The method of obtaining vodoviteho aluminosilicate dispersed systems

 

(57) Abstract:

The invention relates to the field of chemical industry, in particular to a method of obtaining a new water-binding aluminosilicate dispersed systems. The purpose of the invention synthesis of new water-binding unidentified patterns aluminosilicate dispersed systems coordination compounds of zinc chloride with a mixture limit (bold) primary amines (MS) General formula RNH2where R C17-C20-alkyl, with improved quality characteristics compared with known generally. The method is performed by processing of zinc chloride molten mixture limit (bold) primary amines (MS) General formula RNH2where R C17-C20alkyl, the molar ratio of zinc chloride and MS, equal(1,5-1,7):(1,0-1,2). 1 the sludge. 3 table.

The invention relates to a method of obtaining a new water-binding aluminosilicate dispersed systems unidentified structure of coordination compounds of zinc chloride with a mixture limit (bold) primary amines (MS) General formula RNH2where R C17-C20-alkyl, which helps to more efficiently remove excess moisture and thereby reduce the th heaving of the soil currently used Portland cement [1] the Main disadvantage of using Portland cement is the lack of effect of reducing frost heaving immediately after treatment of the soil and the need for the manifestation of this effect for a long period (28 days), defined term hardening binder. To obtain the effect of reducing frost heaving (KPuig.=0,9-0%) requires a large consumption of scarce binder (8-12% by weight of soil, see table. 3, a drawing).

It is now known generally aluminosilicate dispersed systems, reducing frost heave of the soil, which is a coordination compound of iron chloride with aniline FeCl2An, where An aniline [2] the Method of obtaining FeCl2An is the mixing of still residue after distillation of aniline with waste titanium containing FeCl2in a molar ratio of 1:5.

Known generally has a drawback. The coordination compound FeCl2An does not provide sufficient binding moisture of the soil and not creates a strong structural connection. In this regard, to obtain the effect of reducing frost heaving (KPuig.=0,7-0,05%) is needed in the soil FeCl2An in a large number of 2.5-3.0% by weight of soil (see table. 3, a drawing).

The purpose of the invention synthesis of new water-binding dispersion alumosilicic systems unidentified structure of coordination compounds of zinc chloride with a mixture limit the governmental characteristics compared with known generally.

The objective is achieved by the fact that zinc chloride ZnCl2handle molten mixture limit (bold) primary amines (MS) General formula RNH2where R C17-C20-alkyl, in a molar ratio of zinc chloride and MS, equal(1,5-1,7): (1,0-1,2). The formed precipitate was separated from the filtrate on a porous filter (type a Buchner funnel) and washed with ethyl alcohol, water, and dried in air.

When you use the product to reduce frost heaving clay soil requires a significantly smaller amount in comparison with the known generally aluminosilicate dispersed systems. Thus, the introduction of 0.5-1.0% of the substance from the mass of soil translates clayey soil in napucenosti. To get a similar effect takes about 2.5-3.0 percent FeCl2An and 8-12% of Portland cement 400 from the mass of soil (table. 3, a drawing).

Obtaining coordination compounds of zinc chloride with MS.

P R I m e R 1. 0,37 kg of zinc chloride in the form of 50-55% aqueous solution (waste) is treated with 1.68 kg of molten MS (waste). The formed precipitate was separated from the filtrate on a porous filter (type a Buchner funnel) and washed with ethyl alcohol, water, and dried in the temperature of the melting point of the obtained product 120aboutC. zinc Chloride is used in the form of 50-55% aqueous solution of waste production ON "Khimprom", Novocheboksarsk), which is generated by the selection of zinc chloride of high purity. The mixture limit (bold) primary amines (MS) General formula RNH2where R C17-C20-alkyl, is used in the form of waste "Azot" (, Berezniki, Perm region), on THE other 113-03-3-12-89, which is generated by the selection of flotation reagent MS high purity. The departure of MS. contains 56% of the amines, the rest of the hydrocarbons.

P R I m m e R 2. 0,37 kg of zinc chloride is treated with 1.05 kg of molten MS. The formed precipitate was separated from the filtrate on a porous filter (type a Buchner funnel) and washed with ethyl alcohol, water, and dried in air. Get 1 kg of coordination compounds of zinc chloride and MS ZnCl2MS with the practical output of 88%, the melting point of the obtained product 120aboutC. zinc Chloride and MS used in the form of ready-made sales of drugs. The mixture limit (bold) primary amines (MS) General formula RNH2where R C17-C20-alkyl, were used in the form of ready-made sales of the drug, produced BY "Nitrogen" (, Berezniki, Perm region), THE 6-02-740-79 as flotation relationship of zinc chloride and MS are given in table. 1. From table. 1 shows that the molar ratio of zinc chloride and SHE should be(1,5-1,7):(1,0-1,2) (options 17-19, 24-26, 31-33), since at such a molar ratio of greatest practical yield of the target product, which has an IR spectrum with a clear position of the corresponding absorption bands. Since there are no results for the elemental analysis of the target product, IR spectroscopy was used to identify it. The assignment of absorption bands in the infrared spectrum ZnCl2SHE is given below. With decreasing molar amount of zinc chloride to 1.3 to 1.4 (range 1-14), or increasing the molar amount of zinc chloride to 1.8 to 1.9 (range 36-49), and the decrease of molar number of MS to 0.8-0.9 (options 1, 2, 8, 9, 15, 16, 22, 23, 29, 30, 36, 37, 43, 44) or increasing the molar amount of MS to 1.3 to 1.4 (options 6, 7, 13, 14, 20, 21, 27, 28, 34, 35, 41, 42, 48, 49) formed product with a reduced practical output and clear enough IR spectrum, i.e., outside of the proposed method (options 1-3, 8-11, 15, 16 22, 23, 27, 29, 30, 34-49), either not formed product (options 4-7, 12-14, 20, 21, 28). Thus, from table. 1 it follows that the molar ratio of zinc chloride and SHE should be(1,5-1,7):(1,0-1,2).

The connection of zinc chloride with MS represents crayons>2MS in water has a pH of about 7.

As ZnCl2MS is a substance of unknown structure and elemental analysis in this case can be no, for the identification of the target product, the characteristics of the chemical nature of communication used method of IR-spectroscopy in the field 4000-150 cm-1. The measurement of the IR spectra was carried out on the spectrometer UR-20 and FIS-21 Hitachi. The assignment of absorption bands in the IR spectra of the free MS and ZnCl are given in table. 2.

From table. 2 shows that the interaction of the amino groups MS with zinc cation acceptor electron pairs leads to a sharp decrease of the frequencies of the symmetric (s) and antisymmetric (a) stretching vibrations of NH of amino groups. In table. 2 contains the results of calculations characterizing the status amino MS in the coordination, execution, using the given values of the frequencies of stretching vibrations of NH. Calculation of force constants fNHcommunication NH, valence angles (HNH) and bond lengths rNHamino MS was performed by the method of Linnet [3], the coefficients hybridization b, the overlap integrals Isthe orbitals of the hydrogen atom with a hybrid orbital of the nitrogen atom of SNHcalculated by the methods of the AE ZnCl2MS compared with MS is the occurrence of the additional positive charge on the nitrogen atoms of amino groups MS in the delay of its lone-electron pair cation of zinc, which plays the role of electronicstore. The estimation of the additional positive charge on the nitrogen atom in ZnCl2SHE produced according to the equation Linnet [3] the usefulness of the empirical approach using approximate valence-force diagram for the analysis of vibrational spectra of free and coordinated amines confirmed by the data [5]

In the IR spectrum of ZnCl2SHE has an absorption band that is responsible, according to literature data [6] valence fluctuations Zn-N and valence fluctuations Zn-Cl (see tab. 2). In accordance with literature data, the position of the absorption bands of Zn-Cl meets the tetrahedral structure of the complex ZnCl2MS c valence angle (Cl Zn CL)=110aboutC.

The IR spectra of the target product, obtained from ready-made sales of drugs and waste production are identical. On the basis of IR spectroscopic study of the target product, it follows that he is a coordination compound of zinc chloride with MS ZnCl2MS..

Coordination is the shaft systems (table. 3). Specified practical use ZnCl2SHE is new. In the literature there is no information about using ZnCl2SHE considered for practical application. The main difficulty in the strengthening of aluminosilicate dispersed systems, which include, in particular, moisture clayey soils, is to eliminate excessive stickiness, which prevents the use of most of the excavation, groundsmaster and vehicles. Generated in the process of loosening clods of clay soil moisture stick together and stick to working bodies and chassis of cars. Therefore, soil moisture is very difficult to mix with astringent components and even more difficult to condense. In this regard, before the introduction of binders, in particular cement, it is necessary to remove excess moisture, which contributes to reduced frost heaving.

The mechanism of interaction of coordination compounds, primary amines (linecomplete) with loamy soils of high humidity can be represented as follows. Interaction of mineral particles of clay soils with linecomplete preceded by definite their orientation. Aminoquinuclidine hydrophilicity clay soils in the presence of linecomplete. Linecomplete attracted and held on the surface of section in the oriented state of the polar group (the amino group) to polar sorbent (clay particles), nonpolar hydrocarbon (inactive) in the external field (pore solution). Group NH2give strong hydrogen bonds with neighboring electronegative atoms. In this regard, the interaction between electronegative oxygen ions to the surface of the crystal structures of clay minerals and reagents appears to occur through hydrogen polar groups, for example, R-H O (surface and mineral), where R is a hydrocarbon radical. In the case of linecomplete amino group with one hydrogen involved in hydrogen bonds with the oxygen atoms located on the surface of the mineral:

-

Know the facts indicate that the ligands coordinated to the Central atom in a complex connections in the connections with metal not use all of its electron density. According to quantum-chemical calculations on coordinated ligands remains part of the negative charge, which is manifested, in particular, the existence of coordination polymers. There is thus the possibility of participation of coordinats is but that linecomplete simultaneously translated part of the free water in the bound state due to hydrogen bonds according to the following scheme:

- + ___ -

This conclusion is confirmed by the literature data, according to which part of primary amines in hydrogen bonds as an acceptor of protons leads to an increase in maximum deformation NH vibrations. To NH deformation vibrations of the amino group of linecomplete in IR-spectra belongs to the band around 1600 cm-1. The IR spectrum of the suspension ZnCl2MS H2On clay soil, there is an increase of the maximum absorption band (1600 cm-1) NH deformation vibrations of the amino group ZnCl2MS, which confirms the formation of hydrogen bond between the nitrogen of the amino group of the complex with the hydrogen of water molecules. The change in the surface forces of the clay particles under the influence of linecomplete ZnCl2MS affects water-holding capacity of clay soils due to the creation of new structural relations. The coordination compound ZnCl2MS having a high water-binding ability, in a small number lowers frost heave of clay soil.

Effect on frost heave of clay soil koordinacioni 400.

We used clay soil, selected in Krasnoselsky district, St. Petersburg.

Clay soil is hydrologists loam, yellowish-brown, plastic, with small gray spots, likely spots gleyed, with inclusions of gravel, Gruss, the roots of plants, with the slots of the iron-containing contaminants. X-ray diffraction study of clay soil showed that it is represented by hydromica (prevails), chlorite (slave number), kaolinite (traces). The natural moisture of the soil W=15--16% density varies from of 2.05 to 2.11 g/cm3. When testing the relative humidity of the clay soil was 0.8.

Study of the effect on frost heave of clay soil of coordination compounds FeCl2An, ZnCl2MS and Portland cement-400 was conducted by the method [1]

Clay soil was treated with different amounts of coordination compounds FeCl2An, ZnCl2MS and Portland cement, followed by stirring to education non-sticky, granular homogeneous adobebibutils mass. The resulting mixture was condensed on a hydraulic press in a special form cylinders with a diameter of 100 mm and height 80 mm, with the over 1 and 28 days in the forms in the air-humid environment, then saturated water to a full water saturation (for 3 days) and tested for resistance to frost by the method of [1] with the definition of the frost heave coefficient representing the ratio of the deformation of frost heaving (value frosty raise to the height of the sample. Tests have shown (PL. 3, a drawing) that clayey soil, related in raw form by the degree of heaving (KPuig=5,8%) for heaving soils (group IV), the processing ZnCl2MS in quantities of 0.5-1.0% by weight of the soil is characterized by the coefficient of frost heaving, the lesser of 1.0% (the drawing), which translates it into a group narcisistic soils (group I). Moreover, the introduction in clayey soil ZnCl2MS in the amount of 1% prevents frost heave (KPuig.=0%). The results of studying the effect on frost heave of clay soil coordination compounds ZnCl2MS. synthesized from waste products (example 1) and of the finished products (example 2) are the same. To get a similar effect of reducing frost heaving clay soil, using coordination compounds FeCl2An require a significantly greater amount of 2.5-3.0% To get a similar effect when 0%) manifests itself only after a 28-day period, necessary for the hardening of cement. 1-day age, i.e., immediately after treatment, soil cement, reducing frost heaving is practically not observed (Puig=5,0% ). The optimal number of ZnCl2x x MS needed to prevent frost heaving clay soil, was determined as follows: lower limit of conditions that reduce frost heaving when using ZnCl2MS was more effective than using FeCl2In not less than 20% upper limit on the number of ZnCl2MS, calling the complete absence of frost heaving. These limits ZnCl2SHE is 0,5-1,0%

To improve the quality characteristics generally aluminosilicate dispersed systems is proposed coordination compound ZnCl2MS. As follows from the data table. 3 and drawing, to prevent frost heaving clay soil, fewer ZnCl2MS compared with FeCl2An and Portland cement grade 400. Therefore, ZnCl2MS has a higher water-binding ability compared with FeCl2An and Portland cement grade 400. The coordination compound ZnCl2MS can be used as the material dlitelnaya ZnCl2MS is performed using the waste from chemical plants, and therefore it can be recommended for widespread implementation as generally aluminosilicate dispersed systems. Simultaneously solve some of the issues of environmental protection, waste utilized as chemical plants.

The drawing shows the variations in the coefficient of frost heaving (KPuig). clay soil depending on the type of substance (D,), where 1 coordination compound FeCl2An (1 or 28 days of incubation, samples); 2 Portland cement (1 day of incubation, samples), 3 Portland cement (28 day cure samples) 4 coordination compound ZnCl2MS (1 or 28 days of incubation, samples), the dashed line shows the classification of the soil to the appropriate group in KPuig.

The METHOD of OBTAINING VODOVITEHO ALUMINOSILICATE DISPERSED SYSTEMS by reacting a metal salt with aminecontaining component, wherein as the metal salt using zinc chloride as aminecontaining component of the fused salt limit primary amines of General formula

RNH2,

where R is C17C20-alkyl,



 

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