials, preferably comprising the above micronutrient and macrocell nutrients and / or the above extracts of castor bean grass and lupine seed, the compositions of this invention are converted into compositions with a high level of moisture absorption by adding polymers to the granules, having exceptional absorption properties, which are usually used in an amount of 10% to 50%, preferred Between 10% and 25% (wt.), the weight of the composition.

Suitable materials having exceptional absorption properties include, in particular, starch hydrolysis products and polyacrylonitrile.

The method and composition according to this invention are further illustrated by the examples below.

Example 1 Glucohumate Complexes

In this example and the examples below, American Leonardite (North Dakota or New Mexico) is used, characterized by the following analytical indicators, expressed as a percentage based on weight:

Organic carbon of biological origin 52% Organic nitrogen 0.75% Total organic matter 90% Extraction of organic matter, expressed as a percentage of the total organic matter 85% The content of humified organic matter, expressed as a percentage of the content of organic matter capable of undergoing extraction 93% pH in water 3-3.5

Leonardite is subjected to fine grinding, preferably in a rod-type mill with a speed in the range from 8000 to 12000 rpm, after which it is introduced into a rotary mixing apparatus (concrete type mixing apparatus), to which water is then added until a turbid mixture is obtained; gluconic acid (50% concentration) is added in an amount of 5 to 8% by weight of Leonardite, and the mixture is slowly stirred for approximately 2 hours; the resulting mass is left in a stationary state for about 6 to 12 hours at a temperature in the range from 17 ° C to 30 ° C; then add liquid potassium hydroxide with a concentration of from 48 to 50% in an amount of 6 to 15% by weight of leonardite present in the mixture, and the resulting mixture is slowly stirred for approximately 6 to 12 hours (depending on the temperatures used).

The product thus obtained is transferred to a drum-type dryer and granulator to produce natural organic fertilizer in granular form.

Alternatively, the same mixture may not be transferred to a drum dryer and granulator, but filtered after a suitable dilution with water in a suitable centrifuge to obtain a liquid fertilizer composition, which is intended, in particular, for use in a localized fertilizer by irrigation.

Example 2

The preparation of the composition is carried out in accordance with the method described in example 1, using instead of potassium hydroxide, ammonium hydroxide at a concentration of 28 degrees Bome.

Glucohumate complexes obtained in accordance with the method described above, in particular in solid granular form, are fertilizers with controlled release of the active substance, which are useful for increasing the fertility of arable soils, as well as for cleaning arable soils contaminated with chemicals and / or toxic metal ions.

In particular, their application leads to technological, agronomic and environmental advantages, which can be summarized as follows.

1. High levels of activity when cleaning soils contaminated with chemicals (chlorine derivatives, bromine derivatives, etc.), toxins, toxic metal ions, with an improvement in the physical, chemical and biological characteristics of the soil.

2. A significant increase in the fertility of depleted soils or soils on which crop rotation, sandy soils, saline soils with high conductivity have not been used.

3. The release of all nutrient elements of the fertilizer into the soil with an increase in the ability of the soil to cation exchange.

4. Introduction to the soil of organic matter with a high level of humification, more accessible to plants.

5. Increase in all types of biochemical activity of the soil.

6. Increase in the processes of chlorophyll photosynthesis in plants.

7. Improving the resistance of plants to stress due to adverse climatic factors for the soil.

8. Increase seed germination.

9. A noticeable decrease (up to 70%) in the application of mineral and chemical fertilizers to the soil.

10. The general exception of the introduction of nitrates into the soil by traditional methods of plant nutrition.

11. Noticeable improvement in agricultural products in terms of quality and quantity.

12. Increasing the content of sugars, vitamins, mineral salts and carotenoids (lycopenes) in fruits and vegetables.

13. Reducing the cycle of plant development with the corresponding transfer to an earlier date of receipt of fruits and vegetables on sale.

14. Improving the internal protection of plants from parasites of the fungal and bacterial type.

15. Providing soil cultivation that is always fertile and productive.

16. The complete absence of fermentation processes of the introduced organic matter, since it is completely mineralized.

17. High levels of antimicrobial activity due to the presence of gluconic acid in the preparation.

18. Complete elimination of groundwater pollution due to leaching of mineral salts.

19. The maximum guarantee of obtaining fruit and vegetable products free from toxic elements and / or polluting chemicals.

Thus, the compositions are used depending on the above distinguishing features and advantages that must be obtained.

Example 3 - Urea Glucohumate

75 liters of water, preferably demineralized, and 20 kg of finely ground Leonardite are introduced into the dissolution device and slowly mixed with the addition of 100 cm ^{3 of an} organosilicon antifoam and 4 kg of 50% (wt.) Gluconic acid, and the resulting mixture is stirred for about 3 to 4 hours (depending on operating temperatures).

After a specified period of time, 6 kg of potassium hydroxide in the form of flakes were added to the mixture, and the resulting mixture was stirred vigorously for 6 hours. Then the mass is left in a stationary state for 24 hours, after which the liquid phase (colloidal suspension) is separated from the solid phase by centrifugation. A certain amount of the liquid phase (40 kg) is transferred to a second dissolution device equipped with stirrers, where 60 kg of urea nitrogen is added based on liquid urea nitrogen with a urea nitrogen titer of 30%. After this, the product thus obtained is placed in containers of opaque polyethylene, and in fact it is ready for use.

The product has the following final composition:

Total organic matter from leonardite: humified organic matter 5.93% Potassium: potassium oxide (K ₂ O), soluble in water 4,51 Gluconic acid 0.83 Total nitrogen 18.05% Urea Nitrogen 18.00

As an alternative to the method described above, the same amount of urea nitrogen is added directly to the mixture in the first dissolution apparatus, and the resulting mixture is slowly stirred for 3 to 6 hours.

After this, the product is fed into the dryer and granulator to obtain granular fertilizer.

In particular, the use of the fertilizer compositions described above (urea glucohumate) eliminates the disadvantages associated with the use of urea, which is the most common nitrogen fertilizer.

The biggest drawback associated with the use of urea is its low soil resistance, which, on average, is about 15 to 20 days, depending on the type of soil and the ambient temperature, due to the geographical location of the region. Another negative characteristic feature of the use of urea fertilizer is its high toxicity, which under certain conditions, such as high pH, high temperatures and high conductivity, can occur in vegetation.

The use of urea glucohumate includes the following technical and agronomic advantages:

a) a marked increase in the stability of urea nitrogen in the soil, which, depending on the ratio of it and the glucohumic substances present in the preparation, can reach 4 months;

b) the complete elimination of risks associated with the phytotoxicity of urea;

c) Slow, continuous and protected release of urea nitrogen without leaching problems;

d) significantly reduced soil ammonia emissions after application of the drug;

f) a decrease (up to 50%) in the number of fertilizers based on nitrogen crops due to the complete absence of losses due to leaching and / or adverse soil conditions;

f) the use of the drug in all types of pre-sowing treatment, both extensive and intensive, in the field and under protected treatment, regardless of technical, agronomic conditions or ambient temperature;

g) the possibility of localized introduction of the product (into the furrows for presowing treatment);

h) use on lawns, specialized planting of flowers, planting in nurseries, potted plants;

i) the introduction into plants of mineralized organic matter with a high level of humification;

l) improving the physical, chemical and biological characteristics of the soil.

The urea liquid glucohumates that make up the subject of Example 3 use:

- for fertilizer by irrigation in greenhouses and in the field in quantities of 10 to 15 kg / 1000 m ^{2 of} surface area every 8 to 10 days; and

- for foliar spraying in quantities of 5 to 6 kg / 1000 liters of water every 10 to 12 days.

Preliminary tests conducted in the field in vegetable growing associated with growing pumpkin, celery, leaf lettuce, radish and tomato plants showed an increase in productivity by 10% to 20%, a qualitative improvement of 10% to 25% and an increase in resistance to fungal infection in the order of 20 to 25% compared with untreated cultures.

Example 4 - High Moisture Absorption Glucohumates

The method is carried out in accordance with the method of example 3, and after adding potassium hydroxide and slowly mixing the mixture for 12 hours, other nutrients (macronutrients and micronutrients) are added to the resulting “turbid” mixture in amounts of not more than 15% (wt.) Of the processed masses; then plant extracts of castor bean plant and lupine seeds are added in an amount of 15 to 20% of the total processed mass.

After this, the product is fed into the dryer and granulator. At the outlet of the granulator, the granules obtained in this way are fed to the mixer in the absence of air, where substances with exceptional absorption properties (derivatives of hydrolyzed starch) are added in quantities ranging from 15 to 25% (wt.) Of the processed mass.

Substances with exceptional absorption properties are fixed on the outer surface of the fertilizer granules, which are then packaged in a vacuum to prevent absorption of moisture from the environment.

It is clear that in the described example, the addition of nutrients and extracts of castor bean and seeds of lupine is optional.

The granular compositions thus obtained are used, in particular, as fertilizers, in particular for cultivation in arid zones. Bright characteristic features of such a composition are:

i) good retention of moisture resulting from irrigation or in the form of environmental moisture, which is always available in the root system;

ii) a significant reduction in the phenomenon of leaching of the soil, since granular fertilizer captures the water present, swelling in volume with an increase in mass up to 150 times;

iii) balanced nutrition of plants with continuous availability of mineral salts contained in the preparation, which in a stable jelly-like solution are always ready for assimilation by plants;

iv) pure soil structuring with an improvement in its physical condition due to hyperation of soil particles after an increase in the mass of granules;

v) the introduction of all the nutrients necessary for the metabolic functions of plants;

vi) elimination of transplant shock for young plants;

vii) a marked reduction in irrigation;

viii) the possibility of developing plant root systems;

ix) in addition to the introduction of protein substances with a high content of organic nitrogen, the introduction of the active ingredients of plant origin contained in common castor oil plant and lupine seeds, which, in addition, have a strong repellent effect on land-living insects and hypogenic nematodes.

x) a significant reduction in the introduction of nutrients (N, P, K and trace elements) into the soil; the impossibility of washing out the nutrients contained in the granules, since they are protected inside a gel-like mass formed in the presence of moisture;

xi) the possibility of cultivating arid and desert territories or soils with high conductivity, since environmental moisture (which is released in these areas at night) allows the systematic cultivation of species of interest to agriculture and the food industry.

Typically, the granule size of the fertilizer composition can be in the range from 0.5 mm to 1 cm, and the granules are capable of absorbing a mass that is 150-200 times greater than their own mass, due to the gelling substance present in them having exceptional absorption properties.

Claims (20)

1. A method of obtaining a fertilizer composition, characterized in that it includes the following stages:
a) the interaction of a humified fossil, which is selected from the group consisting of leonardite, lignite, xylolite and peat, in water in the presence of gluconic acid, and gluconic acid is added to the specified fossil in an amount that allows the pH of the reaction medium to be brought to a value of less than 2.5 , and
b) sequentially adding an alkaline reagent to the mixture in an amount that allows the pH to be adjusted to a value corresponding to the alkaline medium. 2. The method according to claim 1, characterized in that the amount of added gluconic acid based on 50 wt.% Gluconic acid is from 3 to 10 wt.% Fossil. 3. The method according to claim 1, characterized in that the alkaline agent is potassium hydroxide or ammonium hydroxide. 4. The method according to claim 1, characterized in that the alkaline agent is potassium hydroxide added in an amount of 6 to 15% by weight of the fossil, where the specified amount is expressed based on 48-50% wt. potassium hydroxide. 5. The method according to claim 1, where stage a) is carried out at a temperature not exceeding 30 ° C. 6. The method according to claim 1, where stage a) is carried out with stirring for 2 to 4 hours, followed by a stationary period of 6 to 12 hours. 7. The method according to claim 1, where in stage b), stirring continues for 6-12 hours, followed by an optional period of stationary state lasting up to 24 hours 8. The method according to claim 1, characterized in that it includes adding to the product of stage b) substances containing nutritious macro- and microelements. 9. The method according to claim 8, characterized in that it includes the addition of urea in amounts ranging from 10 to 60% of the mass of the fossil. 10. The method according to claim 8 or 9, characterized in that it includes the addition of plant extracts, in particular extracts of castor oil plants and common lupine seeds. 11. The method according to claim 1, where the product obtained in stage b) is subjected to drying and granulation to obtain a composition in granular form. 12. The method according to claim 11, characterized in that the granular composition is mixed with polymeric substances having exceptional absorption properties, in particular derivatives of hydrolyzed starch, to obtain a granular composition with a high level of water retention. 13. The method according to any one of claims 1 to 8, characterized in that the product of stage b) is filtered to separate the liquid phase, which is intended for use as a liquid fertilizer. 14. The method according to item 13, wherein the urea is added to the liquid phase obtained by filtration in an amount of 20 to 60% by weight of the liquid phase. 15. The method according to claim 1, characterized in that the fossil substance is a Leonardite ore. 16. Fertilizer compositions in liquid form, which can be obtained by the method according to any one of claims 1 to 10 and 13-15. 17. Fertilizer compositions in granular form, which can be obtained by the method according to any one of claims 1 to 12. 18. The use of the granular composition according to 17 as a fertilizer, in particular, to stimulate plant growth. 19. The use of the granular composition according to 17 for increasing the fertility of arable soils or for cleaning arable soils contaminated with chemical products and / or toxic metal ions. 20. The use of a liquid composition according to clause 16 for fertilizing by localized watering and / or spraying of leaves.