Method for preparing copper (ii) acetate monohydrate

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing copper (II) acetate monohydrate that represents organic carboxylic acid salt. Copper (II) acetate monohydrate is prepared by crystallization from solution obtained by mixing acetic acid, alkaline metal acetates or ammonium with copper-containing spent solution used in etching printing boards. Method provides reducing cost of the proposed method for preparing copper (II) acetate monohydrate, retaining purity of product with simultaneous utilization of toxic waste in electronic engineering manufacture - the spent solution in etching printing boards. Also, invention provides reducing material consumptions in preparing copper (II) acetate monohydrate, expanding assortment of materials used for its preparing and utilization of toxic waste in electronic engineering manufacture. Product obtained by the proposed method can be used as pigment, fungicide and copper microfertilizer in agriculture, as catalyst in processes of polymerization, as a stabilizing agent of artificial fibers, for preparing galvanic solutions and preparing other copper compounds.

EFFECT: improved preparing method.

14 cl, 5 ex

 

The invention relates to the field of chemical technology of organic compounds, in particular to a method for producing acetate monohydrate, copper(II), which can be used as a pigment, fungicide and copper micronutrients in agriculture, the catalyst for the polymerization of organic substances, stabilizers, artificial fibers, for the preparation galvanic solutions, to obtain other compounds of copper.

It is known that an aqueous solution of copper acetate(II) are monoclinic crystals of the monohydrate, copper acetate(II), si(CH3Soo)2·H2O (De Meester, P., Fletcher S.R., Scapski A.C. // Joumal of Chemical Society. Dalton Transactions, 1973, V.23 Supported, P.2575. Brown G.M., R. Chidambaram // Acta Crystallographica, 1973, V.B29, No. 12, P.2393).

Known methods for producing acetate monohydrate, copper(II), comprising preparing an aqueous solution containing copper(II) acetate, as a result of exchange reactions between the acetates of calcium, barium or lead and copper sulfate(II), followed by the separation of precipitation of sulfates of calcium, barium or lead from solution by filtration, concentration of filtrate and crystallization of the product (Guide preparative inorganic chemistry (Ed. by Brauer G)) Of the aliens. lit., 1956, P.472. Ripen R., Cetanu I. Inorganic chemistry. Vol.2. - M.: Mir, 1972, S). These methods are based on reactions:

CuSO4+is a(CH 3Soo)2+2H2About→ si(CH3Soo)2+CaSO4·2H2O↓

CuSO4+VA(CH3Soo)2Si(CH3Soo)2+BaSO4

CuSO4+Pb(CH3Soo)2Si(CH3Soo)2+PbSO4.

The disadvantage of these methods is the need for additional costs for filtration and evaporation of the solution and also costs for reagent copper sulfate(II).

Known methods for producing acetate monohydrate, copper(II), consisting in the preparation of an aqueous solution containing copper(II) and acetate by dissolving metallic copper in the presence of oxygen), copper oxide(II)hydroxide copper(II), the basic carbonate of copper(II), basic copper acetate(II) in acetic acid, followed concentrated solution by evaporation and crystallization of the product (Guide preparative inorganic chemistry (Ed. by Brauer G)) Of the aliens. lit., 1956, P.472. Ripen R., Cetanu I. Inorganic chemistry. Vol.2. - M.: Mir, 1972, S. Remy, the Rate of inorganic chemistry. Vol.2. - M.: Mir, 1974, S). These methods are based on the following reactions:

Si+SN3COOH+O2Si(CH3Soo)2·H2About

SiO+2CH3COOH→ si(CH3Soo)2·H2O

Si(OH)2+2CH3WITH THE H→ Si(CH3Soo)2·H2O+H2O

Si(OH)2·ISSS3+SN3COOH→ si(CH3Soo)2·H2O+CO2+H2O

Hsi(OH)2·Wuxi(CH3Soo)2·z2O+HCN3COOH→

(x+y)si(CH3Soo)2·H2O+(z+x-y)H2O

The disadvantage of these methods is the need for additional cost heating solution and the cost of copper-containing reagents.

Closest to the claimed method is a method of producing acetate monohydrate, copper(II), comprising preparing a reaction solution containing copper(II) acetate, crystallization of the product, separating the crystals from the solution and drying (Karyakin J.V., Angels I.I. Pure substances. - M.: Chemistry, 1974, S). The reaction solution in the prototype is prepared by adding a basic carbonate of copper(II) 11%aqueous solution of acetic acid when heated to 60°C. and then concentrated by evaporation up to 1/3 of original volume. Crystallization of the product is carried out at a cooling solution. Crystals separated from the solution by filtration under reduced pressure and dried at room temperature. The way the prototype provides clear acetate monohydrate, copper(II) with the output of the m 80-88%. The disadvantage of this method is the need for the extra cost of heating and evaporation of the reaction solution and the cost of the reagent is a basic carbonate of copper(II).

In the claimed invention, the aim was to reduce material costs acetate monohydrate, copper(II) and to dispose of toxic waste production.

This is achieved by a method of producing acetate monohydrate, copper(II) involves preparing a reaction solution containing copper(II) acetate, crystallization of the product, separating the crystals from the solution and drying. New this method is that the reaction solution is prepared by mixing reagent, which is the source of acetate, and electronic waste production waste solution etching of printed circuit boards, and the reaction solution establish a pH of from 0.5 to 7.0 and the molar ratio of copper(II) acetate, 1.0:(2,0-25,0). As the spent solution from the etching of printed circuit boards, it is desirable to use a solution containing copper(II)ammonia, ammonium chloride, or a solution containing copper(II)ammonia, ammonium chloride, ammonium carbonate, or a solution containing copper(II)ammonia, ammonium sulfate, or a solution containing copper(II)ammonia, ammonium sulfate, peroxodisulfate ammonium, and as a reagent, which is the source of acetate - acetic Ki the lot or acetic and hydrochloric acids. As the spent solution from the etching of printed circuit boards is also desirable to use a solution containing copper(II), hydrochloric acid, or a solution containing copper(II), hydrochloric acid, ammonium chloride, or a solution containing copper(II), sulfuric acid, peroxodisulfate ammonium, and as a reagent, which is the source of the acetate, acetic acid and sodium hydroxide or acetic acid and potassium hydroxide or acetic acid and ammonium hydroxide, or sodium acetate or potassium acetate, or ammonium acetate. As a reagent, which is the source of acetate, it is desirable to use waste product containing acetic acid or sodium acetate or potassium acetate, or ammonium acetate. Crystallization of the product are preferably at a temperature of from -5 to 60°C.

The method of producing acetate monohydrate, copper(II) is preparing a reaction solution by adding acetic acid to the well-tested copper-ammonium solution etching of printed circuit boards or acetate of sodium, potassium, ammonium worked to the acid solution in the etching of printed circuit boards, adjusted (if necessary) the pH of the reaction solution, the allocation of acetate monohydrate, copper(II) in the form of a crystalline precipitate, separating the precipitate from the solution by the known methods of washing (if necessary) sludge solvent, is sosiani sediment in the air.

Used solutions etching of printed circuit boards (copper-ammonia - based copper(II)ammonia, ammonium chloride, copper-alkaline - based copper(II)ammonia, ammonium chloride, ammonium carbonate, copper sulphate - based copper(II)ammonia, ammonium sulfate, peroxodisulfate - based copper(II)ammonium sulphate, peroxodisulfate ammonium, ammonia or sulfuric acid, acid - based copper(II), hydrochloric acid or copper(II), hydrochloric acid, ammonium chloride) are toxic electronic waste production and are subject to neutralization (Fedulova AA., Ustinov Y.A., Cats, H.E., Shustov VP, AVIC E.R. multilayer printed circuit boards. - M.: Radio and communication, 1990, S), which requires significant material costs. Acetic acid GOST 61-75, sodium hydroxide GOST 4328-77, sodium acetate GOST 199-78, ammonium acetate GOST 3117-78 produced by the chemical industry and have low cost. In addition, to obtain acetate monohydrate, copper(II) can be recycled food and reactive acetic acid and acetates of alkali metals or ammonium. With the addition of these reagents to waste etching solutions PCB occur following chemical reaction:

[Cu(NH3)4]Cl2+2CH3COOH+2hcl+H2About→ si(CH3Soo)2·H2O+4NH4Cl/p>

[Cu(NH3)4]SO4+SN3COOH+H2O→ si(CH3Soo)2·H2O+(NH4)2SO4+2CH3COOH

(NH4)2[CuCl4]+2CH3COOH+2NaOH→ si(CH3Soo)2·H2O+2NH4Cl+2NaCl+H2O

H2[CuCl4]+SN3The N+H2O→ si(CH3Soo)2·H2O+2CH3COOH+4NaCl.

The result of the reaction solution is highlighted crystalline monohydrate, copper acetate(II). The proposed method allows to obtain the acetate monohydrate, copper(II) using available and inexpensive reagents acetic acid, sodium hydroxide, sodium acetate, ammonium acetate without using a copper-containing reagent and simultaneously dispose of waste electronic and chemical industries.

To obtain acetate monohydrate, copper(II) it is desirable to use waste solutions etching of printed circuit boards containing copper(II)ammonia, ammonium chloride, ammonium sulfate, hydrochloric acid, sulfuric acid, which have a composition, for example:

Copper(II) (in the form of ammonium complex) 50-120 g/l

Ammonia 50-100 g/l

Ammonium chloride 50-150 g/l

or

Copper(II) (in the form of ammonium complex) 50-120 g/l

Ammonia 30-100 g/l

Ammonium chloride 5-50 g/l

Ammonium carbonate 20-400 g/l,

or

Copper(II) (in the form of Ammi is knogo complex) 60-100 g/l

Ammonia 80-130 g/l

Ammonium sulfate 30-100 g/l,

or

Copper(II) (in the form of chlorocomplexes) 80-140 g/l

Hydrogen chloride 10-30 g/l

Ammonium chloride 50-150 g/l

To obtain acetate monohydrate, copper(II) it is desirable to install in the reaction solution, the optimum pH value. The acetate monohydrate, copper(II) soluble in water, and its solubility increases in the presence of strong acids (sulfuric, hydrochloric, nitric), so if the pH is less than 0.5, the output acetate monohydrate, copper(II) is significantly reduced. The experimental data at pH 7.0 to 9.0 acetate monohydrate, copper(II) polluted basic salts of copper(II); at pH greater 9.0 acetate monohydrate, copper(II) from solution does not fall, as the copper(II) in solution is related to the complex [Cu(NH3)4]2+. Therefore, to obtain pure acetate monohydrate, copper(II) with high yield, it is desirable to prepare the reaction solution with a pH from 0.5 to 7.0.

To obtain pure acetate monohydrate, copper(II) with high yield, it is desirable to prepare a reaction solution containing copper(II) acetate in an optimal molar ratio. The experimental data from solutions in which 1.0 mol of copper(II) is less than 2.0 mol of acetate, roll the mixture of acetate monohydrate, copper(II) basic salts of copper(II). From solutions in which 1.0 mol of copper(II) is 2.0 or more mol of acetate, falls h is a simple acetate monohydrate, copper(II) with high yield of copper(II), but the yield on acetate with changing the molar ratio of copper(II) acetate is reduced, which leads to wasteful consumption of acetate. Therefore, to obtain pure acetate monohydrate, copper(II) high yield it is necessary to prepare the reaction solution containing copper(II) acetate in a molar ratio 1,0:(2,0-25,0).

The solubility of the monohydrate, copper acetate(II) increases with the temperature of the solution; the solution of copper acetate(II) resistant to 66°C (Guidance preparative inorganic chemistry (Ed. by Brauer G)) Of the aliens. lit., 1956, P.472), so to increase output and receive acetate monohydrate, copper(II) without admixture of basic salts of copper(II) crystallization is carried out at a temperature of preferably from -5 to 60°C.

The acetate monohydrate, copper(II) well-crystallized from aqueous solutions, the precipitate is easily deposited without forming colloidal particles, therefore, to its separation from the mother liquor can be applied to many well-known methods (e.g., filtration under normal or reduced pressure, centrifugation).

In the process of filtering the precipitate is easily separated from the mother liquor. If you need a more complete removal of the substances present in the mother solution, the precipitate is washed on the filter with a suitable solvent, such as chilled water, aqueous solution of acetic acid, this is I, the acetone.

The acetate monohydrate, copper(II) not oxidized by oxygen and stable in air up to 100°C. the Dried product can be carried out at ordinary temperature, or to speed up the process of drying in a current of air at ordinary temperature or when heated to a temperature of 40-80°C.

Example 1.

To 10.0 ml of the spent solution from the etching of printed circuit boards with copper(II) 1.5 mol/l, ammonia 3.3 mol/l, ammonium chloride and 0.2 mol/l of ammonium carbonate and 3.6 mol/l add first 10 ml of water, then with stirring, 20 ml of acetic acid, GOST 61-75 marks “h”. The solution is left to crystallize for 1 day at a temperature of 18°C. the Precipitate is filtered off on a glass filter, THEN 100, washed with acetone and dried in air at room temperature to constant weight. Yield 82%.

Found, %: C - 23,9; N - 4,0; Si - 31,7.

Calculated for si(CH3Soo)2·H2O, %: 24,06; N - 4,04; Si - 31,83.

Example 2.

To 10.0 ml of the spent solution from the etching of printed circuit boards with copper(II) 1.7 mol/l, ammonium chloride 1.5 mol/l, chloride of 0.4 mol/l with stirring, is added first to 2.9 ml of acetic acid, GOST 61-75 marks “analytical grade”, then portions of 0.5 ml of 30%solution of sodium hydroxide to achieve a pH of 3.0. The solution is left to crystallize for 1 day at a temperature of 22°C. the Precipitate is filtered off on Stekla the nom filter THEN 40 under reduced pressure, washed with 70%aqueous solution of acetic acid and dried in air at room temperature to constant weight. Yield 72%.

Found, %: C - 24,2; N - 3,8; C To 31.8.

Example 3.

To 10.0 ml of the spent solution from the etching of printed circuit boards with copper(II) 0.96 mol/l, ammonia and 7.3 mol/l of ammonium sulfate to 0.45 mol/l is added first with 6.5 ml of water, then 17.5 ml of an 80%aqueous solution of acetic acid, THE 6-09-07-1716-95. The solution is kept for crystallization at 20 h at 20°C. the Precipitate is filtered off on a glass filter THEN 16 under reduced pressure, washed with 50%aqueous solution of acetic acid and dried in air at room temperature to constant weight. Yield 72%.

Found, %: C - 24,1; N - 3,9; Si - 32,2.

Example 4.

To 10.0 ml of the spent solution from the etching of printed circuit boards with copper(II) 1.7 mol/l, ammonium chloride 1.5 mol/l, chloride of 0.4 mol/l with stirring was added a solution 6,94 g three-hydrate sodium acetate, GOST 199-78 mark “h” in 5.0 ml heated to 40°With water. The solution is kept for crystallization at 1.5 h at 20°C. the Precipitate is filtered off on a glass filter THEN 40 under reduced pressure, washed with chilled water and dried in air at room temperature to constant weight. Yield 88%.

Found, %: C - 23, 8mm; N - 3,7; C To 31.8.

Example 5.

To 10.0 ml of spent Rast is ora etching of printed circuit boards with copper(II) 1.1 mol/l, ammonia 4.2 mol/l of ammonium chloride and 0.4 mol/l with stirring, add 10 ml of acetic acid, GOST 61-75 marks “chemically pure”. The solution is left to crystallize for 2 days at a temperature of 0°C. the Precipitate was washed with 70%aqueous solution of acetic acid, press on filter paper and dried in air at room temperature to constant weight. Yield 86%.

Found, %: C - 23,7; N - 3,9; Si - 31,7.

Obtained in examples 1-5 acetate monohydrate, copper(II) is a crystalline substance of a dark green colour, soluble in water, glycerol, dimethylformamide, dimethyl sulfoxide, slightly soluble in ethanol, acetone, acetic acid, slightly soluble in carbon tetrachloride, benzene.

As seen from the above examples, the claimed method allows high yield monohydrate, copper acetate(II), exactly corresponding to the formula si(CH3Soo)2·H2O. the Reduction of material costs for the product is due to the fact that as a reagent instead of copper(II) use copper-containing waste solutions etching of printed circuit boards of different composition. Simultaneously with obtaining a valuable product cannot be disposed of toxic electronic waste production, reduce the cost of environmental protection.

1. Way to obtain is novedrate copper acetate(II), comprising preparing a reaction solution containing copper(II) acetate, crystallization of the product, separating the crystals from the solution and drying, characterized in that the reaction solution is prepared by mixing reagent, which is the source of acetate, and the extract solution etching of printed circuit boards, and the reaction solution establish a pH of from 0.5 to 7.0 and a molar ratio of copper(II) acetate, equal 1,0 : (2,0-25,0).

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

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

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

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

6. The method according to claims 1 to 5, characterized in that, as a reagent, which is the source of acetate using acetic acid.

7. The method according to claims 1 to 5, characterized in that, as is eagent, which is the source of acetate using acetic acid and hydrochloric acid.

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

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

10. The method according to claim 1, characterized in that the spent solution from the etching of printed circuit boards using a solution containing copper(II), sulfuric acid, ammonium sulfate, peroxodisulfate ammonium.

11. The method according to claim 1,8-10, characterized in that, as a reagent, which is the source of acetate using acetic acid and sodium hydroxide or acetic acid and potassium hydroxide or acetic acid and ammonium hydroxide.

12. The method according to claim 1,8-10, characterized in that, as a reagent, which is the source of acetate using sodium acetate or potassium acetate, or ammonium acetate.

13. The method according to claims 1 to 5, 8-10, characterized in that, as a reagent, which is the source of acetate, using a waste product containing acetic acid or sodium acetate or potassium acetate, or ammonium acetate.

14. The method according to claim 1, characterized in that the crystallization of the product is carried out at a temperature of from is 5 to 60° C.



 

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