The method of obtaining dihydrate bis(1-hydroxyethane-1,1 - diphosphonate(2-)) cuprate (ii) ammonium

 

(57) Abstract:

The invention relates to a method for dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium, which is as follows: dehydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium is produced by crystallization from a solution prepared by mixing the spent solution from the etching of printed circuit boards containing copper(II) and ammonia or ammonium salts, and 1-hydroxyethane-1,1-diphosphonic acid in an amount to provide a molar ratio of copper(II):1-hydroxyethane-1,1-diphosphonic acid 1.0:(2,0-4,0), and having a pH value preferably of 2.0 to 3.5. The product obtained in this way can be used for antibacterial treatment of water for protection against corrosion of equipment in the oil-producing, oil-refining, pulp and paper industry, as a fungicide and copper micronutrients in agriculture, for the preparation of electrolyte galvanic copper plating, for other copper complexes. The technical result - the reduction of dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium, while maintaining its phase homogeneity with simultaneous disposal of toxic waste radio is>sabreena relates to chemical technology of organophosphorus substances, in particular to a method for producing complex (chelate) copper(II) with 1-hydroxyethane-1,1-diphosphonic acid CH3S(HE)(RHO3H2)2[C2H8O7P2] the composition (NH4)2Cu(C2H6O7P2)2·2H2O, which can be used for antibacterial treatment of water for protection against corrosion of equipment in the oil-producing, oil-refining, pulp and paper industry, as a fungicide and copper micronutrients in agriculture, for the preparation of electrolyte galvanic copper plating, for other copper compounds.

A method of obtaining dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium composition (NH4)2C(C2H6O7P2)2·2H2O by precipitation with acetic acid from aqueous solution prepared by mixing solutions of the chloride or nitrate of copper(II) and 1-hydroxyethane-1,1-diphosphonate(1-) ammonia in a molar ratio of 1:3 [Afonin E., Synthesis and disproportionation in aqueous solution of bis[1-hydroxyethane-1,1-diphosphonate(2-)]cuprate(II) ammonium//Journal of General chemistry. - 2000. - So is she).

Closest to the proposed invention is a method of obtaining dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-cuprate(II) ammonium by crystallization from a solution prepared by mixing an aqueous solution of salt of copper(II) (chloride or nitrate) solution of 1-hydroxyethane-1,1-diphosphonate(1-)ammonium and ammonia solution taken in a molar ratio of 1:3:3 [Afonin E., Synthesis and disproportionation in aqueous solution of bis[1-hydroxyethane-1,1-diphosphonate(2-)]cuprate(II) ammonium//Journal of General chemistry. - 2000. - So 70. No. 9. - S. 1433]. The disadvantage of this method is the need for the extra cost of the reagents CuCl2·H2O or C(NO3)2·3H2O, and the use of the reagent NH4(C2H7O7P2)·2H2O not produced by the chemical industry.

In the claimed invention, the aim was to reduce the dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium, while maintaining its phase homogeneity and to dispose of toxic waste production.

This is achieved by a method of obtaining dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium includes the preparation of a solution containing copper(II) ammonium 1-gidroksidov this method is the fact, that solution is prepared by mixing the spent solution from the etching of printed circuit boards containing copper(II) and ammonia or ammonium salts, and 1-hydroxyethane-1,1-diphosphonic acid in an amount to provide a molar ratio of copper(II):1-hydroxyethane-1,1-diphosphonic acid 1.0:(2,0-4,0), preferably equal to 1.0:(2.1 to 3.0). As the spent solution from the etching of printed circuit boards it is necessary to use a solution containing copper chloride(II), ammonium chloride and ammonia, or a solution containing copper chloride(II), ammonium chloride, ammonia, carbonate of ammonia, or a solution containing copper chloride(II), ammonium chloride, hydrochloric acid, with the concentration of copper(II) above 0.1 mol/L. it is Desirable to prepare a solution by mixing the spent solution from the etching of printed circuit boards and 1-hydroxyethane-1,1-diphosphonic acid, taken in the form of a solid reagent or an aqueous solution with a mass fraction of 1-hydroxyethane-1,1-diphosphonic acid 10-70%. Preferably, the solution containing copper(II) ammonium 1-hydroxyethane-1,1-diphosphonic acid had a pH value of 2.0 to 3.5, which it is desirable to create by adding 25% ammonia solution. Crystallization of the product are preferably at a temperature (-5)-25S.

The method of obtaining dihydrate bis(1-hydroxy what its aqueous solution to the exhaust solution etching of printed circuit boards, containing copper(II) and ammonia or ammonium salts, adjusted (if necessary) pH by adding ammonia solution, the allocation of the dihydrate crystalline precipitate of bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium, the separation of crystals from a solution of known methods (for example, methods of centrifugation, filtration under reduced pressure), washing (if necessary) the precipitate with a solvent, drying the precipitate in air at room temperature.

Used solutions etching of printed circuit boards (copper-alkaline - chloride of copper(II), ammonium carbonate, ammonium chloride, ammonia; copper-ammonium - chloride of copper(II), ammonium chloride, ammonia; acid - chloride of copper(II), ammonium chloride, hydrochloric acid) are toxic electronic waste production and are subject to neutralization, which requires the cost of their neutralization [Fedulova A. A., Ustinov, J. A., Kotov, E. P., Shustov B. N., AVIC E. R. Technology of multilayer printed circuit boards. - M.: Radio and communication, 1990, S. 191. OST 107.460092.004.01-86. Cards printed. Standard processes. H 1, 1987, S. 284]. 1-Hydroxyethane-1,1-diphosphonic acid is produced by the chemical industry on THE other 6-09-713-84 and THE 6-09-20-174-90. Therefore, p is s, using available reagent - 1-hydroxyethane-1,1-diphosphonic acid, but at the same time to dispose of toxic waste production. This forms a pure and single phase product with high yield.

As the spent solution from the etching of printed circuit boards it is possible to use solutions containing copper(II) ammonia or ammonium salts, for example mededeling, copper-ammonia, acidic [Fedulova A. A., Ustinov, J. A., Kotov, E. P., Shustov B. N., AVIC E. R. Technology of multilayer printed circuit boards. - M.: Radio and communication, 1990, S. 186. OST 107.460092.004.01-86. Cards printed. Standard processes. H 1, 1987, S. 234]. It is undesirable to use solutions on the basis of ammonium persulfate, sodium chlorite, as these components of the solution can oxidize 1-hydroxyethane-1,1-diphosphonic acid. You cannot use a solution of chloride of iron(III), as the iron forms with 1-hydroxyethane-1,1-diphosphonic acid residue complex.

1-Hydroxyethane-1,1-diphosphonic acid is soluble in water and quickly reacts in solution with copper(II), therefore, for preparation of a solution containing copper(II) ammonium 1-hydroxyethane-1,1-diphosphonic acid, to exhaust solution etching printed circuit boards are added or solid 1-hydroxyethane-1,1-diphosphonate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium in water is quite high and is 0.133 mol/l at 25 ° C [Afonin E., Synthesis and disproportionation in aqueous solution of bis[1-hydroxyethane-1,1-diphosphonate(2-)]cuprate(II) ammonium//Journal of General chemistry. - 2000. - So 70. No. 9. - S. 1433]. It decreases with increase in the concentration in solution of ammonium ions, 1-hydroxyethane-1,1-diphosphonate ions and some other ions. Therefore, to obtain a product with high concentration of copper(II) in the extract solution etching printed circuit boards shall be not lower than 0.1 mol/L. Typically used solutions etching of printed circuit boards contain copper(II) in a concentration of 0.5 to 2.5 mol/l, the washing water of the first washing 0.01 to 0.2 mol/L.

The experimental data net dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium without admixture of other complexes of copper(II) with 1-hydroxyethane-1,1-diphosphonic acid crystallizes from aqueous solutions containing 1-hydroxyethane-1,1-diphosphonic acid and copper(II) in a molar ratio higher than 2.0:1.0 in. For example, according to elemental analysis and x-ray diffraction of powder, sludge precipitated from a solution containing 1-hydroxyethane-1,1-diphosphonic acid and copper(II) in a molar ratio of 2.0:1.0 that represents the dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium (NH4)2Cu(C2H6O7P22O. the Precipitate deposited from a solution containing 1-hydroxyethane-1,1-diphosphonic acid and copper(II) in a molar ratio of 2.1:1.0 that represents a pure single-phase substance (NH4)2C(C2H6O7P2)2·2H2O without admixture of other substances. A further increase in molar ratio of 1-hydroxyethane-1,1-diphosphonic acid:copper(II) leads to increased product yield of copper(II), but reduces the yield on 1-hydroxyethane-1,1-diphosphonic acid. Therefore, the optimal molar ratio of 1-hydroxyethane-1,1-diphosphonic acid:copper(II) providing a single-phase product with a high yield, is (2.1 to 3.0):1,0.

The experimental data, pure dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium crystallizes from aqueous solutions having a pH value below a 3.5. From solutions having a pH value above a 3.5, can drop the mixture of (NH4)2C(C2H6O7P2)2·2H2O and (NH4)2Cu3(C2H6O7P2)2·4H2O. From solutions having a pH below 3.5-inch, crystallized pure substance (NH4)2C(C2H6O7P2)2·2H2O; its output decreases aluchemie single-phase product with high yield, is 2,0-3,5.

The dihydrate solubility of bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium in water increases significantly with increasing solution temperature [Afonin E., Synthesis and disproportionation in aqueous solution of bis[1-hydroxyethane-1,1-diphosphonate(2-)]cuprate(II) ammonium//Journal of General chemistry. - 2000. - So 70. No. 9. - S. 1433], therefore, the crystallization of the product should be carried out at ordinary temperature or cooled solution.

Example 1 (the prototype).

7,8 g dihydrate 1-hydroxyethane-1,1-diphosphonate(1-) ammonium dissolved in 9 ml of water, add a 2.45 ml of 25% ammonia solution (density 0,906 g/cm3) and a solution of 1.7 g of chloride dihydrate, copper(II) in 5 ml of water. After 5 hours the solution is poured, the precipitate washed with 5 ml of aqueous ethanol (1:1), press on the filter paper. Dried in air at room temperature to constant weight. The output of copper 96%.

Found, %: N 5,2; P 22,6; C 11,7.

Calculated for (NH4)2Cu(C2H6O7P2)2·2H2O, %: N 5,15; P 22,79; Si Of 11.69.

Example 2.

To 10.0 ml of the spent solution from the etching of printed circuit boards with copper(II) of 1.65 mol/l of ammonium chloride and 0.15 mol/l of ammonium carbonate to 3.52 mol/l, AMIA is The 6-09-713-84 mark “h” in 7 ml of water. The next day the precipitate is filtered off on a glass filter THEN 40 under reduced pressure, washed with aqueous ethanol (1:1) (with three portions of 2 ml) and ethanol (two servings 2 ml). The precipitate is dried in air at room temperature to constant weight. The output of copper to 98.5%.

Found, %: N 5,1; P 23,0; C 11,6.

Example 3.

To 10.0 ml of the spent solution from the etching of printed circuit boards with copper(II) of 1.65 mol/l of ammonium chloride and 0.15 mol/l of ammonium carbonate to 3.52 mol/l, ammonia 2,85 mol/l was added with stirring in portions of 1 ml of a solution of 10.4 g of 1-hydroxyethane-1,1-diphosphonic acid in 30 ml of water and with stirring, dropwise 25% ammonia solution to achieve a pH of 3.0. The next day the precipitate is filtered off on a glass filter THEN 40 under reduced pressure, washed with aqueous ethanol (1:1) (three portions 3 ml) and ethanol (three portions 3 ml). The precipitate is dried in air at room temperature to constant weight. The output of copper 73%.

Found, %: N 5,0; R 22,7; C 11,8.

Example 4.

To 10.0 ml of the spent solution from the etching of printed circuit boards with copper(II) 1.18 mol/l, ammonium chloride 1.06 mol/l, ammonia of 1.65 mol/l was added with stirring in portions of 1 lannom the filter THEN 40 under reduced pressure, washed with aqueous ethanol (1:1) (with three portions of 2 ml) and ethanol (two servings 2 ml). The precipitate is dried in air at room temperature to constant weight. The output of copper 97%.

Found, %: N 5,1; R 22,5; C 11,7.

Example 5.

To 10.0 ml of the spent solution from the etching of printed circuit boards with copper(II) 1.70 mol/l of ammonium chloride to 2.40 mol/l, chloride of 0.27 mol/l was added a solution of 7.50 g of 1-hydroxyethane-1,1-diphosphonic acid in 8 ml of water and with stirring, dropwise 25% ammonia solution to achieve a pH of 2.8. After 2 hours the precipitate is filtered off on a glass filter THEN 100 under reduced pressure, washed with aqueous ethanol (1:1) (two servings 2 ml) and ethanol (three portions 3 ml). The precipitate is dried in air at room temperature to constant weight. The output of copper 98 %.

Found, %: N 4,9; P 22,8; C 11,7.

According to elemental analysis, the preparations obtained by the proposed method (examples 2-5), have the composition (NH4)2C(C2H6O7P2)2·2H2O. According to the chest x-ray powder diffractometer DRON-3, SiC-radiation, Ni-filter, 2=3-60) obtained in examples 2-5 drugs dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))other complexes of copper(II) with 1-hydroxyethane-1,1-diphosphonic acid. Proof of this is the full agreement between the experimental x-ray powder and x-rays, computed according to x-ray analysis of the single crystal of the dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium [Sergienko, B. C., Alexander, G., Afonin E., Crystal structure of dihydrate ammonium salt [catenate(-1-hydroxyethane-1,1-diphosphonate)copper(II)] (NH4)2[Cu(H2L)2]·2H2O //Coordination chemistry. - 1998. - So 24. No. 6. - S. 455] (see table).

As seen from the above examples 2-5, the proposed method allows to obtain high (up to 99.5%) output single-phase dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium, while reducing material costs to obtain, because instead of the salts of copper(II) use tried and tested solutions etching printed circuit boards. This leads to a reduction in the cost of the product and at the same time allows you to dispose of toxic waste production, reduce the cost of environmental protection.

1. The method of obtaining dihydrate bis(1-hydroxyethane-1,1-diphosphonate(2-))cuprate(II) ammonium, comprising preparing a solution containing copper(II) ammonium 1-hydroxyethane-1,1-diphosphonic acid is p prepared by mixing the spent solution from the etching of printed circuit boards, containing copper(II) and ammonia or ammonium salts, and 1-hydroxyethane-1,1-diphosphonic acid in an amount to provide a molar ratio of copper(II):1-hydroxyethane-1,1-diphosphonic acid 1.0:(2,0-4,0).

2. The method according to p. 1, characterized in that the spent solution from the etching of printed circuit boards using a solution containing copper chloride(II), ammonium chloride, ammonia.

3. The method according to p. 1, characterized in that as the spent solution from the etching of printed circuit boards using a solution containing copper chloride(II), ammonium chloride, ammonia, carbonate of ammonia.

4. The method according to p. 1, characterized in that the spent solution from the etching of printed circuit boards using a solution containing copper chloride(II), ammonium chloride, hydrochloric acid.

5. The method according to PP.2-4, characterized in that the spent etching solution PCB contains copper(II) in a concentration above 0.1 mol/L.

6. The method according to p. 1, wherein the solution prepared with a molar ratio of copper(II):1-hydroxyethane-1,1-diphosphonic acid 1.0:(2.1 to 3.0).

7. The method according to p. 1, wherein the solution is prepared by mixing the spent solution from the etching of printed circuit boards and 1-hydroxyethane-1,1-diphospho is about acid 10-70%.

8. The method according to p. 1, characterized in that the solution containing copper(II) ammonium 1-hydroxyethane-1,1-diphosphonic acid, has a pH value of 2.0 to 3.5.

9. The method according to p. 8, characterized in that the pH value of 2.0 to 3.5 created by adding 25% ammonia solution.

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

 

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