RU2580469C2 - Method of producing liquid humic organo-mineral fertiliser for plants - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: invention relates to agriculture. A method of producing a compound bio-preparation from humus-containing substances via alkaline extraction, separating and neutralising the alkaline extract, wherein alkaline extraction is carried out with 0.1 M potassium pyrophosphate in 0.1 n KOH solution or 0.1 M sodium pyrophosphate in 0.1 n KOH solution or 0.1 M sodium pyrophosphate in 0.1 n NaOH solution at 80°C, and after separation, neutralising the alkaline extract with nitric acid HNO₃ to pH 7.0-8.0, mixing, settling and obtaining a liquid end product.

EFFECT: invention increases the content of humic substances in the end product, enables to control the amount and ratio of sodium and potassium in the end product, as well as potassium and sodium salts of humic substances, increases the content of common phosphorus in the end product owing to the use of sodium pyrophosphate in the extractant, and common phosphorus and common potassium when using potassium pyrophosphate.

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Description

The invention relates to the field of agriculture and can be used to obtain biological products - liquid humic organic-mineral fertilizing for plants from humus-containing substrates, namely from vermicomposts and composts.

It is well known that water-soluble salts of natural humic compounds: humic acids and fulvic acids — humates and fulvates of Na, K or NH ₄ in very low concentrations (0.001-0.0001%) [1] are effective stimulants of plant growth and development.

In recent decades, in many countries of the world, including Russia, some companies for the production and production of various bacterial and humic biological products for agricultural purposes began to widely use end products of aerobic fermentation of organo-waste products (composts and vermicomposts) as raw materials.

The production of humic biological products from vermicompostes by alkaline treatment in the liquid phase is the most widely used technology. Alkaline treatment of the initial substrates in water allows one to obtain more concentrated preparations that contain almost all components (water-soluble and alkali-soluble) of vermicompost: salts of humic acids and fulvic acids, amino acids, peptides, vitamins, antibiotics, plant growth and development hormones, and other soil vital products microorganisms and earthworms themselves (vermiculture). Moreover, alkaline treatment allows not only more fully extracting all its components from vermicomposts, but also repeatedly enhancing the physiological activities of humic acids themselves, forming their water-soluble salts: humates of sodium, potassium or ammonium. This technology is waste-free, since the precipitate of vermicompost after alkaline extraction contains the organo-mineral part of vermicompost and water-insoluble humates of calcium, iron, copper and other metals. After drying, this precipitate can be used as a high-value component in the composition of soil.

A known method of obtaining a biological product of complex action, which consists in the fact that vermicompost is pre-soaked in 3-5 volumes of water at a temperature of + 20 ... + 35 ° C, stirred and sedimented for 30 minutes, an aqueous extract from vermicompost containing soil bacteria, poured into a separate tank, then extracted from the sediment of vermicompost alkali-soluble substances and salts of humic substances in 20 volumes of 0.1 N. alkali solution KOH, NaOH or NH ₄ OH at a temperature of + 20 ... + 40 ° C. The alkaline extract is separated into a separate tank, washed with water, the combined alkaline extract is neutralized with a solution of nitric acid HNO ₃ to a pH of 7.0-8.0, then an aqueous bacterial suspension is added, mixed, defended and a liquid target product is obtained - a biological preparation of complex action for plants [2].

The disadvantages of this method of obtaining a liquid biological product of complex action are:

- low content of water-soluble salts of humic substances: humates and fulvates in the final target product, since alkaline extraction is carried out at a high ratio of solid and liquid phases (1:20), followed by washing the precipitate with water, which leads to a strong dilution of humates, fulvates and other physiologically active substances in the final product;

- low content of macronutrients: total phosphorus and total potassium.

A known method of producing a biostimulator of plant growth and development from humus-containing substances by pre-soaking the feedstock in water, followed by its homogenization and microbiological fermentation to increase the biomass of soil microorganisms at a temperature of 20-35 ° C for several hours with continuous aeration. The aqueous bacterial suspension is separated from the precipitate of a humus-containing substance, which is then subjected to alkaline extraction of 0.1 N. KOH or NaOH solution at a temperature of 80-100 ° C. The precipitate is washed with water, the combined alkaline extract is neutralized with nitric acid HNO ₃ to a pH of 8.0–9.5, after which a pre-prepared aqueous suspension of soil microorganisms is added to it, mixed, settled and a liquid target product is obtained [3].

The disadvantages of this method of obtaining such a biological product are:

- low content of water-soluble salts of humic substances: humates and fulvates in the final target product; and

- low content of macronutrients: total phosphorus and total potassium.

Thus, both methods of producing liquid biological products based on vermicompost, ultimately, do not allow to obtain highly concentrated final products and, as a result, their operational characteristics during large-scale use, transportation, and storage are unsatisfactory.

Back in 1961, Kononova and Belchikova proposed using 0.1 M sodium pyrophosphate Na ₄ P ₂ O ₇ * 10H ₂ O in a mixture with 0.1 N to accelerate the determination of the humus composition of various soil types. NaOH solution. They showed that this reagent allows one to more quickly determine and more comprehensively extract humic acids and fulvic acids from various types of soils [4]. This accelerated pyrophosphate method using sodium hydroxide and sodium pyrophosphate has become widely used in scientific research to isolate humic substances from the soil and study the organic matter of fossil soils [5]. This method is long, since the extraction of humic substances from the soil is carried out at room temperature for 12-18 hours.

A known method of obtaining a plant growth stimulator from sewage sludge from urban wastewater treatment plants. The method includes countercurrent extraction of sewage sludge with an aqueous solution of an alkaline agent. The extraction is carried out in two stages, in the first stage - with a solution containing potassium or sodium hydroxide and potassium or sodium pyrophosphate in a molar ratio of 4: 1-0.5 at a total concentration of 0.2-0.5 mol / l, at a temperature of 40- 50 ° C, with a liquid to solid ratio of 3-5: 1. In the second stage, extraction is carried out at a temperature of 20-40 ° C, the ratio of liquid and solid phases 3-5: 10.5-2.0% solution of ammonium hydroxide, into which, after extraction, potassium or sodium hydroxide and pyrophosphate are introduced in a ratio of 4: 1 -0.5 to a concentration of 0.2-0.5 mol / L. Then, the resulting solution is used for alkaline extraction in the first stage. The method allows to obtain a combined biologically active substance containing phytohormones and trace elements necessary for plants, as well as to simplify the process by reducing the flow rate of water for washing and the use of low temperatures [6].

The disadvantage of this method of obtaining such a biological product from sewage sludge is the complexity and multi-stage method of countercurrent extraction.

The present invention is aimed at improving the quality of the target product, obtained on the basis of humus-containing substrates, in particular highly humic organic fertilizers - vermicomposts, as well as from composts, zoogumus and sapropel or their mixtures by improving the conditions for extraction of humic substances from humic substances in the presence of such an alkaline solution salts like sodium pyrophosphate or potassium pyrophosphate, which leads to an increase in the content in the final product as salts of humic acids and fulvic acid from and total phosphorus and total potassium. This, ultimately, increases the agrochemical value and efficiency of the use of such biological products.

This object is achieved in that in the proposed method, a complex biological product for treating plants and soil from humus-containing substances is obtained by alkaline extraction, the alkaline extract is separated and neutralized, but in contrast to the analogue and prototype, humic substances are extracted with 0.1 M sodium pyrophosphate Na ₄ P ₂ O ₇ * 10H ₂ O or potassium pyrophosphate K ₄ P ₂ O ₇ * 3H ₂ O in 0.1 N alkali solution (KOH or NaOH) at a temperature not exceeding 80 ° C. In contrast to the method described in Russian patent No. 2178396 dated January 20, 2002 [6], in which it is recommended to use potassium or sodium hydroxide and potassium or sodium pyrophosphate in a molar ratio of 4: 1-0.5 at a total concentration of 0.2 -0.5 mol / l, at a temperature of 40-50 ° C, with a ratio of liquid and solid phases of 3-5: 1, the proposed method uses solutions of potassium or sodium hydroxide and potassium or sodium pyrophosphate not higher than 0.1 M, since at higher molar concentrations of these alkaline reagents, the volume of the solid phase of vermicompost increases during ction extraction process, which reduces the process efficiency and workability in the preparation of the final product. In addition, the optimal ratio of solid and liquid phases in the proposed method was 1:10.

After separating the alkaline extract from the water and alkali-soluble precipitate, neutralize it with nitric acid HNO ₃ to a neutral or slightly alkaline pH of a solution of 7.0-8.0, settle, filter and obtain a liquid target product.

Using the proposed method allows you to:

- significantly increase in the final target product the content of humic substances, in particular humates and fulvates;

- to regulate the amount and ratio in the final product of sodium and potassium, as well as potassium and sodium salts of humic substances;

- increase the content in the final target product due to the introduction of total phosphorus into sodium pyrophosphate in the extractant, and when using potassium pyrophosphate and total phosphorus, and total potassium (table 1).

It should be noted that the introduction of sodium pyrophosphate in the extractant additionally enriches the target product with macro-nutrients: phosphorus and sodium, and potassium pyrophosphate with phosphorus and potassium. The use of a 0.1 M sodium pyrophosphate solution in an alkaline extractant additionally increases the total phosphorus content in terms of P ₂ O ₅ by 1.60% and the total sodium in terms of Na ₂ O by 1.24%. The use of a 0.1 M potassium pyrophosphate solution in an alkaline extractant additionally increases the total phosphorus content in terms of P ₂ O ₅ by 1.60% and total potassium in terms of K ₂ O by 1.76%. Depending on the use of potassium pyrophosphate and / or sodium pyrophosphate in the alkaline extractant, both the sodium or potassium content in the final product and the ratio of these nutrients important for plants in the final product can be controlled in the final product. This is important because there are plants that need potassium or sodium more, or the ratio of these two elements that are most important for plant nutrition is of great importance.

Comparative analysis with the prototype shows that the claimed method is characterized by a new set of features consisting in the extraction of humic substances of 0.1 N. a solution of alkali (KOH or NaOH) containing 0.1 M sodium pyrophosphate or potassium pyrophosphate, a decrease in the mass ratio of substrate: extractant and optimization of the temperature of alkaline extraction (not higher than 80 ° C) in fractional fractionation of humus-containing substances are fundamentally new.

The above circumstances indicate that the claimed technical solution meets the criterion of "Novelty."

A comparison of the claimed method with known methods shows that it does not follow explicitly from the prior art for a specialist. This indicates the conformity of the claimed technical solution to the criterion of "Inventive step".

The invention is illustrated by examples.

Example 1. To obtain the claimed biological product, 10 kg of humus-containing material with a moisture content of 60-70% is loaded into the fermenter, 90 l of a 0.1 M solution of potassium pyrophosphate in 0.1 N are added. KOH solution. Alkaline extraction is carried out with constant stirring of the mixture using a mixer at a temperature of 80 ° C for 30 minutes, then the mixture is left to stand for 30-60 minutes, the alkaline extract is drained (pumped) into a storage tank. The alkaline extract is cooled and then neutralized with a solution of nitric acid HNO ₃ to a pH of 7.0-8.0.

The following materials can be used as humus-containing substances to obtain a complex biological product: vermicomposts, composts, zoogumus and sapropels, or mixtures thereof.

Example 2. The same as in example 1, but only instead of 90 l of a 0.1 M solution of potassium pyrophosphate in 0.1 N. KOH solution to the humus-containing raw materials add 90 l of a 0.1 M solution of potassium pyrophosphate in 0.1N. NaOH solution at a temperature of 80 ° C. Alkaline extraction is carried out with constant stirring of the mixture at a temperature of 80 ° C for 1 hour, then the mixture is left to stand for 30-60 minutes, the alkaline extract is drained (pumped) into a storage tank.

Example 3. The same as in example 1, but only instead of 90 l of a 0.1 M solution of potassium pyrophosphate in 0.1 N. KOH solution to the humus-containing raw materials add 90 l of a 0.1 M solution of sodium pyrophosphate in 0.1 N. NaOH solution at a temperature of 80 ° C. Alkaline extraction is carried out with constant stirring of the mixture at a temperature of 80 ° C for 1 hour, then the mixture is left to stand for 30-60 minutes, the alkaline extract is drained (pumped) into a storage tank.

In order to preserve the nativeness of the polymer molecules of humic acids and preserve their biological activity, alkaline extraction is carried out for 30 minutes at temperatures not exceeding 80 ° C. At this temperature, alkaline extraction does not hydrolyze the molecules of humic substances.

Using these techniques, it is possible to obtain the final target product from vermicompostes, in which the content of humic substances can be up to 5 g per liter, and when using vermicomposts in a mixture with peat or brown coal, up to 10-15 g per liter.

The proposed method allows you to extract almost all water-soluble and alkali-soluble components of humic substrates in a physiologically active state: humic acids, fulvic acids, vitamins, amino acids, plant growth and development regulators, bactericidal and fungicidal substances, micro and macro elements in a state bioavailable to plants.

Liquid complex biological products obtained by the present method from the above substrates are odorless dark brown liquids. The content of humic substances in the final products may be at the request of the manufacturer from 5 to 15 g per liter. The proposed method of obtaining a biostimulator of plant growth is simple in terms of hardware design and can be implemented in an industrial environment. Moreover, the method provides a liquid preparation of stably higher quality and with a higher content of physiologically active substances, water-soluble sodium and / or potassium salts of humic acids and fulvic acids, as well as with a higher content of macronutrients (total phosphorus, total potassium and sodium), which ultimately leads to its higher agrochemical effectiveness.

The use of these drugs in agricultural practice is environmentally safe for both humans and animals and soil microflora. They have the following properties:

- increase seed germination and germination energy;

- stimulate root formation; contribute to the rapid rooting of cuttings;

- stimulate the growth and development of plants;

- increase crop yields;

- increase the resistance of plants to adverse environmental influences during sheet spraying;

- improve soil structure during irrigation;

- reduce the amount of nitrates in plants;

- increase the content of proteins, sugars, vitamins in fruits and vegetables;

- eliminate chlorosis;

- stimulate flowering and fruiting;

- enhance the resistance of plants to bacterial and fungal diseases;

- increase the quality of the crop and extend the shelf life.

Information sources

1. Popov A.I. On the mechanism of the influence of humic substances on the production process of plants. "Humus and soil formation." Sat scientific Proceedings of St. Petersburg, state. Agricultural University, 2000. - No. 2. - S. 13-14.

2. Jemoyda V.L. A method of obtaining a complex biological product. Patent of Ukraine No. 633760 dated January 15, 2004

3. Titov I.N. A method of obtaining a biostimulator of the growth and development of plants from humus-containing substances. Patent of Russia No. 2253641 dated December 25, 2002

4. Kononova M.M., Belchikova N.P. Accelerated methods for determining the composition of humus. Soil Science, 1961, No. 10.

5. Martynova N.A. Chemistry of soils: soil organic matter: teaching aid. Irkutsk: Publishing house of the ISU, 2011 .-- 255 p.

6. Elkind K. M., Smirnova V. M., Tishkov K. N., Trunova I. G., Busorgin V. G., Kuznetsova T. N., Dubrovin A. M., Kasatikov V. A. A method of obtaining a plant growth stimulator. Patent of Russia No. 2178396 dated January 20, 2002.

Claims (1)

A method of obtaining a complex biological product from humus-containing substances by alkaline extraction, separation of the alkaline extract and its neutralization, characterized in that they are subjected to alkaline extraction with a 0.1 M solution of potassium pyrophosphate in 0.1 N. a solution of KOH or in a 0.1 M solution of sodium pyrophosphate in 0.1 N. KOH solution or 0.1 M sodium pyrophosphate in 0.1 N. NaOH solution at a temperature of 80 ° C, and then after separation of the alkaline extract, neutralize it with nitric acid HNO ₃ to pH values 7.0-8.0, mix, defend and get a liquid target product.