Silicon-humus soil ameliorant

FIELD: chemistry.

SUBSTANCE: invention relates to environmental conservation technologies, cutting-edge agricultural technologies and chemistry of organosilicon compounds and can be used to restore the structure of disturbed soils by stabilising water-stable aggregate. In particular, the present invention employs water-soluble humic silanol derivatives that are modified in a special way to endow them with the capacity to be irreversibly sorbed on surfaces of mineral particles and other hydroxyl-containing carriers. Humic derivatives are added to the degraded soil in form of aqueous solutions.

EFFECT: method for use in agricultural technologies includes using humic derivatives as structure-forming agents (soil ameliorants) by via attachment thereof to the surface of soil aggregates in order to endow the latter with water-stable properties.

8 cl, 11 dwg, 8 tbl

 

The technical field to which the invention relates.

The invention relates to the field of environmental technology, advanced agricultural technologies and chemistry of organosilicon compounds and can be used to restore the structure of damaged soils by stabilization of water-stable aggregates. In particular, the invention uses a water-soluble humic silanol derivatives that have been modified in a special way, to give them the ability to irreversibly absorb on the surfaces of mineral particles and other hydroxyl-containing media. The method of application in agro-technology is the use of humic derivatives as structure-formers (soil improver) by attaching to the surfaces of soil aggregates in order to give the last water stable properties. Make a humic derivative in a degraded soil in the form of aqueous solutions.

The level of technology

Soil degradation is a significant threat to the environment. This is due to the accelerated decomposition of organic carbon obstructing soils and, consequently, with the increase in carbon dioxide emissions from soils. The main factor preventing the decomposition of organic matter in soils, is the formation of water stable aggregates [Mayer L.M., Schick LL., Hardy, K.R., Wagai, R., McCarthy J. 2004 Organic matter in small mesopores in sediments and soils. Geochimica et Cosmochimica Acta, 68, 3863-3872]. Therefore, with increasing anthropogenic pressures from native to tilled soil in them is sharply reduced as the amount of water stable aggregates and organic matter content [Six, J., Elliott E.T., Paustian K., Doran J.W. 1998. Aggregation and soil organic matter accumulation in cultivated and native grassland soils. Soil Sci. Soc. Am. J. 62, 1367-1377]. Until recently it was believed that the main mechanism for the formation of water stable aggregates is gluing mineral particles bridge the connections formed by the interaction of the carboxyl groups of humic components of soil organic matter and metal ions in the composition of the mineral complex [Varadachari, C., ..Mondal, D.C.Nayak, and K.Gosh. 1994. Clay-humus complexation: Effect of pH and the nature of bonding. Soil Biol. Biochem. 26, 1145-1149]. At the same time, recent studies show the leading role of hydrophobic interactions in this process, due to the unique properties of humic films attached on the surface of finely dispersed mineral particles to stick together these particles in aggregates [Shein E.V., milanovsky EJ 2003, the Role and importance of organic matter in the formation and stability of soil aggregates. Pochvovedenie, No. 1, 53-61, Goebel, M.O., S.K. Woche, J. Bachmann, A. Lamparter, W.R. Fischer. 2007. Significance of wettability-induced microscopic changes in water distribution for soil organic matter decomposition. Soil Sci. Soc. Am. J. 71: 1593-1599].

The analogue of the m of the proposed development can be considered as a way to restore vodoprochnost soil aggregates, described [Piccolo, A., and J.S.C. Mbagwu. 1999. Role of considered are hydrophobic components of soil organic matter in soil aggregate stability. Soil Sci. Soc. Am. J. 63: 1801-1810]. The authors studied the effect of hydrophilic and hydrophobic components of soil organic matter on the formation of water stable aggregates and found the maximum increase their quantity in the soil, which had consistently contributed humic acid coal and vysokoshirotnoy stearic acid. Another analogue, which is selected as a prototype, is a method of conditioning soils described in U.S. patent (US 5248327), which consists in introducing in degraded soil-based product coal. This product is oxyquinoline acid or their salts, the special feature of which is the ability to form gels upon swelling in water. Thus both of these methods involve making salts of humic acids from coal, the effect of which is increased either by combining with a hydrophobic polymer (stearic acid), or by modification of coal, from which then produce humic acid. The drawback of the proposed methods is that both products are water soluble humates, which are quickly leached from the soil layer. This determines the fragility of the recovery effect of vodoprochnost soil aggregates.

Specified under Titkov deprived gramnegative derivatives, proposed for use as a soil improver with the broken structure. Their advantage is that they have a high adhesive ability with respect to hydroxyl-containing surfaces, contributing to the formation of hydrophobic humic films. Surfaces has an important role for the formation of water stable aggregates in the soil (Piccolo, A., and J.S.C. Mbagwu. 1999. Role of considered are hydrophobic components of soil organic matter in soil aggregate stability. Soil Sci. Soc. Am. J. 63: 1801-1810). This allows to consider the proposed humic derivatives as reagents for the new generation, with great potential for practical application in conservation, and advanced agricultural technologies. An important advantage of humic derivatives is to long life in the soil conditions, the security positions of secondary pollution and biocompatibility.

Disclosure of inventions

The claimed solution belongs to a class of new compounds, namely humic silanol derivatives that are modified so that they gained the ability to strongly absorb on hydroxyl-containing solid surfaces, causing them to partially hydrophobic, and can be used both in dissolved and immobilized form.

Accordingly, the subject invention are themselves new humic silanol p is osvitnye, and ways of handling their surfaces natural minerals, aimed at increasing vodoprochnost soil aggregates and improving the structure of degraded soils.

Another object of the present invention are humic silanol derivatives to improve the structure of soils that have the ability to strongly absorb hydroxyl-containing solid surfaces due to the formation of siloxane bonds, which contributes to the formation of humic coatings and, accordingly, provides an increase in the hydrophobicity of the treated surfaces.

Another object of this invention is the method of synthesis of humic silanol derivatives, enabling such humic derivatives, using which it is possible to realize improvement of soil quality.

It was unexpectedly found that treatment of humic substances by aminoalkylsilane in the aqueous medium, followed by distillation of water and heating of the product leads to the production of silanol humic derivatives, which are soluble in alkaline aqueous media, but are easily transferred from solution to the solid phase in contact with a solid media containing hydroxyl groups on the surface. Thus formed humic silanol derivative capable of firmly contact gidroksilirovanii the surface of a solid is oblozhki due to the formation of Si-O-Si siloxane bonds (in the case of silicon-containing substrates of the type of silica, silicates, aluminosilicates and the like) and Si-O-M (where M is a metal) bonds in the case of oxides and hydroxides of metals. This allows the use of silanol humic derivatives as soluble reagents to increase vodoprochnost soil aggregates and improve soil structure. In the case of soil, humic silanol derivatives are fixed in the soil, hydrophobicity the surface of mineral particles due to the formation of organic films, and contribute to their bonding in water-stable aggregates.

Another advantage of the application of humic derivatives as soil ameliorants is the availability of cheap and abundant humic materials necessary for obtaining humic derivatives mentioned in this invention. Such raw materials include various types of coal, peat, sapropel, oil shale, called natural, as well as composting, vermicomposting and other similar materials. The original humic substances can be used both in the protonated form (humic and fulvic acids)and salts (humates and fulvates) and as pre-modified derivatives enriched with various functional groups. Can also be used products of microbial decomposition of lignin, wood, coal, and other microbial products with the of NASA, as well as lignosulfonates and other oxidized materials. Taking into account that humic substances do not have a constant stoichiometric composition and regular patterns, they are characterized by a content of main constitutional elements. Under such a we understand that unmodified HS consist of compounds with the following content elements: from about 20 to about 70.% (mass.) With from about 2 to about 10% (mass.) N, from about 15 to about 55% (mass.) Oh, from about 0 to about 10% (mass.) N, and can contain from about 0 to about 10% (mass.) S, and from about 0 to about 50% (wt.) ash. In addition, these compounds may contain from about 1 to about 15 mmol/g of carboxyl groups, from about 1 to about 10 mmol/g of hydroxyl groups and from about 0.5 to about 10 mmol/g of carbonyl groups. For the preparation of humic derivatives of the present invention can be used aminoalkylsilane with different substituents in the aliphatic chain and alkoxysilane the substituents at the silicon atom which can react with carboxyl groups of humic substances. Under aminoalkylsilane we understand alkoxysilane that have one amino group separated from the Si atom, at least one, but preferably three methylene groups and at least one, but preferably three, alkoxy substituents.

Up to the present is the time the possibility of obtaining soluble humic derivatives, capable of spontaneously absorb on mineral surfaces is described only in the patent RU 2429068. The principal distinction of this invention is that humic silanol derivative gain in the aquatic environment, whereas the synthesis described previously alkoxysilyl derivatives of lead in the environment anhydrous organic solvent (such as DMF). Another fundamental difference is that the dissolution alkoxysilylated humic derivatives in aqueous medium followed by hydrolysis alkoxysilyl groups and the allocation of aliphatic alcohols, polluting the environment. This disadvantage is missing silanol derivative of the present invention, soluble in water without the formation of by-products. In addition, alkoxysilane derivatives will usually contain residual amounts of solvent (e.g., DMSO)that is also associated with the risk of secondary pollution. Synthesis of silanol derivatives of the present invention is carried out in water, which allows you to resolve this issue.

It was unexpectedly found that the introduction of silanol groups in the humic macromolecules does not lead to the formation of insoluble humic polymers, crosslinked siloxane bonds. In contrast, humic silanol derivatives are highly soluble in aqueous media in the field of alkaline pH, but which may easily be removed from solution by contact with solid substrates, containing a hydroxyl group on the surface. The process of immobilization of humic derivatives on inorganic surfaces occurs due to the reaction of silanol groups with the hydroxyl with the formation of covalent Si-O-Si or Si-O-M bonds (where M is a metal). Thus silanol groups act as linkers between humic film and solid substrate. The advantage of the formation of humic films on mineral surfaces is hydrophobic in nature, which ensures the bonding of the modified particles in water stable aggregates.

The scope of the invention is the recovery of vodoprochnost soil aggregates and improve soil structure by adding solutions of humic silanol derivatives with subsequent tillage treated layer of soil. Introduction humic derivatives is done by drip irrigation or a mixture of liquid and complex fertilizers. Sorption of humic derivatives on mineral components of degraded soils provides bonding in water-stable aggregates and, consequently, allows you to restore soil structure.

To obtain spontaneously adsorbed humic derivatives according to the method proposed in the present invention, the humic preparation, which can be used humic acid, or is of univocality in protonated form or in the form of salts of alkali metals, as well as dissolved organic matter and humanophobia oxidation products of lignin, dissolved in water and the resulting solution was added dropwise aminoethanol (for example, 3-aminopropyltrimethoxysilane APTS), or 3-aminopropyltriethoxysilane APTS), or 1-aminohexanoate 6-aminomethylenemalonate AGTS)). Next bring the pH of the solution to 3-7 with mineral acid (such as HCl). Then the water is evaporated and the reaction product is placed in a drying Cabinet at 30-150°C for 6-8 hours, the resulting product can be defined as silanol humic derivatives. They differ from the original GW as its physicochemical properties, and elemental and functional composition. Silanol humic derivatives containing from 2 to 10 mmol/g of silanol groups and have elemental composition (% mass.): Si 2-8; 30-55, N. 3-5 and N is 2-5. Some recipes humic derivatives may contain sulfur in the range from about 0.5 to about 5% (wt.). They can be dissolved in water and irreversibly immobilized on mineral and other hydroxyl-containing solid substrates.

Brief description of drawings

Figure 1 - IR spectra of humic substances and modified drug GW-APTS.

Figure 213C NMR spectra of drugs GW of leonardite and silanol derivative of GW-APTS.

Figure 3 - IR spectra of humic substances and coal silanol derivative of GW-AGTS.

4 is a13 C NMR spectra of preparations of HS and HS-AGTS.

5 - IR spectra of humic substances from peat (PHA-Na) and modified RNA preparation was APTS.

6 is a micrograph of a drop of water in different glasses; (A) APTS-modified glass; (C) original glass; (C) glass modified drug GW-APTS.

Fig.7 - image of the original glass (left) and modified HS-APTS (right)obtained using atomic force microscopy (AFM).

Fig assessment vodoprochnost soil aggregates treated with humic silanol derivatives. Left - soil units before the experiment, on the right is the final stage of the experiment.

Fig.9 - kinetic dependence of the number of soil aggregates disintegrated under the action of water, subject to their pre-treatment water, the source potassium HUMATE and drug GW-APTS.

Figure 10 - the formation of water-stable aggregates of soil particles with a size of <0.25 mm under the influence of humic silanol derivatives (HS-APTS).

11 - effect of GW coal and silanol derivatives (HS-APTS) on the content of agronomically valuable aggregates in the soil.

The implementation of the invention

The invention consists in obtaining water-soluble humic silanol derivatives capable of irreversibly absorb on the solid matrix, which becomes partially hydro is one of the properties. For this humic substances modify aminoalkylsilane in the aquatic environment. Introduced in the structure of humic substances silanol groups can react with hydroxyl groups on the surface of a solid substrate, forming a covalent Si-O-Si and Si-O-M connection.

Any known or humic humanophobia substances can be used in the invention. It can be various coals, peat, sapropel, composts and other These substances or their modifications can be used both in protonated form and in the form of salts. Moreover, addition of humic substances, other humanophobia substances can be used in the invention: compost and vermicompost, and other materials containing organic component with carboxyl groups (products of biological degradation of lignin, wood, coal, and others). Because humic substances do not have a specific chemical structure, they characterize the content of major elements. Thus, here, under the humic substances include compounds containing from 20 to 70 weight % of carbon, from 2 to 10 weight % of hydrogen, from 15 to 55 weight % of oxygen, from 0 to 10 weight % of nitrogen and from 0 to 50 weight % of ash. Sometimes humic substances contain from 0 to 10 weight % of sulfur.

Solid surface for sorption silanol derivatives of humic substances described izobretenii, must contain a hydroxyl group. Under this definition: silica gel, sand, quartz, silicates, aluminosilicates, alumina, aluminum, calcite, inorganic oxides (Al2O3, FexOy, TiO2, Cr2O3and others), glass, asbestos, granular medium (gravel) and other similar materials.

As noted, the modification of humic substances can be produced using aminoalkylsilanes. The main types organosilanes that can be used for these purposes are shown in table 1. Under alkoxysilyl groups refers to groups containing from 1 to 20 carbon atoms. The present invention describes the use of methoxy, ethoxy derivatives due to their higher ability to hydrolysis and, consequently, a higher reactivity with respect to the surfaces containing hydroxyl groups. In the framework of this invention can be used aminoalkylsilane containing one, two or three alkoxysilyl group, or their mixture. As such organosilanes can be used as follows:

3-aminopropyltrimethoxysilane, 3-aminopropyltrimethoxysilane,

3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane,

3-aminopropyltriethoxysilane, 3-aminopropyltriethoxysilane,

1-aminohexanoate 6-am is nautilusdirectory,

1-aminohexanoate 6-aminomethylenemalonate and other

It is preferable to use tralkoxydim, as in this case, the modified humic substances contain three reactive of alkoxygroup that leads to more effective interaction with the hydroxyl-containing surfaces. However, this invention does not preclude the use of mono and di-alkoxysilane for modification of humic substances.

It was unexpectedly found that after treatment of humic substances by aminoalkylsilane in water, acidified to a pH of 3-7, and subsequent heating of the product at 30-150°C for 6-8 hours or longer derived humic derivatives, which are able to dissolve in alkaline solutions, which allows them to be used as macromolecular similitude agents. Silanol derivative of humic substances have not been previously described. Silanol humic derivatives differ significantly from the original on elemental and functional composition, but also by the ability to irreversibly absorb mineral-HE - and-O-containing surfaces. Differences in the composition and the properties of the original and modified humic substances have been demonstrated using various physico-chemical methods such as elemental analysis, titrimetry, IR - and NMR-spectroscopy.

Table 1
Organosilane, which can be used for modification of humic substances
FunctionalityNameStructure
Amino3-aminopropyltriethoxysilane APTS)H2N(CH2)3SiRn(OR)3-n,
where n=0-2, R is methyl or ethyl radical
Amino1-aminohexanoate 6-aminomethylenemalonate AGTS)H2N(CH2)6NHCH23SiRn(OR)3-n,
where n=0-2, R is methyl or ethyl radical

Silanol humic derivatives are characterized by the following composition and properties. Their elemental composition satisfies the following intervals (%): Si 2-8, 30-55, N 3-7 and N is 2-8. They contain from 0.5 to 5 mmol silanol groups per 1 g of humic substances depending on the degree of modification of functional groups of humic substances. They can be dissolved in alkaline solution and irreversibly sorbed on the OH-containing solid substrates.

Cooking silanols the x derivative of humic substances produced by the following method:

1. The original solid HW homogenized.

2. Homogenized humic substances dissolved in aqueous alkali and the resulting solution make dropwise a solution of mineral acid (such as HCl) to establish a pH 3-7

3. Then dropwise with constant stirring add aminoalkylsilane to achieve a molar ratio of functional groups of the reactants (organosilane : GW) from 0.1:1 to 2:1. The reaction is carried out at room temperature for 1 hour.

4. The reaction product is separated from the water using a rotary evaporator.

5. The resulting material is heated in a vacuum furnace at a temperature of 30-150°C for 6-8 hours or longer.

The authors it was found that the resulting silanol humic derivatives can be used to produce films on hydroxyl-containing surfaces. These films obtained using the following techniques:

1. Solid humic derivatives obtained by the above method, homogenized and mixed with a concentrated solution of alkali (from 1 to 50%) in a volume ratio from 1:1 to 1:5.

2. The alkaline solution of humic derivatives were diluted with distilled water to a concentration of from 0.01 to 10%, and (if necessary) is acidified to a pH of 5-7.

3. The resulting solution is used for treatment of hydroxyl-containing surfaces.

Received silanol si the new derivatives can be used to increase vodoprochnost soil aggregates and improve the structure of degraded soils. This effect is achieved using the following methods.

1. Solid humic derivatives obtained by the above method, homogenized and mixed with a concentrated solution of alkali (from 1 to 50%) in a volume ratio from 1:1 to 1:5.

2. The alkaline solution of humic derivatives were diluted with distilled water to a concentration of from 0.1 to 10%, and (if necessary) is acidified to a pH of 5-7.

3. The resulting solution was used for inclusion in the degraded soil through drip irrigation or watering both separately and in conjunction with the introduction of a comprehensive and liquid fertilizers.

The invention is illustrated by examples (but not limited).

Examples 1-3 describe the synthesis of silanol humic derivatives. The composition and structure of the obtained derivatives were confirmed by the methods of elemental analysis, titrimetry, IR and13C NMR spectroscopy. The results of elemental and functional composition are presented in tables 2-7, IR and13C NMR spectra are given in figure 1-4. Example 4 describes the properties of surface-modified humic silanol derivatives, in particular its hydrophobicity. Examples 5-6 show an increase in vodoprochnost soil aggregates as a result of processing silanol derivatives. Example 7 describes an improvement in the structure of soils treated with humic who lanoline derivatives.

Example 1

This example describes the synthesis of silanol derivatives of humic substances using aminoalkylsilane and humic substances leonardite in the form of potassium HUMATE. The reaction was carried out in odnogolosy flask equipped with a mixer. A portion of 50 g of potassium HUMATE was dissolved in distilled water and then, with vigorous stirring, bury 15 ml 3-aminopropyltriethoxysilane APTS). This molar ratio of reactants is 1:0.5 to as 1 g used GW contains 2.7 mmol carboxylic groups, which react with APTS; 1 ml of APTS contains 4.2 mmol of amino groups. Next, to the solution was dropwise introduced 28 ml of hydrochloric acid (5M) to establish a pH of 4. The reaction was performed for 10 minutes at room temperature. After completion of the reaction water was off on a rotary evaporator and the compound obtained was placed in a drying Cabinet at a temperature of 125°C for 6 hours. Then the compound obtained homogenized and placed in a desiccator. Weight of the obtained compound was 56.2,

The structure of the silanol derivative was confirmed by the methods of elemental analysis and titrimetry (results are presented in tables 2 and 3), and by IR and13C NMR spectroscopy. Spectra are given in figure 1 and 2.

td align="center" namest="c0" nameend="c4"> The elemental composition of the original and modified GW per ashless sample (%)
Table 2
SampleNNSi
GW of leonardite52,65,12,16,3
GW-APTS55,56,14,48,4

Table 3
The content of carboxyl groups in the original and modified HS (mol/g)
Sample-COOH Cave±ΔC
GW of leonardite2,7±0,2
GW-APTS1,7±0,5
*Δ - confidence interval, n=3, P=0.95.

From the results of elemental analysis should increase the content of nitrogen and silicon in the modified drugs. From titrimetric data should decrease the content of carboxyl groups in modificarea the different drugs. These changes confirm the high degree of modification of carboxyl groups in the original GW.

It was found that GW of leonardite modified with APTS may contain from 2 to 10% of Si, from 30 to 55%, from 3% to 5% N 2% to 5% N. they can Also react with hydroxyl-containing surfaces, forming a covalent bond Si-O-Si or Si-O-M, where M is a metal surface containing hydroxyl groups.

Figure 1 shows the IR spectrum of the preparation of the original GW. The presence of bands of fluctuation relations C=C aromatic ring (about 1610 cm-1in the IR spectrum of pure drug GW of leonardite indicates the presence of aromatic skeleton part. The band around 1710 cm-1refers to fluctuations due to C=O and confirms the presence of carboxyl and carbonyl groups in the product band in the region of 1250 cm-1refers to the stretching vibrations of C-O phenolic and carboxylic groups, band in the range of 1050-1150 cm-1correspond to fluctuations due to C-O alcohol groups. The presence of these bands indicates the presence of different oxygen-containing functional groups in drugs GW.

In the spectra of modified drugs are present as bands that are characteristic of humic substances, and modifier. Figure 1 shows that in the preparation of HS-APTS in addition to the superposition of GW and APTS (two strong bands at e 1050 cm -1characteristic of Si-O vibrations) there is a band at 1265 cm-1that characteristic oscillations in the plane of the amide bond (amide band 3), which indicates the formation of amide linkages. This is confirmed by the shift of the broad band at 1600 cm-1in the short wavelength region, which indicates an increase of the contribution of the carbonyl vibrations of the atoms in the structure of amides in this peak.

According to NMR spectroscopy on nuclei13C in the original GW were allocated to the following main types of carbon, depending on its chemical environment: 220-185 ppm - carbonyl carbon (CC=O); 185-165 ppm - carboxyl carbon (CCOOH); 165-140 ppm (aromatic carbon linked to oxygen (CArO); 140-100 ppm is unsubstituted or C-substituted aromatic carbon (CAr); 100-50 ppm - aliphatic carbon bound to oxygen (CAlkO); 50-3 ppm - carbon alkyl groups (CAlk). In the spectrum of the drug GW-APTS you can make the following assignment of the peaks 11.1 ppm, 26.8 43.8 ppm and ppm - carbon, through appropriate chain in the structure of the modifier. It should be noted that the spectra of the modified GW peak appears at 167-168 ppm, characteristic of carbon amide bond, and decreases the intensity of the peak at 175 ppm, characteristic of the carboxyl groups. These changes in the spectra indicate the responsive is the research Institute of the amidation reaction.

Example 2

This example illustrates the possibility of using as aminoalkylsilane 1-aminohexanoate 6-aminomethylenemalonate AGTS). The reaction was carried out in odnogolosy flask equipped with a mixer. A portion of 5 g of potassium HUMATE, isolated from coal, was dissolved in distilled water and then, with vigorous stirring, bury 4,2 ml of 1-aminohexanoate 6-aminomethyltransferase AGTS). This molar ratio of reactants is 1:1, as 1 g used GW contains 2.7 mmol carboxylic groups, which react with AGTS; 1 ml of ARTS contains 3.3 mmol of amino groups. Next, to the solution was dropwise introduced 5 ml of hydrochloric acid (5 M) to establish a pH of 4. After adding the acid in the flask was brought to 100 μl of PMS-300 as antifoam. The reaction was performed for 10 minutes at room temperature. After completion of the reaction water was off on a rotary evaporator and the compound obtained was placed in a drying Cabinet at a temperature of 125°C for 6 hours. Then the compound obtained homogenized and placed in a desiccator. Weight of the obtained compound was 7.4, the structure of the obtained substance was proven methods of elemental analysis and titration (table. 4 and 5), and also by the method of IR-spectroscopy and13C NMR spectroscopy (Figure 3 and 4).

Table 4
Elemental composition (ash-free sample) (% wt.) source drug GW and ITS-derived HS
SampleNNSi
The potassium salt of humic substances of leonardite52,65,12,16,3
GW-ARTS53,57,17,68,8

Table 5
The content of acid groups in the source and ITS-derived humic substances (mmol/g)
Sample-COOH Cave±ΔC
GW of leonardite2,7±0,2
GW-ARTS2,5±0,5
*ΔC - confidence interval (mmol/g), n=3, P=0.95

From the data of elemental analysis follows the increase of the content of silicon and nitrogen in the modified product. The titer of the metric data show a decrease in the content of carboxyl groups, as evidenced by the fact that they have entered into reaction with AGTS.

Figure 3 shows the IR spectra of the original GW and silanol derivatives of HS obtained when used as a modifier of AGTS. In the spectrum of HS-ARTS in addition to the bands obtained by superposition, we can note the presence of the bands at 1690 cm-1which is characteristic for C=O in amide linkages, as well as the band at 1268 cm-1characteristic of amides.

For13C NMR spectrum of the drug GW-ITS-100 (figure 4) peaks 26.1 ppm, 26.8 ppm, 31.4 ppm, 34.5 ppm, 40.5 ppm, 50.4 ppm refer to the carbon atoms of aliphatic chains in the composition of the modifier. In addition, the spectra of the modified GW peak appears at 167-168 ppm, characteristic of carbon amide bond, and decreases the intensity of the peak at 175 ppm, characteristic of the carboxyl groups. Thus, NMR and IR spectroscopy it was shown that the addition of aminoguanidine ITS to humic frame is formed by an amide bond.

Example 3

This example demonstrates the possibility of applying for modification of humic substances extracted from peat raw materials. For the reaction used nefrackzionirovannam humic substances isolated from lowland peat. The reaction was carried out in odnogolosy flask equipped with a mixer. A portion of 5 g of sodium HUMATE was dissolved in 100 ml of distilled water and then, the ri vigorous stirring, was bury 3.5 ml of 3-aminopropyltriethoxysilane APTS). This molar ratio of reactants is 1:1, as 1 g used GW contains 3.0 mmol carboxylic groups, which react with APTS; 1 ml of APTS contains 4.2 mmol of amino groups. The reaction was performed for 10 minutes at room temperature. Next, to the solution was dropwise introduced 5 ml of hydrochloric acid (5 M) to establish a pH of 4. After adding the acid in the flask was brought to 100 μl of PMS-300 as antifoam. After completion of the reaction water and hydrolyzed alcohol drove on a rotary evaporator and the compound obtained was placed in a drying Cabinet (120-150°C, 760 mm Hg). Then the compound obtained homogenized and placed in a desiccator. Weight of the obtained compound was 6.3, the structure of the obtained substance was proven methods of elemental analysis and titration (table. 6 and 7), as well as the method of IR spectroscopy (figure 5).

td align="left"> 49,5
Table 6
The elemental composition in the calculation of the ash-free sample (% wt.) source drugs PHA-Na and silanol derivatives
SampleNNSi
PHA-Naa 4.93,70,6
RNA was APTS51,16,27,05,5

Table 7
The content of acid groups in the silanol derivative PHA-Na (mmol/g)
Sample-COOH Cave±ΔC
PHA-Na2,9±0,2
RNA was APTS1,7±0,5
*ΔC - confidence interval (mmol/g), n=3, P=0.95

From the results of elemental analysis should increase the content of nitrogen and silicon in the modified drugs. From titrimetric data should decrease the content of carboxyl groups in the modified drugs. These changes confirm the high degree of modification of carboxyl groups in the initial PHA-Na.

It was found that humic substances from peat modified with APTS may contain from 2 to 8% of Si, from 30 to 55%, from 3% to 5% N 2% to 5% N. they can Also react with hydroxyl-containing surfaces is, forming covalent bonds Si-O-Si or Si-O-M, where M is a metal surface containing hydroxyl groups.

Figure 5 presents the IR spectrum of drug GW source of peat, modifier and modified compounds. In the original GW availability of bandwidth fluctuations relationships OS aromatic ring (about 1610 cm-1in the IR spectrum of the modified drug GW peat indicates the presence of aromatic skeleton part. The band around 1710 cm-1refers to fluctuations due to C=O and confirms the presence of carboxyl and carbonyl groups in the product band in the region of 1250 cm-1refers to the stretching vibrations of C-O phenolic and carboxylic groups, band in the range of 1050-1150 cm-1correspond to fluctuations due to C-O alcohol groups. The presence of these bands indicates the presence of different oxygen-containing functional groups in drugs GW.

In the spectra of modified drugs are present as bands that are characteristic of the civil code and modifier. Figure 5 shows that in the preparation of HS-APTS in addition to the superposition of GW and APTS (two strong bands at 1100 and 1050 cm-1characteristic of Si-O vibrations) there is a band at 1265 cm-1that characteristic oscillations in the plane of the amide bond (amide band 3), which indirectly indicates the formation of amide linkages. You may also notice the offset is their broad band at 1600 cm -1in the shorter wavelength region, which indicates an increase in the share of contribution of carbonyl vibrations of the atoms in the structure of amides in this peak.

Example 4

The example describes the modification of hydroxyl-containing solid surface is glass - using humic silanol derivatives and demonstrates its hydrophobicity as a result of this processing. To study the hydrophobicity of the coatings formed silanol derivative of GW, the modification of the glass plates. This allowed us to directly determine their hydrophobicity on the value of the contact angle of water droplets on the treated surface.

For the experiment used glass slides and glass Borafloat for atomic force spectroscopy, cut into equal pieces measuring 1 cm by 2 cm For the application of silanol derivatives of humic substances to the surface of the glass is first activated. For this purpose, the plates were placed in a muffle furnace in the heating mode up to 260°C - 1 hour and aging at 260°C for 22 hours. Then the plates were cooled to room temperature and placed in alkaline ethanol solution (10% NaOH and 40% ethanol) for 2 hours at room temperature. Next, the glass thoroughly washed first with distilled water, then with ethanol and dried in the air. Then prepare a solution of silanol derivatives of humic substances concentration is the situation of 1 g/L. For this purpose a portion of the drug 50 mg moistened with 0.5 M NaOH and placed in an ultrasonic bath for 30 min at 30°C. the Solution was brought to 50 ml of phosphate buffer (pH 6.0, 0.03 M) and centrifuged at 10,000 rpm for 10 minutes to separate the insoluble residue. Then selected 40 ml brought the pH of the solution to 6.0 diluted HCl and diluted with phosphate buffer to a concentration of 1 g/l, after which they were immersed glass plates obtained in the solution for 24 hours. Then the plates were thoroughly washed with distilled water and dried in the air.

Evaluation of the hydrophobicity of the surface of the obtained plates were performed by measuring the wetting angle of water on the surface. This glass was placed on the substrate of the device. Then on the glass caused a drop from a syringe and shot micrograph (examples shown in Fig.6), then from photographs was determined by contact angle of wetting of the glass plates.

Table 8 shows data obtained by measuring a contact angle of water on the original glass plates and the plates, various modified silanol derivative of GW.

Table 8
The value of the wetting angle on the original and the modified glass
MedicationThe wetting angle, deg
The original glass41
GW-APTS58
GW-ARTS58
RNA was APTS48

From the presented data shows that the hydrophobicity of the glass is increased when they are processed silanol derivative of humic substances in the immobilization of organic humic film. When this film peat preparation less hydrophobic than coal. This can be explained by the fact that the composition of peat humic substances contain a hydrophilic peripheral part, represented by polysaccharides.

The morphology of the formed humic films studied by atomic force microscopy (AFM). Figure 7 shows the image surface of the original glass, processed coal humic modifier GW-APTS.

From the presented images show that the treated surface is observed uneven monocline floor with separate inclusions with an average diameter of about 100 nm and a height of 15 nm. This surface morphology may be related to the fact that the silanol derivative of humic substances present in the solution in the form of Zola, therefore, are sorbed particles dost is exactly large. Judging by the thickness of the layer of the described particles acquire planar conformation to provide the most efficient binding to the surface.

Thus, we can conclude that the silanol derivative of humic substances have the ability to increase the hydrophobicity of the mineral surface due to the formation of humic film, which is a favorable property in respect of application for restoration of degraded soils.

Example 5

The example demonstrates the increase in vodoprochnost soil aggregates treated with humic silanol derivatives. Were chosen for the study of the original GW, GW-APTS and phosphate buffer. A solution of 1 g/l of the original GW was prepared by dissolving in phosphate buffer (0.03 M, pH 6), a solution of 1 g/l GW-APTS were prepared by serial dilution in KOH (3 M), acidification to pH 6 with diluted phosphoric acid and subsequent dissolution in phosphate buffer (0.03 M, pH 6).

To assess vodoprochnost units used method Andrianova. The soil sample of typical Chernozem under steam from the skilled plot in the Kursk region in the air-dry sieved on a sieve and selected fraction with the size of the units 3-5 mm In a Petri dish was placed filter paper and secured it with a glass of weights. Testing took 50 units, which are evenly laid out on cha is ke Petri. Next, the aggregates capillary saturated, moistening the filter paper in the Petri dish test solution. Left for drying in air for 24 hours. Then the units were first saturated capillary distilled water for 3 minutes, and then carefully adding water to the level of 0.5 cm above the units. Every minute counted the number of broken aggregates. The observation was carried out for 10 minutes. Next, calculate the coefficient of vodoprochnost soil aggregates by the following formula:

K=n=19(c-a)*(n10+0.05)+bc

where a is the number of broken units per minute,

b - the number of undecayed units in 10 minutes

with the total number of units.

On Fig see pictures of the experiment before and after the disintegration of soil aggregates. Kinetic dependences presented in Fig.9.

From the figure it is evident that the soil aggregates treated with silanol derivative of humic substances significantly increases photoproject. Calculated by the formula factors in the doprocess was 0,51, of 0.27 and 0.22 for the units processed CHS-APTES-30, H2O and CHS-K, respectively.

Example 6

The example demonstrates the restoration and improvement of the structure of degraded soils as a result of processing of humic silanol derivatives.

Soil structure is the distribution of soil structural units. To agronomically valuable structure include soil aggregates of 0.25-10 mm is One of the most important properties of the structure is water resistance - the ability of aggregates to resist the destructive action of water. Thus, the larger particles with sizes of <0.25 mm in the soil, the more degraded the soil structure.

Therefore, as a model substrate used soil particle size <0,25 mm Particles were obtained by dry sieving of sod-podzolic soil through a sieve <0,25 mm as an indicator of recovery of degraded soil structure was estimated percentage formed under the influence of humic silanol derivatives of water-stable aggregates (particles >0.25 mm).

In the Petri dish was introduced 25 g of particles of 0.25 mm sod-podzolic soil, there was added 25 ml of a solution of humic silanol derivatives, have established pH 6.8±0.2, concentration derivatives: 2.5, 5, and 10 g/l as a control under the same conditions made the original GW of coal used for modification. In addition, if the mortgaged option with distilled water.

Petri dishes with soil was dried at room temperature in a vacuum Cabinet to air-dry state.

Then from the options selected samples (5 replicates for each variant), which was determined by the content of water-stable aggregates. For this sample, gently mash with the pestle with rubber tip on the structural individually weighed, was passed through a 0.25 mm sieve and again weighed to the denition of the number formed of air-dry aggregates. Then a portion of the obtained aggregates >0.25 mm was placed on a sieve (0.25 mm) and saturated capillary distilled water through a wet filter paper. Saturated aggregates were immersed in water for 10 minutes, then was passed through a 0.25 mm sieve ten motion of the sieve of 45° and the movements of the sieve in the water upside-down. Passed through a sieve particles were dried in a water bath, and finally dried at 105°C in an oven and weighed. The mass difference between the obtained dry sieving the aggregates and particles that passed through the sieve when sieving in water was determined the number of the resulting water-stable aggregates. On the basis of the obtained data was calculated the percentage of the formed water stable aggregates. All the obtained averages were compared with each other by t-test (α=0,05).

Figure 10 shows the formation of water-stable aggregates of p is connich structureless particles smaller than 0.25 mm in the processing silanol derivative of GW. For comparison, the formation of aggregates under the action of the original GW of coal used for modification.

Humic silanol derivative and source of humic substances significantly increased the formation of water-stable aggregates of the particles <0.25 mm compared to the option with distilled water. The average values obtained for humic silanol derivatives, exceeded those for the original GW of coal. While significant differences between the silanol derivative and native HS was observed at the level of their make up to 5 g/L. Further increasing the concentration to 10 g/l neutralized the difference between the original and modified HS.

Thus, it is shown that:

- humic silanol derivatives significantly increase the content of water-stable aggregates in the model of degraded soils;

- humic silanol derivatives increase the content of water-stable aggregates in the model of degraded soil more efficiently than conventional humic substances;

concentration for the application of humic silanol derivatives with the aim of restoring degraded soils should not exceed 5 g/L.

Example 7

The example demonstrates the use of silanol derivative of GW as an ameliorant for improving the soil structure in the conditions of small-plot experiment.

Tests were businessmen who were on silsoecollege sod-podzolic soil. Tillage was performed by irrigating solutions of the studied drugs in a concentration of 2.5 g/L. the consumption Rate was 10 l/m2. As control was used well water. Next were wheat (500 PCs/m). The care of the crops included manual weeding and watering as necessary. The duration of the experiment was 99 days. Before the start of the experiment and after it carried out the determination of agronomically valuable aggregates of 0.25-10 mm).

It was found that during the experiment (99 days) make GW APTS led to the increase of the coefficient of structure of soil, determined by the contents of agronomically valuable aggregates, 11% (11).

The above description of possible applications of the present invention as fully demonstrate the nature of the present invention that others can, by applying this knowledge, it is easy to change or modify the described General method for the purposes of other special applications, without changing its substance. Therefore, such adaptations and modifications of the proposed approach should be considered as not containing in itself independent of the subject invention. However, it goes without saying that the main purpose of terminology or verbal expressions used in the description of this image is the shadow, was the disclosure of the invention, it was assumed that this can be done using other expressions without restrictions on the used terminology.

Describes the methods, materials and the various stages of the claimed steps can be implemented using other approaches that would not change the essence of the invention. For example, expressions such as "using" or "by...", as well as any other phraseological description of the methods used in the description of the examples above or in the description of the following claims, which preceded the presentation of the method being invoked to determine and to cover all possible structural, physical, chemical, and engineering elements and patterns, as well as any methodological steps that may already exist today or to be devised in the future to carry out the functions listed in this invention, regardless of how fully they are equivalent to the above examples applications, that is allowed to use any other methods and instructional techniques for the above-mentioned functional properties, it is assumed that all used private methods should be interpreted in its broadest sense.

1. Gramnegative the second derivative, containing silanol groups, characterized by solubility in an alkaline environment and the ability to irreversible sorption on a solid substrate containing on a surface-Oh groups obtained by the process involving the interaction of humic substances with aminoalkylsilane in the aquatic environment, the humic substances used substance isolated from natural sources, and as aminoalkylsilane use 3-aminopropyltriethoxysilane or 1-aminohexanoate 6-aminomethylenemalonate with subsequent distillation of the water and heating the product at a temperature of 30-150°C.

2. Application gramnegative derived for the restoration of degraded soils in situ, including the introduction of humic derivative according to claim 1 in the form of an aqueous solution on the area of degraded soil.

3. Application gramnegative derivative according to claim 1, in which humic derivative in aqueous solution contribute either through drip irrigation or with sprinklers.

4. The use according to claim 3, in which humic derivative used in the form of 0.01-10 wt.% aqueous solution.

5. The use according to claim 3, in which gramnegative derivative used in the form of 0.01-10 wt.% aqueous solution in combination with liquid and complex fertilizers.

6. Reagent for the recovery of degraded soils n situ, including gramnegative derivative according to claim 1.

7. The reagent according to claim 6, in which gramnegative derivative is used in aqueous solution.

8. The reagent according to claim 6, in which gramnegative derivative is used in the form of an aqueous solution with a concentration of 0.01-10 wt.%.



 

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FIELD: agriculture.

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1 dwg, 4 tbl, 2 ex

FIELD: agriculture.

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2 cl, 5 tbl, 2 ex

FIELD: chemistry.

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2 cl, 11 tbl

FIELD: agriculture.

SUBSTANCE: method of production of structured peat-sapropelic concentrate comprises cavitational dispergating of humate-containing agent using an alkaline solution of potassium hydroxide, at that in a moving stream of water the fragmented peat with a particle size of not more than 5 mm, as well as putrid mud, potassium hydroxide, white mud is fed. All the components are taken at a certain ratio. The resulting solution is subject to cavitational dispergating to temperature of 90°C.

EFFECT: invention enables to simplify the method of preparation of high-quality organo-mineral complex fertiliser, to reduce the energy consumption of the process while increasing its ecological compatibility.

FIELD: chemistry.

SUBSTANCE: invention relates to agriculture. The method of producing humic preparations involves ultrasonic dispersion of humate-containing substances. At least one jet or vortex flow of humate-containing substances is created, which is treated with an air or steam stream using a jet-edge generator with ultrasonic radiation intensity greater than 10 W/cm2.

EFFECT: invention provides an efficient technique of processing humate-containing substances, which enables to obtain water-soluble organic substances with high content of fulvic and humic acids with a simple process for production thereof, low labour input and material consumption of the process.

2 cl, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to agriculture. Organomineral complex fertiliser contains peat, mineral components and nutritional microelements as humate-containing substances, with nitrogen-ammonia constituent in form of urea and water, processed with UV-irradiation, being introduced into complex composition. All components are taken in specified ratio.

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2 cl, 8 tbl

FIELD: chemistry.

SUBSTANCE: method of decontaminating oil-contaminated soil involves preparation of a treatment area, collecting, excavating and delivering oil-contaminated soil to the treatment area, preparing the oil-contaminated soil, adding a humic-mineral complex and providing processes for biological decomposition of the oil-contaminated soil. The method of decontaminating spent drilling mud involves lime treatment, reagent coagulation, adding flocculants and a humic-mineral complex, step-by-step cutting of the drilling mud into a buffer layer while laying the mud in a layer of not more than 8-10 cm, drying the drilling mud and stacking into piles for subsequent recycling. The humic-mineral complex is obtained by low-temperature mechanochemical extraction of humic acids with by crushing brown coal in a dispersion machine while mixing the crushed brown coal with an alkali.

EFFECT: invention increases efficiency of methods in which a humic-mineral complex is used.

2 cl, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to agriculture. The method of producing humic fertiliser for organic farming, meant for treating soil and vegetative plants, wherein said fertiliser is obtained in two steps: at the first step, natural humic acids contained in brown coal are transferred into an aqueous solution in form of ammonium humate by treating with 1.5-2.0% aqueous ammonium hydroxide solution to pH 6.9-7.1 with the ratio of the liquid component to the solid component of 7-7.5:1, and the obtained solution is separated from the mineral ballast which is not chemically bonded to the humic acids; and at the second step, metal cations chemically bonded to the ammonium humate are removed from the ammonium humate solution by treating with a cationite to pH 4.0-4.2.

EFFECT: invention enables to obtain water-soluble humic acids which do not container both the mineral ballast and metal cations.

2 cl, 4 tbl, 8 ex

FIELD: agriculture.

SUBSTANCE: invention relates to the field of environmental protection and can be used in the rectification of the consequences of the oil spill on the soil. The method consists in mixing the oil-contaminated soil, spread over the surface of freshly ploughed uncontaminated field with the thickness layer from 1/10 to 1/6 of the ploughing depth, to the full depth of ploughing using the tiller several times.

EFFECT: invention enables to restore oil-contaminated soil without application of additional neutralising foreign substances and reagents.

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