The method of obtaining bis (1-hydroxyethane-1,1-diphosphonate(1-)) cobalt (ii) (options)

 

The invention relates to chemical technology of organophosphorus substances that can be used to prepare electrolyte galvanic and chemical abaltimore, as well as receive other organophosphorus substances, used as fertilizers in agriculture. Describes how to obtain bis(1-hydroxyethane-1,1-diphosphonate(1-)) cobalt (II), comprising preparing an aqueous solution of salt of cobalt (II) of 0.7 to 1.5 mol/l and 1-hydroxyethane-1,1-diphosphonic acid of 1.5-4.0 mol/l, followed by crystallization of the product, the separation of the precipitate from the solution and drying. The method can also be carried out using an aqueous solution of salt of cobalt(II) and 1-hydroxyethane-1,1-diphosphonic acid in concentrations of 0.1-1.3 mol/l and 0.3 to 3.0 mol/l, respectively, while the aqueous solution additionally injected miscible with water, an organic solvent. The technical result is to increase output while maintaining the homogeneity and crystallinity of the product. 2 S. and 6 C.p. f-crystals, 1 table.

The invention relates to chemical technology of organophosphorus substances, in particular to a method for producing bis(1-hydroxyethane-1,1-diphosphonate(1-)) to the ub>S(HE)(RHO3H2)2(H4L) Co(H3L)2·4H2O, which can be used to prepare electrolyte galvanic and chemical abaltimore, for other 1-hydroxyethane-1,1-diphosphonates of cobalt, in micronutrients in agriculture.

A method of obtaining bis(1-hydroxyethane-1,1-diphosphonate(1-)) cobalt (II), based on the reaction of saturated aqueous solutions of Son2L and H4L, taken in a molar ratio of 1:1, at pH of 1.0 [Keshikbaeva B. H., Mitrofanova N. D., Martynenko L. I. Solid acetylacetonate cobalt (II).//The journal of inorganic chemistry. 1988. So 33. Vol.6. S. 1509]. The disadvantage of this method is the need to use hard-to-reach reagent Son2L·4H2O, which is not produced by the chemical industry. This method also has disadvantages described below for the prototype.

Closest to the proposed invention is a method of obtaining bis(1-hydroxyethane-1,1-diphosphonate(1-)) cobalt (II), an aqueous solution which is prepared by the reaction of:

Co(OH)2·Coco3+4H4L2SD(N3L)2+CO2+3H2About

[Keshikbaeva B. H., Mitrofanova N. D., Martinrea B. H. Synthesis, properties and structure of complexions of some transition metals (cu, Ni, Co, Mn, Zn) with oksietilidendifosfonovaya and ethylenediphosphonic acids. Diss....Kida.the chemical.Sciences. M.: Moscow state University. 1988]. Solid bis(1-hydroxyethane-1,1-diphosphonate(1-)) cobalt (II) was isolated from solution by fast (when heated) or slow (without heating) evaporation of the solution [Keshikbaeva B. H., Mitrofanova N. D., Martynenko L. I. Solid acetylacetonate cobalt (II).//The journal of inorganic chemistry. 1988. So 33. Vol. 6. S. 1509. Keshikbaeva B. H. Synthesis, properties and structure of complexions of some transition metals (cu, Ni, Co, Mn, Zn) with oksietilidendifosfonovaya and ethylenediphosphonic acids. Diss....Kida.the chemical.Sciences. M.: Moscow state University. 1988].

The formation of different hydrates bis(1-hydroxyethane-1,1-diphosphonate(1-)) cobalt (II) Co(H3L)2·11H2O and H3L)2·6N2Oh, characterized by a powder x-ray that contains only 9 and 3 reflect [Keshikbaeva B. H. Synthesis, properties and structure of complexions of some transition metals (cu, Ni, Co, Mn, Zn) with oksietilidendifosfonovaya and ethylenediphosphonic acids. Diss.Kida.the chemical.Sciences. M.: Moscow state University. 1988]. This indicates a weak zakristallizovannykh substances what about the prototype (examples 1, 2), does not correspond to the calculated for bis(1-hydroxyethane-1,1-diphosphonates(1-)) cobalt (II) of the proposed sources of information [Keshikbaeva B. H., Mitrofanova N. D., Martynenko L. I. Solid acetylacetonate cobalt (II).//The journal of inorganic chemistry. 1988. So 33. Vol. 6. S. 1509. Keshikbaeva B. H. Synthesis, properties and structure of complexions of some transition metals (cu, Ni, Co, Mn, Zn) with oksietilidendifosfonovaya and ethylenediphosphonic acids. Diss....Kida.the chemical.Sciences. - M.: Moscow state University. 1988], and to the product obtained in example 1 indicate its heterogeneity.

When creating the present invention, the aim was to obtain high yield of uniform bis(1-hydroxyethane-1,1-diphosphonate(1-)) cobalt (II) in crystalline form.

The problem is solved in that a method of obtaining bis(1-hydroxyethane-1,1-diphosphonate(1-)) cobalt (II) includes the preparation of an aqueous salt solution of cobalt (II) and 1-hydroxyethane-1,1-diphosphonic acid, the crystallization of the product, separating the precipitate from the solution and drying. New this method is that prepare a solution with a salt concentration of cobalt (II) of 0.7 to 1.5 mol/l and 1-hydroxyethane-1,1-diphosphonic acid of 1.5-4.0 mol/l, Preferably prepare a solution viola (II) preferably using salt, selected from the group consisting of sulfate, sulpham, chloride, perchlorate, nitrate, tetrafluoroborate, hexafluorosilicate, thiocyanate, cobalt (II). Crystallization of the product are preferably at a temperature (-5)-25°C.

The task is also solved by the fact that the method of obtaining bis(1-hydroxyethane-1,1-diphosphonate(1-))cobalt (II) includes the preparation of an aqueous salt solution of cobalt (II) and 1-hydroxyethane-1,1-diphosphonic acid, the crystallization of the product, separating the precipitate from the solution and drying. New this method is that prepare a solution with a salt concentration of cobalt (II) 0.1 to 1.3 mol/l and 1-hydroxyethane-1,1-diphosphonic acid 0.3 to 3.0 mol/l aqueous solution further add miscible with water, an organic solvent. It is preferable to prepare an aqueous solution with a molar ratio of the salt of cobalt (II):1-hydroxyethane-1,1-diphosphonic acid is 1:(2-3). As the organic solvent preferably used a solvent selected from the group consisting of methanol, ethanol, propanol, isopropanol, formic acid, acetic acid, acetone. The organic solvent is preferably added in an amount to provide the volume ratio of aqueous solution: zakluchaetsa in dissolving the required amounts of salts of cobalt (II) and 1-hydroxyethane-1,1-diphosphonic acid in water, the allocation of a crystalline precipitate, separating the precipitate from the solution with known methods (for example, by filtration under vacuum, centrifugation, washing the precipitate on the filter with a solvent and drying the precipitate in air at room temperature.

In the solution of the above composition is set balance:

The use of high concentrations of the reactants and excess 1-hydroxyethane-1,1-diphosphonic acid as compared with the stoichiometric ratio of Co2+:H4L equal to 1:2, allows to displace the equilibrium of reaction (1) in the direction of formation of the reaction product, and the selection in the course of the reaction (1) hydrogen ions suppresses unwanted reaction (2) dissociation of the complex With(N3L)2in the solution. As a result, the solubility of bis(1-hydroxyethane-1,1-diphosphonate(1-))cobalt (II) is significantly reduced, and its output is greatly increased.

For a homogeneous bis(1-hydroxyethane-1,1-diphosphonate(1-))cobalt (II) crystallization should go from a solution in which 1 mol of the salt of cobalt (II) have 2 or more moles of 1-hydroxyethane-1,1-diphosphonic acid, because at a lower molar ratio of the reagents of the races is A.

Conducting the reaction in a strongly acidic medium and in the presence of excess 1-hydroxyethane-1,1-diphosphonic acid promotes the reaction product of bis(1-hydroxyethane-1,1-diphosphonate(1-))cobalt (II) is formed in a well crystallized form.

The upper limit of the salt concentration of the cobalt (II) and 1-hydroxyethane-1,1-diphosphonic acid is limited by the solubility of substances in water, as well as the need to obtain a solution of moderate viscosity. The lower limit of the concentration of the reactants is determined by the need to obtain bis(1-hydroxyethane-1,1-diphosphonate(1-))cobalt (II) with the release of not less than 25%.

As salts of cobalt (II) it is possible to use a salt having a high solubility in water: sulfate SO4·7H2Oh, sulpham With(N2NSO3)2·4H2O, chloride l2·6N2Oh, perchlorate(ClO4)2·6N3Oh, nitrate(NO3)2·6N2O, tetrafluoroborate Co(BF4)2·6H2O, hexafluorosilicate SiF6·6N2O, thiocyanate Co(SCN)2·4H2O and some others.

Crystallization of the product can be maintained at a temperature of (-10)-70°C, however, given the fact that the solubility of bis(1-hydroxyethane-1,1-diphosphonate(1-))cobalt (II) in water decreases with ponie the>the IP(1-hydroxyethane-1,1-diphosphonate(1-))cobalt (II) it is soluble in water but poorly soluble in the usual organic solvents: aliphatic and aromatic hydrocarbons, chlorinated hydrocarbons, monohydroxy alcohols, esters of monocarboxylic acids, etc. So adding to the aqueous solution containing a salt of cobalt (II) and 1-hydroxyethane-1,1-diphosphonic acid, miscible with water, an organic solvent significantly reduces the solubility of bis(1-hydroxyethane-1,1-diphosphonate(1-))cobalt (II) due to the effect of vysalivaniya, which leads to a significant increase output while maintaining the homogeneity and crystallinity of the product. As the organic solvent can be used monohydroxy alcohols, ketones, monocarboxylic acid. Unsuitable polyhydric alcohols, and solvents having a basic nature: dimethylformamide, triethanolamine, Ethylenediamine, etc.

Example 1 (the prototype).

of 8.4 g of 1-hydroxyethane-1,1-diphosphonic acid THAT 6-09-713-84 mark “h” is dissolved in 0,040 l of water and added 1.2 g of basic cobalt carbonate (II). After dissolving the precipitate obtained solution is evaporated to a volume of 0,010 l when heated to a gentle boil. Precipitated from the hot solution Sadochok washed with ethanol (two portions 0.003 l) and dried in air at room temperature to constant weight. The cobalt 65%.

Found,%: - 9,5; 9,9; 9,6.

Calculated for(C2H7O7P2)2·11H2O%: Co - 8,83.

Example 2 (the prototype).

of 8.4 g of 1-hydroxyethane-1,1-diphosphonic acid are dissolved in 0,040 l of water and added 1.2 g of basic cobalt carbonate (II). After dissolving the precipitate obtained solution is kept at room temperature for evaporation to a volume of 0.017 L. Precipitated precipitate is filtered off on a glass filter THEN 40 under reduced pressure. The precipitate was washed with ethanol (two portions 0.003 l) and dried in air at room temperature to constant weight. The cobalt 60%.

Found, %: Co - 11,3; 11,2.

Calculated for(C2H7O7P2)2·6N2O,%: - OF 10.21.

Example 3.

6.3 g of 1-hydroxyethane-1,1-diphosphonic acid THAT 6-09-713-84 mark “h” and 2.9 g of uranyl nitrate cobalt (II) GOST 4528-78 mark “h” dissolve 0.005 liters of water while heating to a temperature of 50-60°C. the resulting solution was left to crystallize for 2 days at a temperature of 23-25°C. After the precipitation is filtered off on a glass filter THEN 40 under reduced pressure. The precipitate on the filter is washed with ethanol (three portions 0,002 l) and dried in air at room Teso(C2H7O7P2)2·4H2O,%: C - 8,88; N - 4,10; P - 22,90; Co - 10,89.

The infrared spectrum, cm-1: 3580, 3425, 3230, 1405, 1150, 1090, 1075, 1030, 945, 825, 655, 565, 480, 440.

Example 4.

6.3 g of 1-hydroxyethane-1,1-diphosphonic acid and 2.4 g of uranyl chloride cobalt (II) GOST 4525-77 mark “h” dissolve 0.005 liters of water while heating to a temperature of 50-60°C and then proceed as in example 3. The cobalt 82%.

Found, %: C - 8,8; N - 4,2; P - 22,6; Co - 10,7.

The infrared spectrum, cm-1: 3575, 3420, 3230, 1410, 1150, 1090, 1070, 1030, 945, 825, 655, 565, 485, 445.

Example 5.

of 4.2 g of 1-hydroxyethane-1,1-diphosphonic acid and 2.9 g of uranyl nitrate cobalt (II) dissolved 0.005 liters of water while heating to a temperature of 40-50°C. the resulting solution was left to crystallize for 3 days at a temperature of 18-20°C. After the precipitation is filtered off on a glass filter THEN 40 under reduced pressure. The precipitate on the filter is washed with ethanol (four portions 0,001 l) and dried in air at room temperature to constant weight. The cobalt 68%.

Found, %: C - 8,5; 4,1; P - 22,8; -10,9.

Example 6.

6.3 g of 1-hydroxyethane-1,1-diphosphonic acid and 2.9 g of uranyl nitrate cobalt (II) dissolved in 0,008 l of water and then proceed as in example 3. The cobalt 44%.

Middot at 0°C for 1 day. The cobalt 50%.

Found, %: C And 8.6; N - 4,1; P - 22,7; And 10.8.

Example 8.

6.3 g of 1-hydroxyethane-1,1-diphosphonic acid and 2.9 g of uranyl nitrate cobalt (II) dissolved in 0,010 l of water and add 0,010 l acetic acid. The resulting solution was left to crystallize for 1 day at a temperature of 20-22°C. After the precipitation is filtered off on a glass filter THEN 40 under reduced pressure. The precipitate is washed on the filter 0,002 l 80% aqueous solution of acetic acid and ethanol (two portions 0,002 l). Air-dried at room temperature to constant weight. The cobalt 97%.

Found, %: C - 8,9; 4,1; P - 23,1; Co - 10,9.

The infrared spectrum, cm-1: 3580, 3420, 3225, 1405, 1150, 1085, 1070, 1030, 945, 820, 655, 565, 480, 440.

Example 9.

6.3 g of 1-hydroxyethane-1,1-diphosphonic acid and 2.9 g of uranyl nitrate cobalt (II) dissolved in 0,010 l of water and add 0,010 l of acetone. The resulting solution was left to crystallize for 1 day at a temperature of 16-18°C. After the precipitation is filtered off on a glass filter THEN 16 under reduced pressure. The precipitate is washed on the filter 0,002 l 80% aqueous acetone solution and pure acetone (two portions 0,002 l). Air-dried at room temperature until constant weight is 75, 1030, 950, 825, 660, 565, 480, 440.

Example 10.

6.3 g of 1-hydroxyethane-1,1-diphosphonic acid and 2.9 g of uranyl nitrate cobalt (II) dissolved in 0,010 l of water and add 0,010 l of ethanol. The resulting solution was left to crystallize for 4 days at a temperature of 22-24°C. After the precipitation is filtered off on a glass filter THEN 40 under reduced pressure. The precipitate is washed on the filter 0,002 l of an 80% aqueous solution of ethanol and pure ethanol (two portions 0,002 l). Air-dried at room temperature to constant weight. The cobalt 88%.

Found, %: C - 8,8; N - 4,0; R - 23,0; Co - 11,0.

As seen from the above examples 3-10, the proposed methods allow to obtain a homogeneous bis(1-hydroxyethane-1,1-diphosphonate(1-)) cobalt (II), Co(N3L)2·4H2O high yield of product. About the homogeneity of the compounds shows the results of elemental analysis, IR spectra and powder x-ray (see table) preparations of this compound, obtained in different conditions. For powder x-ray products (see table) there are a large number of narrow reflexes that says about their good zakristallizovannykh.

Claims

1. FPIC is cobalt(II) and 1-hydroxyethane-1,1-diphosphonic acid, crystallization of the product, separating the precipitate from the solution and drying, characterized in that prepare a solution with a salt concentration of cobalt(II) of 0.7 to 1.5 mol/l and 1-hydroxyethane-1,1-diphosphonic acid 1.5 to 4.0 mol/L.

2. The method according to p. 1, wherein preparing an aqueous solution with a molar ratio of the salt of cobalt(II):1-hydroxyethane-1,1-diphosphonic acid is 1:(2-3).

3. The method according to p. 1, characterized in that as the salt of cobalt(II) using salt selected from the group consisting of sulfate, sulpham, chloride, perchlorate, nitrate, tetrafluoroborate, hexafluorosilicate, thiocyanate, cobalt(II).

4. The method according to p. 1, characterized in that the crystallization of the product is conducted at temperatures (-5) - 25C.

5. The method of obtaining bis(1-hydroxyethane-1,1-diphosphonate(1-)) cobalt(II), comprising preparing an aqueous solution of salt of cobalt(II) and 1-hydroxyethane-1,1-diphosphonic acid, the crystallization of the product, separating the precipitate from the solution and drying, characterized in that prepare a solution with a salt concentration of cobalt(II) 0.1 to 1.3 mol/l and 1-hydroxyethane-1,1-diphosphonic acid 0.3 to 3.0 mol/l aqueous solution further add miscible with water, an organic solvent.

6. The way Apostolova acid, equal to 1:(2-3).

7. The method according to p. 5, characterized in that the organic solvent used, the solvent is selected from the group consisting of methanol, ethanol, propanol, isopropanol, formic acid, acetic acid, acetone.

8. The method according to p. 5, characterized in that the organic solvent is added in an amount to provide a volumetric ratio of aqueous solution of organic solvent is 1:(0.5 to 5).

 

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