RU2742764C1 - Method for obtaining biologically active products in liquid and solid form from vegetable raw materials - Google Patents

Abstract

FIELD: chemical industry.

SUBSTANCE: invention relates to a method for obtaining biologically active products in liquid and solid form from plant materials. Disclosed is a method of obtaining biologically active products in liquid and solid form containing humic acids, fulvic acids, folate and soluble silicon from plant materials, which are preliminarily ground, treated with an aqueous alkaline solution of sodium hydroxide and / or potassium hydroxide to form a suspension. After that the suspension is separated into liquid and solid parts. Pasteurization of the liquid part and drying of the solid part are carried out to obtain liquid and solid biologically active products under certain conditions

EFFECT: obtaining biologically active products from plant materials in liquid and solid form with high content of biologically active substances - folate (vitamin B9), humic and fulvic acids, water-soluble silicon.

9 cl, 27 ex

Description

The invention relates to a method for producing biologically active liquids and biologically active solid additives from plant raw materials as additives in food and drinks, as well as to obtaining feed additives used in the diets of agricultural and domestic animals and poultry.

In addition, the fluids obtained according to this invention have positive biological activity when growing crops.

Since the 1990s, a large number of studies have been carried out on the production of humic acids and, as a rule, their accompanying fulvic acids in the form of liquid solutions and solid substances containing them. A number of outstanding properties of humic and fulvic acids have been revealed in their ability to grow crops and animals, as well as a positive effect on human health.

Moscow State Academy of Veterinary Medicine and Biotechnology named after K.N. Scriabin published "The use of lignohumate in poultry farming (guidelines)" (Moscow. 2004). The recommendations state: “In recent years, convincing results have been achieved in the use of substances of a humic nature as biologically active additives to feed in poultry farming. In small doses, humic substances have a significant effect on the main links of metabolism, which increases the productivity of the bird and its resistance to adverse environmental conditions.

Researchers associate the biological activity of humic substances with their effect on redox processes, and this effect is explained by the presence in the composition of humic acids of chemical groups (polyphenols, oxyquinones, quinones), which play the role of hydrogen carriers and oxygen activators, which stabilizes the intracellular breath. At the same time, humic acids are not only a source of energy, but also a biologically active substrate that catalyzes metabolic processes. Finally, humic acids stimulate the work of the pancreas and endocrine glands, improve the digestibility of components in feed.

NPO "RET" together with the Department of Poultry and Bird Diseases MGAVM and B them. K.N. Skryabin and specialists from leading poultry enterprises conducted numerous studies on poultry egg and meat productivity. The results of these studies confirmed the high biological and economic efficiency of lignohumates as a feed additive and immunomodulators. It was found that potassium or sodium lignohumate is not toxic to poultry in recommended doses and has a stimulating effect on productivity. Potassium lignohumate - a preparation in liquid form (20% solution) was given to laying hens with drinking water at a dilution of 1:20, 60 ml per 1 kg of live weight, once a day. At the same time, the rate of egg-laying increased by 5.3% in comparison with the control data. Experiments were also conducted on the use of lignohumate for the growth and development of chickens. It was noted that the introduction of the drug into the diet contributed to the better growth and development of chickens by 3.4% compared to the control. At the same time, the best results were obtained when using sodium lignohumate in a dose of 20 ml per dry matter per 1 kg of live weight.

In patent document DE 102015100645 A, 07.21.2016, "Production of bulk fertilizer based on liquid humic and fulvic acids, as well as solid inorganic and organic substances as an additive to water and soil for a positive effect on the balance of nutrients" it is stated (0017): " The classical method for obtaining humic acids is the extraction of peat or brown coal diluted with an aqueous solution of sodium or potassium hydroxide. "

The humates are dissolved in the extraction solution and separated by filtration, decantation or centrifugation from undissolved peat or coal components. After acidification of the extract with excess mineral acid, humic acids insoluble in water are formed, which can be separated. However, as stated in the patent CN 1098437 A, 08.02.1995: "Due to the technological complexity, investments in technological equipment, low efficiency, often the extract contains a significant amount of harmful substances and is limited to raw materials."

In accordance with the patent CN 1098437 A, 08.02.1995, obtaining a solution of humic acid involves:

- 1.milling: first stems and leaves (leaves, twigs, cotton stems, corn stems, citrus fruits), seeds (castor, hemp, cotton, sunflower, etc.) and cereals (corn, millet, sorghum, etc.) .) with grinding up to 20-80 mesh .;

- 2. mixing for the first fermentation in the ratio: stems and leaves 45-55%, seeds 15-20%, cereals 8-12%, water 20%, and loaded into a fermentation tank at a temperature of -20-35 ° C. Natural fermentation for 2-3 days with an increase in temperature to 60-70 ° C;

- 3. secondary fermentation, with the addition of 5-10% yeast enzymes and lowering the temperature to 32-36 ° C, fermentation for 3-4 days;

- 4. extraction of the fermentation product with 1-2% alkali solution for 6-8 hours at room temperature, then extrusion using an extruder, while the filtrate was a nutrient solution of humic acid;

- 5. sterilization and packaging, the solution was sterilized at a temperature of 121 ° C.

The patent states that "as feed additives, the mixture is used not only to increase the production of milk, eggs, livestock, but also to increase immunity and resistance to disease, the resulting organic meat and eggs are ideal complements."

The present inventors have also found that the mixture in medicine and the beverage industry also has a wide range of uses. The liquid component of this substance also affects pathogens, inflammation, bleeding, cancer, etc., and can also improve immune function.

Therefore, in many respects, new methods of obtaining humic acids are being developed both from various types of organic raw materials and the peculiarities of their production. So, in the patent of the Russian Federation No. 2112763, 06/10/1998, a method is described for obtaining a liquid biostimulator of plant growth and development from humus-containing substances by alkaline extraction followed by neutralization of the extract, characterized in that manure wastes from livestock enterprises that have previously undergone a biotechnological process are used as the initial humus-containing substance processing to obtain compost, in addition, an aqueous bacterial suspension is isolated from the compost, for the production of which the compost is soaked in water, the bacterial mass is extracted from it into an aqueous solution, the resulting bacterial suspension is separated from the solid fraction of the compost, and the resulting solid fraction is subjected to alkaline extraction, and the extract of the extract spend 0.1-1.0 N. alkali solution at 20-50 ° C, followed by separation of the liquid extract, while the latter is mixed with a bacterial suspension and defended to obtain the target product.

The results of field experiments showed the high efficiency of the drug: the yield of winter wheat increased by 11.3-12.4%, spring barley by 11.3-15.5%. However, the complexity of the method described in this patent led to the refusal of its application and the termination of the patent from 01.01.2002.

In the patent of the Russian Federation 2296731, 10.04.2007, a method for obtaining complex humic organomineral fertilizers is described, including mixing of caustobioliths of the coal series with mineral fertilizers and alkalis, dehydration, granulation and thermal drying of granules, which differs in that humic acids and humates are preliminarily obtained by means of cavitation dispersion caustobiolites in an aqueous solution of alkalis until the complete yield of humic acids, followed by the production of humates by adding hydroxides, carbonates and hydrogencarbonates of potassium, sodium, ammonium and cavitation dispersion until the temperature of the mixture reaches 80-90 ° С, an organomineral component is obtained by cavitation dispersion of lignocellulosic raw materials in an aqueous medium , mineral fertilizers and microelements, as well as the organocarbohydrate component by cavitation dispersion in the water environment of municipal solid waste before converting starches into easily digestible substances, hydrolyzing fats to a low molecular weight lary carboxylic acids, after which all the obtained components of the fertilizer are mixed, the mixture is cavitationally homogenized, dehydrated, granulated and heat dried.

However, this patent was not implemented and expired on 05/04/2008.

In the patent of the Russian Federation 2420500, 06/10/2011, a method for obtaining organic fertilizers is described, including mixing of coal series caustobioliths with mineral fertilizers, alkalis, a lignocellulose component and highly toxic agricultural waste, disinfection, dehydration and transfer to granulation, characterized by the fact that humates are preliminarily obtained actions by cavitation dispersion of caustobiolites in an aqueous solution of alkalis until the complete release of humates and reaching a temperature of 75-90 ° C, or humates of prolonged action by cavitation dispersion of caustobiolites in an aqueous solution of acid until a temperature of 60 ° C is reached, and then alkali is added and dispersed until the temperature is set 75-90 ° C and obtaining humates with controlled release of the active substance, a lignocellulosic component of fast action is obtained by cavitation fermentation dispersion of raw materials in an aqueous solution with the addition of a starter culture ophilic bacteria with the participation of chemical and catalytic fermentation, or the lignocellulosic component of prolonged action by cavitation dispersion of raw materials in an aqueous solution of mineral fertilizers and microelements with the addition of pig manure or poultry manure until the temperature reaches 75-90 ° C, highly toxic agricultural waste - pig manure and poultry droppings, which make up the organic part of fertilizers, are processed into a fast-acting component by cavitation dispersion of raw materials in an aqueous solution of thermophilic bacteria with chemical and catalytic action and a prolonged-action component by cavitation dispersion of raw materials in an aqueous solution of mineral fertilizers and microelements until the temperature reaches 75-90 ° C, the suppression of all bacteria, microbes, pathogens, worm eggs, seeds of plants that have not lost their germination is carried out by cavitation dispersion and providing mechanical, warm new, electrical and chemical action, dehydration of the organomineral suspension is carried out by spraying the suspension heated to 75-90 ° C in a vacuum with the organization of explosive boiling, fine atomization and rapid dehydration.

The lignocellulosic component of the fertilizer is prepared for fast and long-acting fertilizers.

a) Preparation of lignocellulosic raw materials for fertilizers with prolonged action and its cavitation treatment is carried out according to the technology described above.

b) Preparation of lignocellulosic raw materials for fast-acting fertilizers consists in carrying out chemical anaerobic or catalytic fermentation.

- During chemical fermentation, to ensure the hydrolysis of cellulose, mineral acids are added, which provide starch and sugar from cellulose. At the end of the chemical fermentation process, the suspension is neutralized with sodium or potassium hydroxide.

- In the Catholic fermentation of lignocellulosic raw materials, catalysts developed by the Institute of Catalysis named after G.K. Boreskov SB RAS.

Anaerobic fermentation with the participation of thermophilic bacteria is used to decompose plant materials (flax fire, straw, sunflower husks). During fermentation with the participation of thermophilic bacteria, water is poured into the fermentation vessel, light-celluloid raw materials and a starter culture from thermophilic bacteria are poured. Then the mixture is sent to a cavitation apparatus with a soft cavitation mode, and from it again to a container, etc.

Cavitation-enzymatic processing of the mixture is carried out until it reaches a temperature of 80 ° C, after which the suspension is left in a container until it cools down to 40 ° C.

There is a known method of obtaining a solution of biologically active substances from poultry droppings, described in RF patent 2687452, 05/13/2019. The method includes preliminary grinding and homogenization of poultry droppings, followed by the stage of hydrolysis in the presence of an alkaline solution and the stage of anaerobic fermentation in a mesophilic mode at a humidity of 90-93% of the mass. further separation of the suspension obtained after the stage of anaerobic fermentation with separation of the liquid and solid phases, the use of a part of the liquid phase at the stages of hydrolysis and anaerobic fermentation and the removal of the remainder of the liquid phase as a solution of biologically active substances, which differs in that the stage of hydrolysis is carried out in two stages: the first stage is carried out for at least one day at a temperature of 25-30 ° C, a humidity of 85-87% of the mass. the initial pH of the medium is 8.3-8.5, in the presence of a solution of potassium hydroxide or sodium hydroxide or a mixture thereof, the second stage is carried out at a temperature of 34-36 ° C, humidity 88-90% of the mass. the initial pH of the medium is 7.6-7.8, the stage of anaerobic fermentation is carried out at a temperature of 34-36 ° C, the initial pH of the medium is 7.0-7.3, while part of the liquid phase obtained after separation is used to dilute the suspension to the required moisture content at the stages of hydrolysis and anaerobic fermentation, the rest of the liquid phase is removed after temperature pasteurization as a solution of biologically active substances, and the solid phase obtained after separation is sent for extraction with water to obtain a liquid extract, which is fed for grinding and homogenization, and solid residue, which is used as a soil improver. The solution of biologically active substances contained 2.1-2.4% of the mass. humic acids and 1.3-1.7% of the mass. fulvic acids.

When testing the solution, when treating cucumber seeds, germination increased by 12%, the biomass of seedlings increased by 7%.

In the patent of the Russian Federation 2630281, 09/06/2017, "Supplement from vegetable raw materials", a silicon-containing additive is proposed for food and feed purposes, as well as for fertilizers, including vegetable raw materials and an additional component subjected to mechanochemical activation, while the additive from vegetable raw materials contains rice husk and includes an additional component selected from the group: soluble sugar, and / or baking soda, and / or a chelating agent of the catechin type, in an amount up to 40% of the mass. and the additive particles are less than 100 nm in size. At the same time, it was indicated that the new additives dissolve faster and provide a high concentration of monomeric forms of silicon dioxide in the solution at a level of 100-110 mg / liter.

The additive has shown good results in feeding quail, geese and piglets, as well as in crop production.

In the patent of the Russian Federation 2528837, 09/20/2014 "Supplement from vegetable raw materials and a method for its production", a silicon-containing additive for food and feed purposes, as well as for fertilizers, including vegetable raw materials and a component selected from the group: soluble sugar and / or baking soda is declared , and / or chelating agent of the catechin type, in an amount up to 40% of the mass. subjected to mechanochemical activation, characterized in that more than 80% of the additives after mechanochemical activation at a temperature not exceeding 88 ° C have a particle size of less than 80 microns. The additive is distinguished by the fact that, as a vegetable raw material, it contains wastes from the production of flour, the production of cereals, including rice husks, buckwheat husks, oat husks, millet, oatmeal.

The additive contains 10 to 100 mg / liter of silicon.

The disadvantage of all the above methods of obtaining products containing humic and accompanying fulvic acids is the complexity and duration of production.

The objective of the invention is to develop a simple and economical method for producing biologically active liquids and biologically active solid additives from plant materials.

The problem is solved by developing a method for producing biologically active liquids and biologically active solid additives from plant materials, which are preliminarily crushed, treated with an aqueous alkaline solution with an initial suspension alkalinity of at least pH 12, suspension moisture content of 85-90 wt%. at a temperature of 35-50 ° C and a processing time of 5-8 hours, then the suspension is separated into liquid and solid parts, the liquid part is pasteurized and the solid part is dried to obtain liquid and solid biologically active products.

The method provides for the possibility of water extraction of the solid part with subsequent separation, while the aqueous solution is returned to the process, and the solid residue is returned to drying and removal from the system.

The output of active substances in a biologically active liquid is changed by the amount of alkali in relation to dry matter of plant origin from 4 to 10% of the mass. for sodium hydroxide, or from 5 to 14% of the mass. for potassium hydroxide, or in proportion to their content in the mixture of alkalis.

Biologically active solid products obtained by the proposed method contain a significant amount of biologically active substances (humic acids, fulvic acids, folate (vitamin B9), water-soluble silicon), can be used as biologically active additives (BAA).

The use in the claimed method of various types of plant raw materials leads to the production of various types of nutrients:

- husk of cedar cones - mainly to increase the yield of humic acids;

- oat husks - mainly to increase the yield of fulvic acids;

- cedar nut shells, or hay of green stalks of wheat and / or rye - mainly to increase the yield of folate (vitamin B9);

- rice husks - mainly to increase the yield of soluble silicon;

- roasted coffee beans - mainly to increase the yield of humic and fulvic acids, and a pleasant coffee smell remains.

Liquid products obtained from various types of plant materials can be mixed in proportions that provide the optimal content of biologically active substances in marketable forms.

Solid products obtained from various types of plant materials can be mixed in proportions that provide the optimal content of biologically active substances in marketable forms - biologically active additives (BAA).

When developing the proposed method for producing biologically active liquids and solid biologically active additives from various types of plant materials, preliminary studies were carried out.

A sunflower husk was used which was ground in two stages to a fine state in a standard flour mill. After grinding, the dry product was treated with an alkali solution at a temperature of 35 ° C, a humidity of 88% of the mass. and pH 11.6.

After holding for 6 hours, the suspension was compressed into liquid and solid parts. The analysis showed that the solution contains 0.07% of the mass. humic acids. The studies were continued at a pH of the solution equal to 12.3. At the same time, there was a sharp change in the color of the suspension to an almost black color, and within 6 hours the pH of the suspension was set at 11.4. Analysis of the liquid part showed a content of humic acids of 0.41%) wt. fulvic acids 0.23% wt. In addition, a significant content of folate (vitamin B9) was determined - 65 mg / liter (daily intake for humans 0.2 mg - Chemical Encyclopedia vol. 5, p. 216, Moscow, 1999 .), as well as soluble silicon 63 mg / liter.

That is, the transition of the suspension alkalinity from pH 11.6 to 12.3 increased the content of humic acids in the solution by 6 times, without resorting to other chemical, biological or cavitation effects.

In addition, a significant amount of folate (vitamin B9) appeared in the solution (animals are not capable of synthesizing folic acid). Folate (vitamin B9) is used in the prevention and treatment of macrocytic anemia, leukopenia, chronic gastroenterocolitis. Additional prophylactic intake of folate (vitamin B9) is useful for women of childbearing age, pregnant and lactating mothers (Chemical Encyclopedia, Vol. 5) and soluble silicon (silicon is classified as a group of elements necessary for normal growth and development of the body of animals and humans).

Studies of this method were continued on other types of agricultural waste. Treatment with an alkaline solution with a pH of 12.47 of the crushed peel of pine cones brought an unexpected result - the solution contained 1.6% of the mass. humic acids, 0.31% of the mass. fulvic acids and 144 mg / liter of folate (vitamin B9) (700 daily norms for humans), as well as 5.8 mg / liter of soluble silicon.

Chopped hay obtained from green mass of a mown mixture of rye and wheat was studied. With alkalinization, at pH 12.1, the solution contained 0.58% of the mass. humic acids, 0.29% of the mass. fulvic acids, 620 mg / liter of folate (natural vitamin B9, more than 3100 daily norms for humans) and 20.4 mg / liter of soluble silicon.

When processing the proposed method of the pine nut shell, an exceptionally high content of folate (natural vitamin B9) of 1475 mg / liter in solution and 3100 mg / kg in a solid product was obtained (7000 and 15000 daily doses for humans, respectively).

When processing oat husks according to the proposed method, a solution was obtained containing 2.52% by weight (25200 mg / liter) of fulvic acids (according to the company "SOLGAR" USA, the daily norm for a person of fulvic acid is 14 mg).

Thus, the studies carried out made it possible to establish that:

- increasing the supply of alkali (a mixture of sodium hydroxide and potassium hydroxide) to the suspension, with 5% of the mass. on dry matter up to 7% of the mass. and up to 7.8% of the mass. led to an increase in the content of humic acids in the solution with 1.6% of the mass. up to 2.27% of the mass. and 2.61%) mass. respectively (Examples 10, 11, 12).

- found a non-obvious phenomenon that in suspensions of plant materials in an alkaline solution with a moisture content of 85-90% of the mass. and a temperature of 35-50 ° C, when the pH exceeds 12, chemical reactions increase sharply, leading, after separation of the suspension after 5-8 hours of exposure into solid and liquid parts, to the appearance in both liquid and solid parts of a high content of biologically active substances - humic acids , fulvic acids, folate (natural vitamin B9), water-soluble silicon (Example 2).

- changing the ratio of alkali to dry matter of plant origin in the composition of the suspension also changes the content of biologically active substances in the final products - liquid solutions and solid products (Examples 9-13).

- with the versatility of the method of processing different types of plant raw materials proposed by this invention, an extreme content of individual biologically active substances in solution (but not limited to), for example, such as fulvic acids from oat husks (2.52% by weight) (Example 23), or folate (vitamin B9) from pine nut shells (1475 mg / l) (Example 13).

- if the individual biologically active liquids obtained by the method according to the present invention are mixed in a certain proportion, then it is possible to obtain final liquids containing the optimal ratio of various biologically active substances (Examples 25, 26).

- if the solid biologically active products obtained by the proposed method, obtained from different types of plant raw materials, are mixed in a certain proportion, then solid biologically active additives (BAA) can be obtained containing the optimal ratio of biologically active substances (Examples 24, 27).

Biologically active solid products obtained by the proposed method contain a significant amount of biologically active substances (humic acids, fulvic acids, folate (natural vitamin B9), water-soluble silicon), can be used as biologically active additives (BAA).

The performed studies and examples (2-27) convincingly prove that the task at hand - to find a simple and economical way to obtain biologically active liquids and biologically active solid additives from plant raw materials, proposed by the invention, is successfully solved.

The proposed method is illustrated by the following examples:

Example 1. (comparative).

The sunflower husk was milled in a flour mill (to about 100 mesh). Then, in a reactor with a stirrer and a heating jacket, the crushed raw material was mixed with an aqueous solution of sodium hydroxide until a moisture content of 88% of the mass was reached. and the pH of the suspension is 11.6. In this case, the content of sodium hydroxide (in terms of 100% by weight) was 3.5% by weight. in relation to the dry matter of raw materials. The exposure was carried out at a temperature of 38 ° C for 6 hours. Then the suspension was separated by pressing.

For the experiment, we took 1.4 kg of sunflower husk with a moisture content of 7% of the mass. 10 liters of water and 45 g of sodium hydroxide in terms of dry matter (3.5% wt. On dry matter of raw materials). The moisture content of the suspension was 88% of the mass. and the pH is 11.6. After separation, 4.9 kg of a solid product with a moisture content of 74.2% of the mass was obtained. and 6.4 liters of liquid containing 0.07% of the mass. humic acids.

Example 2.

Sunflower husk milled according to the conditions of Example 1, in an amount of 1.4 kg (7% by weight of moisture) was mixed with 10 liters of water and 80 grams (in terms of 100% by weight) of sodium hydroxide (6% by weight of dry raw materials) , the suspension had a moisture content of 88% of the mass. and pH 12.3.

After holding for 6 hours at a temperature of 38 ° C, the suspension was separated by pressing. When this received 4.75 kg of solid, moisture content of 74.8% of the mass. and 6.6 liters of liquid.

After pasteurization, the liquid product contained 0.41% of the mass. humic acids, 0.23% of the mass. fulvic acids, 65 mg of folate and 63 mg of silicon per 1 liter of solution.

After drying at a temperature of 80 ° C to a moisture content of 10% of the mass, 1.3 kg of a solid product containing 1.15% of the mass was obtained. humic acids, 0.65% of the mass. fulvic acids, 165 mg / kg folate (vitamin B9) and 150 mg / kg soluble silicon.

The temperature of the experiments was selected empirically, since at temperatures below 35 ° C, the rate of alkalinization dropped sharply (due to a slower decrease in the pH of the suspension and less intense staining of the suspension), and at temperatures above 50 ° C, the solid phase of the suspension swelled strongly, and the yield of liquid phase with a simultaneous increase in the moisture content of the separated solid phase (from 75% wt. to 84% wt.).

Example 3.

The experiment was carried out under the conditions of Example 2, but the holding temperature of the suspension was 35 ° C. After holding for 6 hours, the suspension was separated by pressing.

This gave 4.6 kg of solid with a moisture content of 73% of the mass. and 6.7 liters of liquid. After pasteurization, the liquid product contained 0.35% of the mass. humic acids, 0.17% of the mass. fulvic acids, 47 mg of folate (vitamin B9) and 35 mg of silicon per 1 liter of solution.

Example 4.

The experiment was carried out under the conditions of Example 2, but the holding temperature was 50 ° C. After holding for 6 hours, the suspension was separated by pressing. This received 6.7 kg of solid product with a moisture content of 82% of the mass. and 4.6 liters of a liquid product containing 0.43% of the mass. humic acids and 0.26% of the mass. fulvic acids, folate (vitamin B9) content 61 mg / liter and silicon 65 mg / liter. The suspension was separated worse and the yield of the biologically active liquid decreased to 70% of the mass. from Example 2 with a slight increase in the content of biologically active substances.

Example 5.

The experiment was carried out under the conditions of Example 2, but with a holding time of 5 hours. After separation of the suspension, 4.6 kg of a solid product with a moisture content of 73% of the mass was obtained. and 6.7 liters of liquid product, which after pasteurization contained 0.3 to 8% of the mass. humic acids, 0.19% of the mass. fulvic acids, 51 mg of folate (vitamin B9) and 42 mg of silicon per 1 liter of solution.

Example 6.

The experiment was carried out under the conditions of Example 2, but at the same time the content of solid raw materials in the suspension was reduced to 1.2 kg (moisture 7% wt.) And sodium hydroxide to 70 g (6.3% wt. On dry raw materials), while the moisture was 90% of the mass. pH 12.1.

After holding at a temperature of 38 ° C for 6 hours and separation by pressing, 4.1 kg of a solid product with a moisture content of 73% of the mass was obtained. and 7.2 liters of a liquid product, which, after pasteurization, contained 0.35% by weight of humic acids, 0.18%) by weight. fulvic acids, 49 mg of folate (vitamin B9) and 37 mg of soluble silicon per 1 liter of solution.

That is, despite the increase in the yield of the liquid solution, the content of biologically active substances in the solution has significantly decreased.

Example 7.

The experiment was carried out under the conditions of Example 2, but the holding time was 8 hours. After separation, 4.7 kg of a solid was obtained with a moisture content of 74.5% of the mass. and 6.6 liters of liquid.

After pasteurization, the liquid product contained 0.42% of the mass. humic acids, 0.24%) mass. fulvic acids, 63 mg of folate (vitamin B9) and 65 mg of silicon per 1 liter of solution, that is, the result was almost identical to that obtained in the experiment of Example 2.

Example 8.

The experiment was carried out under the conditions of Example 2, but the content of the crushed raw material in the suspension was increased to 2000 g, and the alkali content of sodium hydroxide to 115 g (6% by weight for dry raw materials). In this case, the moisture content of the suspension was 85% of the mass. and the pH is 12.2. After holding for 6 hours at 38 ° C, 8.1 kg of a solid product with a moisture content of 79% of the mass was obtained by separation. and 3.9 liters of liquid product, which after pasteurization contained 0.48% of the mass. humic acids, 0.25% of the mass. fulvic acids, 73 mg of folate (vitamin B9) and 68 mg of silicon per 1 liter of solution.

A sharp drop in the yield of a liquid solution from 6.6 liters to 3.9 liters was not compensated by a slight increase in the content of biologically active substances in the solution.

Example 9.

It was carried out under the conditions of Example 2, but instead of 80 g of sodium hydroxide, 110 g of potassium hydroxide (8.5% by weight on dry raw materials) were used, the moisture content of the suspension was 88%) by weight. pH 12.6. 4.80 kg of solid was obtained with 74.6 wt% moisture and 6.6 liters of liquid.

After pasteurization, the liquid product contained 0.42% of the mass. humic acid, 0.22% of the mass. fulvic acid, 63 mg of folate (vitamin B9) and 65 mg of silicon per 1 liter of solution. This is almost equivalent to the result obtained in Example 2.

After drying, a solid product was obtained in the amount of 1.3 kg at a moisture content of 7% of the mass. containing 1.2% of the mass. humic acids, 0.7% of the mass. fulvic acids and 180 mg / kg folate (vitamin B9), which made it useful as an additive in animal feed and as a soil improver.

Example 10.

The husk of pine nut cones was used as a vegetable raw material, which remains as a waste after crushing a whole cone to extract the pine nut.

The husks of pine cones were crushed similarly to Example 1.

The reactor was loaded with 1.4 kg of raw materials, 10 l of water, 65 g of a mixture of potassium and sodium hydroxide (50:50), (5 wt% for dry raw materials). The suspension had a moisture content of 88% of the mass. and pH 12.3. After holding for 6 hours at a temperature of 38 ° C, the suspension was separated by pressing. This gave 2.8 kg of solid with a moisture content of 62% of the mass. and 8.4 liters of liquid. After pasteurization, the liquid product contained 1.6% of the mass. humic acid, 0.32% of the mass. fulvic acid and 144 mg / liter of folate (vitamin B9).

After drying to a moisture content of 7% by weight at a temperature of 80 ° C, the solid product (1.1 kg) contained 2.4% by weight. humic acids, 0.5% of the mass. fulvic acids and 210 mg / kg folate (vitamin B9).

Example 11.

Under the conditions of Example 4, the feed of a mixture of sodium hydroxide and potassium hydroxide (50:50) was increased, from 65 g to 90 g (7% by weight on dry raw materials). The suspension had a moisture content of 88% of the mass. and pH 12.4. After holding for 6 hours at a temperature of 38 ° C, the suspension was separated by pressing. Received 2.7 kg of solid, moisture 62% of the mass. and 8.3 liters of liquid.

After pasteurization, the liquid product contained 2.27% of the mass. humic acids and 0.21% by weight of fulvic acids.

After drying to a moisture content of 10% of the mass. the solid product contained 3.5% of the mass. humic acids and 0.3% of the mass. fulvic acids.

Example 12.

Under the conditions of Example 10, the feed of a mixture of sodium hydroxide and potassium hydroxide (50:50) was increased, up to 100 g (7.8% by weight for dry raw materials), the pH of the suspension was 12.8, humidity was 88%).

After holding for 6 hours at a temperature of 38 ° C, the suspension was separated by pressing. When this was received 2.8 kg of solid, moisture 64% of the mass. and 8.1 liters of liquid.

After pasteurization, the liquid product contained 2.61% by weight of humic acids, 0.26% by weight. fulvic acids.

Solid product after drying to 10% of the mass. moisture in the amount of 1.1 kg contained 4.9% of the mass. humic acids and 0.5% of the mass. fulvic acids.

Example 13.

Pine nut shells were used as plant raw materials, which are obtained as a waste in the production of pine nut kernels.

Pine nut shells were crushed in accordance with Example 1.

1.4 kg of raw material (with a moisture content of 7% by weight), 10 l of water and 90 g of a mixture (50:50) of sodium hydroxide and potassium hydroxide (7% of the mass for dry raw materials) were fed into the reactor.

After holding for 6 hours at 38 ° C, the mixture was separated by pressing. The moisture content of the suspension was 88% of the mass. pH 12.5. Received 3.7 kg of a solid product with a moisture content of 69% of the mass. and 7.4 liters of liquid.

After pasteurization, the liquid product contained 0.4% of humic acids, 0.37% of the mass. fulvic acids and a very high concentration of folate (vitamin B9) - 1475 mg / liter.

Solid product after drying to a moisture content of 10% of the mass. in the amount of 1.25 kg contained 0.88% of the mass. humic acids, 0.80% of the mass. fulvic acids and 3100 mg / kg folate (vitamin B9).

Example 14.

In accordance with Example 1, coffee husks were ground.

1.4 kg of crushed raw materials (with a moisture content of 7% wt.), 10 L of water and 90 g of a mixture (50:50) of sodium hydroxide and potassium hydroxide (7% wt. For dry raw materials), pH 12.4 , humidity 88% of the mass.

After holding for 6 hours at a temperature of 38 ° C, the suspension was separated by pressing. Received 4.2 kg of a solid product with a moisture content of 73% of the mass. and 6.9 liters of liquid.

After pasteurization, the liquid product contained 0.57% of the mass. humic acids and 0.52% of the mass. fulvic acids.

After drying to 10% of the mass. moisture received 1.2 kg of a solid product containing 1.3% of the mass. humic acids and 1.2% of the mass. fulvic acids.

Example 15.

Coffee beans (green), dried to 7-8% of the mass. humidity. Milled similarly to Example 1.

The reactor was loaded with 1.4 kg of raw materials, 10 l of water and 90 g of a mixture (50:50) of sodium hydroxide and potassium hydroxide. The suspension had a moisture content of 88% of the mass. and pH 12.4.

After holding for 6 hours at a temperature of 38 ° C, the suspension was separated by pressing. This received 4.2 kg of solid product, moisture 73% of the mass. and 6.9 liters of liquid.

After pasteurization, the liquid product contained 1.19 wt% of humic acids and 0.60 wt%. fulvic acids.

After drying to 10% humidity, 1.2 kg of a solid product was obtained containing 2.8% of the mass. humic acids and 1.4% of the mass. fulvic acids.

Example 16.

Roasted coffee beans were ground as in Example 1.

The reactor was loaded with 1.4 kg of raw materials, 10 l of water and 90 g of a mixture (50:50) of sodium hydroxide and potassium hydroxide. The suspension had a moisture content of 88% of the mass. and pH 12.23.

After holding for 6 hours at a temperature of 40 ° C, the suspension was separated by pressing. This received 4 kg of solid product, moisture content 74% of the mass. and 7.1 liters of liquid.

After pasteurization, the liquid product contained 1.42% of the mass. humic acids and 0.84% of the mass. fulvic acids. At the same time, the liquid, in a diluted form, retained the taste and smell of coffee.

After drying to 8% of the mass. moisture received 1.16 kg of a solid product containing 4.0% of the mass. humic acids and 2.3% of the mass. fulvic acids.

Example 17.

Hay obtained by drying green stalks of rye and wheat crops was milled similarly to Example 1. The reactor was charged with 1.5 kg of raw materials (with a moisture content of 10 wt%), 10 l of water and 70 g of a mixture (50:50), sodium hydroxide and hydroxide potassium (5% wt. dry raw materials). The suspension had a moisture content of 88% of the mass. and pH 12.6.

After holding for 6 hours, the suspension was separated by pressing. When this received 4.9 kg of a solid product with a moisture content of 75.5% of the mass. and 6.3 liters of liquid.

After pasteurization, the liquid product contained 0.42% of the mass. humic acids and 0.07% of the mass. fulvic acids, 20.4 mg of dissolved silicon and a high content of folate (vitamin B9) - 620 mg / liter.

Solid product after drying to 10% of the mass. humidity in the amount of 1.28 kg contained 1.3% of the mass. humic acids, 60 mg / kg of soluble silicon and 1500 mg / kg of folate (vitamin B9).

Example 18.

Similar to Example 11, but the loading of the mixture (50:50), sodium hydroxide and potassium hydroxide was increased to 95 grams (7% by weight on dry raw materials). The suspension had a moisture content of 88% of the mass. and pH 12.7.

After holding for 6 hours at a temperature of 38 ° C, the suspension was separated by pressing. In this case, 4.6 kg of a solid product was obtained, with a moisture content of 75.5% of the mass. and 6.6 liters of liquid.

After pasteurization, the liquid product contained 1.0% of the mass. humic acids and 0.65% of the mass. fulvic acids, 27 mg / liter of silicon and 570 mg / liter of folate (vitamin B9).

After drying to 10% of the mass. moisture received 1.2 kg of a solid product containing 2.5% of the mass. humic acids, 1.6% of the mass. fulvic acids and 1270 mg / kg folate (vitamin B9).

Example 19.

Green oat hay was deeply dried and milled, similar to Example 1.

The reactor was loaded with 1.5 kg of raw materials. 10 l of water and 70 g of a mixture (50:50) of sodium hydroxide and potassium hydroxide (5% by weight for dry raw materials). The suspension had a moisture content of 88% of the mass. and pH 12.6.

After holding for 6 hours at a temperature of 38 ° C, the suspension was separated by pressing. When this received 4.7 kg of solid product, moisture content of 74.5% of the mass. and 6.5 liters of liquid.

After pasteurization, the liquid product contained 0.5% of the mass. humic acids and 0.27% of the mass. fulvic acids.

After drying to 10% of the mass. moisture received 1.25 kg of a solid product containing 1.2% of the mass. humic acids and 0.6% of the mass. fulvic acids.

Example 20.

Similar to Example 13, but the loading of a mixture (50:50) of sodium hydroxide and potassium hydroxide is increased to 105 grams (7.8% by weight on dry raw materials). The suspension had a moisture content of 88% of the mass. and pH 12.4. After holding for 6 hours at 38 ° C, the mixture was separated by pressing.

This received 4.5 kg of solid product, moisture content 74.5% of the mass. and 6.6 liters of liquid. The liquid product after pasteurization contained 0.82% of the mass. humic acids and 0.51% of the mass. fulvic acids.

After drying to 10% of the mass. moisture received 1.2 kg of a solid product containing 1.9% of the mass. humic acids and 1.2% of the mass. fulvic acids.

Example 21.

Buckwheat husk was ground similarly to Example 1.

The reactor was loaded with 1.4 kg of crushed buckwheat husk (moisture 7% wt.), 10 L of water and 90 g of a mixture (50:50) of sodium hydroxide and potassium hydroxide, (7% wt. On dry raw materials). The suspension had a moisture content of 88 wt% and a pH of 12.3.

After holding for 6 hours at 38 ° C, the mixture was separated by pressing. When this received 4.9 kg of solid product, moisture content of 75.2% of the mass. and 6.2 liters of liquid.

The liquid product after pasteurization contained 0.25% of the mass. humic acids, 0.38% of the mass. fulvic acids and 143 mg / liter of dissolved silicon.

After drying to 10% of the mass. moisture received 1.3 kg of a solid product containing 0.6% of the mass. humic acids, 0.9% of the mass. fulvic acids and 300 mg / kg of soluble silicon.

Example 22.

Oat husks are crushed similarly to Example 1.

The reactor was loaded with 1.4 kg of crushed raw materials, 10 l of water and 90 g of a mixture (50:50) of sodium hydroxide and potassium hydroxide (7% of the mass. On dry raw materials). The initial moisture content of the suspension was 88% of the mass. and pH 12.3.

After holding for 6 hours at 38 ° C, the mixture was separated by pressing. When this received 4.9 kg of solid product, moisture content of 75.4% of the mass. and

6.2 liters of liquid

The liquid product after pasteurization contained 0.15% of the mass. humic acids, 0.33% of the mass. fulvic acids and 148 mg of dissolved silicon.

After drying to 10% of the mass. moisture received 1.25 kg of a solid product containing 0.35% of the mass. humic acids and 0.75% of the mass. fulvic acids.

Example 23.

Oat husks were crushed similarly to Example 1.

The reactor was loaded with 1.60 kg of raw materials (moisture 7% wt.), 10 l of water and 210 g of potassium hydroxide (14% of the mass on dry raw materials). The suspension had a moisture content of 86.9% and a pH of 12.9.

After holding for 6 hours at a temperature of 40 ° C, the mixture was separated by pressing. When this received 5.1 kg of solid product, moisture content of 74.9% of the mass. and 6.3 liters of liquid.

The liquid product after pasteurization contained 0.12% of the mass. humic acids, 2.52% by weight of fulvic acids and 160 mg of dissolved silicon.

After drying to 10% of the mass. moisture received 1.4 kg of a solid product containing 0.31% of the mass. humic acids, 5.9% of the mass. fulvic acids, 410 mg / kg of soluble silicon.

Example 24.

The solid product obtained under the conditions of Example 12 was not dried, but extracted with 10 liters of water, squeezed out by pressing. This gave 2.6 kg of solid product, moisture content 65% of the mass. and 10.1 liters of liquid containing 0.45% of the mass. humic acids. The liquid was used to create a slurry under the conditions of Example 12.

2.8 kg of solid and 8.2 liters of liquid were obtained. The liquid product after pasteurization contained 2.9% of the mass. humic acids.

After drying to 10% of the mass. moisture received 1.0 kg of a solid product containing 0.75% of the mass. humic acids.

Example 25.

The liquid products obtained in Examples 12 and 13 were mixed in a 90:10 ratio. This received a liquid containing 2.44% of the mass. humic acids and 147.5 mg / l of folate (vitamin B9). Thus, 1 liter of the resulting solution contained 368 daily doses of vitamin B9 (at a rate of 0.4 mg) and 349 doses of humic acids (at a daily rate of 70 mg), and was actually balanced for use.

Example 26.

The liquid products obtained in Examples 13 and 22 were mixed in a ratio of 1:99. At the same time, a liquid was obtained containing 14.75 mg / l of folate (vitamin B9) and 822 mg / l of dissolved silicon, which corresponded to 36.9 and 41 daily doses for humans and was an almost balanced solution.

Example 27.

The solid products obtained under the conditions of Examples 12 and 13 were mixed in a ratio of 92: 8 to obtain a mixed product containing 4.7% of the mass. humic acids and 248 mg / kg folate (vitamin B9), which corresponded to 670 and 620 daily doses for humans and was practically balanced in terms of active substances (BAA).

Claims (9)

1. A method of obtaining biologically active products in liquid and solid form, containing humic acids, fulvic acids, folate and soluble silicon, from plant materials, which are preliminarily crushed to a particle size passing through a 100 mesh sieve, treated with an aqueous alkaline solution of sodium hydroxide and / or potassium hydroxide to form a suspension, with an initial alkalinity of the suspension of at least pH 12, a moisture content of the suspension of 85-90% by weight, the amount of alkali in relation to dry matter of plant origin, which ranges from 4% of the mass. up to 10% of the mass. for sodium hydroxide, or from 5% of the mass. up to 14% of the mass. for potassium hydroxide, or in proportion to their content in a mixture of alkalis, at a temperature of 35-50 ° C and a processing time of 5-8 hours, which provides a complex chemical and extractive effect on plant raw materials, then the suspension is separated into liquid and solid parts, liquid is pasteurized parts and drying of the solid part, to a moisture content of 10% of the mass. with obtaining liquid and solid biologically active products. 2. The method according to claim 1, characterized in that the solid part is subjected to extraction with water followed by separation, while the aqueous solution is returned to the process, and the solid residue is dried and removed from the system. 3. The method according to claim 1, characterized in that the husk of cedar cones is used as the plant material. 4. The method according to claim 1, characterized in that oat husk is used as plant material. 5. The method according to claim 1, characterized in that the cedar nut shells or hay of green stalks of wheat and / or rye are used as plant raw materials. 6. The method according to claim 1, characterized in that rice husk is used as plant material. 7. The method according to claim 1, characterized in that roasted coffee beans are used as plant raw materials. 8. A method according to claim 1, characterized in that liquid products obtained from various types of plant raw materials are mixed in proportions that provide the optimal content of biologically active substances in marketable forms. 9. The method according to claim 1, characterized in that the solid products obtained from various types of plant raw materials are mixed in proportions that provide the optimal content of biologically active substances in marketable forms.