Method of preparation of phosphonic electrolytes and solutions

FIELD: metallurgy.

SUBSTANCE: invention refers to electrolytic metallurgy and can be used at preparation of phosphonic complex electrolytes for electrochemical and chemical copper, zinc, nickel and cobalt coating. The method includes solution of such compounds in water, which are the source of cations of metals, and solution of a compound, which is the source of anion of nitrilotri(methylene phosphonic) acid; at that as sources of cations of metals and anion of nitrilotri(methylene phosphonic) acid crystal nitrilotri-(methylenphosphonates)(2-) of metals are used from the group containing copper, zinc, nickel and cobalt.

EFFECT: facilitates preparation of complex phosphonic electrolytes and solutions of specified composition and concentration not containing undesirable impurities, it also facilitates upgraded processibility of the method of preparation of electrolytes and solutions, and expands an arsenal of existing methods of preparation of nitrilotri-(methylenphosphonates) electrolytes and solutions for coating with metals and alloys.

5 cl, 6 ex

 

The invention relates to electroplating, and in particular to methods for preparation of comprehensive and electrolytes to obtain electroplating copper, zinc, Nickel, cobalt and solutions for the production of chemical coatings of copper, Nickel, cobalt.

The invention allows to prepare non-toxic phosphonate electrolytes and solutions containing complex compounds of copper(II), zinc(II), Nickel(II), cobalt(II) with nitrilotri(methylenephosphonic) acid N - (CH2PO3H2)3(C3H12NO9P3), from which the influence of an electric current or chemical reductants can be obtained coating these metals or their alloys on steel, copper, aluminium and their alloys.

Phosphonate electrolytes, which recently have been used in the galvanic production, allow to obtain galvanic and chemical metal coating having a set of unique physical and chemical properties (crystalline structure, high microhardness while maintaining chemical purity and ductility of the metal coating, high scattering power that supersedes even for cyanide electrolytes, no porosity). In combination with toxicity, high stability of the composition and efficacy of f is spontania electrolytes are essential when applying coatings on parts of precision mechanics and electronic engineering.

Expansion of the range of types of metallic coatings obtained from phosphonate electrolytes, requires the development of new methods of preparation of these electrolytes and fluids, because they differ from the traditional.

A known method of preparation of the phosphonate electrolytes to obtain electroplating metals (copper, zinc, Nickel)containing as the main components of the cations of these metals and anion nitrilotri(methylenephosphonic) acid, which comprises dissolving in water of the compounds that are the source of metal cations(II) (copper, zinc, Nickel), and connection, which is the source of anion nitrilotri(methylenephosphonic) acid (X. Kowalski US 3706634, publ. 19.12.1972). As compounds which are sources of metal cations(II) (copper, zinc, Nickel), use a water-soluble metal salts(II) with non-oxidizing anions, such as sulfates, phosphates, chlorides, acetates, citrates. As a connection, which is the source of anion nitrilotri(methylenephosphonic) acid is used nitrilotri(methylenephosphonic) acid or its salts with alkali metals and ammonium.

A known method of preparation of the phosphonate solutions for the production of chemical coatings metals (copper, Nickel, cobalt), which contain as main components of these cations m is for metal(II) and anion nitrilotri(methylenephosphonic) acid, including the dissolution in water of the compounds that are the source of metal cations(II), and compounds, which are a source of anion nitrilotri(methylenephosphonic) acid (Mellory G.O., Johnson C.E. DE 2942792, publ. 30.04.1980). As compounds that are the source of metal cations(II) (copper, Nickel, cobalt), using soluble or moderately soluble metal salts(II), for example chloride, nitrate, sulfate copper(II)chloride, sulpham, sulfate Nickel(II)chloride cobalt(II). As a connection, which is the source of anion nitrilotri(methylenephosphonic) acid is used nitrilotri(methylenephosphonic) acid and its salts with alkali metals and ammonium, in particular pentanitrate salt nitrilotri(methylenephosphonic) acid.

How US 3706634, DE 2942792 based on the reactions, for example:

CuSO4+K6C3H6NO9P3→K4CuC3H6NO9P3+K2SO4

Cu(NO3)2+Na5C3H7NO9P3+NaOH→Na4CuC3H6NO9P3+2NaNO3+H2O

Ni(CH3COO)2+C3H12NO9P3+6KOH→K4NiC3H6NO9P3+2CH3COOK+6H2O

How US 3706634, DE 2942792 allow you to prepare phosphonate electrolytes and solutions containing complex nitrilotri(methylenephosphonic the s) metal(II), they also anions metal salt(II) (chloride, nitrate, sulfate, sulpham, acetate and others) and the cations of the salt nitrilotri(methylenephosphonic) acid (cations of alkali metals and ammonium), the presence of which in the General case is not desirable. In addition, when using the way US 3706634 is an increase in the salt concentration in the electrolyte, which complicates the preparation of the electrolyte with a high concentration of complex nitrilotri(methylenephosphonate) metal(II). The disadvantage of these methods is that when used as a source of anion nitrilotri(methylenephosphonic) acid produced by the domestic industry nitrilotri(methylenephosphonic) acid, THE 2439-347-05763441-2001, with the content of the basic substance 90-96% or disodium salt nitrilotri(methylenephosphonic) of THE acid, 6-09-20-243-94, with the content of the basic substance 95-96% hit in electrolytes and solutions of undesirable substances (chlorides, phosphorous acid, phosphorus and other substances).

Closest to the claimed method is the preparation of phosphonate electrolytes to obtain electroplating metals (copper, zinc, Nickel), which contain as main components cations of these metals and anion nitrilotri(methylenephosphonic) acid, comprising dissolving in water to connect the clusters, which is the source of cations of metals(II) (copper, zinc, Nickel) and anion nitrilotri(methylenephosphonic) acid (X. Kowalski US 3706634, publ. 19.12.1972). As compounds which are sources of metal cations(II) (copper, zinc, Nickel), in the method according to the prototype using the oxide or carbonate of the metal(II), for example, zinc oxide, copper carbonate, Nickel carbonate. As a connection, which is the source of anion nitrilotri(methylenephosphonic) acid is used nitrilotri(methylenephosphonic) acid, or salt nitrilotri(methylenephosphonic) acids with alkali metals, or nitrilotri(methylenephosphonic) acid with the addition of a carbonate of an alkali metal. The way the prototype is based on the reactions, for example:

ZnO+C3H12NO9P3+2K2CO3→K4ZnC3H6NO9P3+3H2O+2CO2

Ni2(OH)2CO3+2C3H12NO9P3→2NiC3H10NO9P3+3H2O+CO2

The way the prototype allows you to prepare electrolyte solutions containing other anions, except anion nitrilotri(methylenephosphonic) acid. However, when used for the preparation of electrolytes produced by the domestic industry nitrilotri(methylenephosphonic) acid, THE 2439-347-05763441-2001, with the content of the basic substance 90-96% electrolytes boot is snauda undesirable impurities, including chlorides, phosphorous acid, phosphorus and other substances that negatively affects the quality of metal coatings. The disadvantage of the prototype, based on the reaction of carbonates (hydroxocobalamin) metal(II) with nitrilotri(methylenephosphonic) acid, is a rich foaming in the allocation of carbon dioxide, as well as the need for heating the electrolyte in the process of their preparation for complete removal of carbon dioxide and increase the rate of reaction.

The objective of the invention is to develop a method for the preparation of electrolytes and solutions for obtaining coatings of metals and alloys containing nitrilotri(methylenephosphonate) complexes of metals without admixture of undesirable substances, improving the processability of the method of preparation of electrolytes and fluids, expanding Arsenal of existing methods of cooking nitrilotri(methylenephosphonic) electrolytes and solutions.

The problem is solved in that the method of preparation of the phosphonate of electrolytes and fluids to obtain galvanic and chemical coatings metals and alloys, which contain as the main component metal cations from the group consisting of copper, zinc, Nickel, cobalt, and anions nitrilotri(methylenephosphonic) acid, includes the dissolution in water of the compounds, which is the source of metal cations, and compounds, which are a source of anion nitrilotri(methylenephosphonic) acid. New this method is that as the source of metal cations and anion nitrilotri(methylenephosphonic) acid using crystal nitrilotri(methylenephosphonate)(2) metals from the group consisting of copper, zinc, Nickel, cobalt. For the preparation of phosphonate electrolytes and solutions used to obtain coatings with copper or copper alloys, use crystal nitrilotri(methylenephosphonic)(2-) copper(II). For the preparation of phosphonate electrolytes used for obtaining coatings of zinc or zinc alloys, use crystal nitrilotri(methylenephosphonic)(2-) zinc(II). For the preparation of phosphonate electrolytes and solutions used to obtain coatings with Nickel or Nickel alloys, use crystal nitrilotri(methylenephosphonic)(2) Nickel(II). For the preparation of phosphonate electrolytes and solutions used for obtaining coatings of cobalt or cobalt alloys, use crystal nitrilotri(methylenephosphonic)(2) cobalt(II).

The method of preparation of the phosphonate electrolytes and solutions is as follows. The calculated amount of crystalline nitrilotri(methylenephosphonate)(2-) metals(II) (copper, zinc, Nickel, cobalt) with stirring, dissolved in distilled water and (optionally) add a solution of alkali (sodium hydroxide, potassium hydroxide) and/or other substances according to the recipe.

Nitrilotri(methylenephosphonate)(2-) copper(II), zinc(II), Nickel(II), cobalt(II) are stable when stored crystalline substances, soluble in water, aqueous solutions of alkalis and ammonia, which can be obtained in the form of individual compounds, containing no impurity chlorides, formaldehyde, phosphorous acids, organophosphorus substances (I. Lukes, Rejskova D., Odvarko R., Vojtisek p // Polyhedron, 1986, V.5, No. 12, P.2063. Sharma C.V.K., A. Clearfield, A. Cabeza, M.A.G. Aranda, S. Bruque // J. American Chemical Society, 2001, V.123, No. 12, P.2885).

Examples of the preparation of electrolytes and fluids.

Example 1.

of 23.2 g of three-hydrate nitrilotri(methylenephosphonate)(2-) copper(II) is dissolved with stirring in 1000 ml of water at a temperature of 28-30°C. the resulting electrolyte of the electrolysis copper plating is carried out at room temperature, cathode current density of 0.2 A/square inch for 60 minutes. As the cathode using pre-fat and potraviny plate brass brand 63 size 40×50 mm, as anodes using two plates of copper brand M0 sizes 50×100 mm each. As a result, the cathode get a smooth matte copper coating dark pink color,is firmly coupled with the base.

Example 2.

To 207,3 g three-hydrate nitrilotri(methylenephosphonate)(2-) copper(II) under stirring and cooling parts adds solution to 66.0 g of potassium hydroxide in 600 ml of water. After cooling to room temperature, the electrolyte is diluted with water to a volume of 1000 ml obtained In the electrolyte of the electrolysis copper plating is carried out at room temperature, cathode current density of 0.5 a/square inch within 18 minutes. As the cathode using pre-fat and potraviny plate brass brand 63 size 40×50 mm, as anodes using two plates of copper brand M0 sizes 50×100 mm each. As a result, the cathode get a smooth matte fine crystalline copper plated light pink color, is firmly coupled with the base.

Example 3.

To 207,3 g three-hydrate nitrilotri(methylenephosphonate)(2-) copper(II) under stirring and cooling parts add 25%solution of potassium hydroxide to achieve a pH of 10.1 and after cooling to room temperature, the electrolyte is diluted with water to a volume of 1000 ml obtained In the electrolyte of the electrolysis copper plating is carried out at room temperature, the initial cathodic current density of 2.0 a/square inch for 1 minute and working cathodic current density of 0.5 a/square inch for 17 minutes. As the cathode using pre-fat and potraviny plate of steel Mar and 10 size 40× 50 mm, as anodes using two plates of copper brand M0 sizes 50×100 mm each. As a result, the cathode get a smooth matte fine crystalline copper plated light pink color, is firmly coupled with the base.

Example 4.

To of 208.3 g of three-hydrate nitrilotri(methylenephosphonate)(2-) zinc(II) under stirring parts add 25%solution of potassium hydroxide to achieve a pH of 8.2. After cooling to room temperature, the electrolyte is diluted with water to a volume of 1000 ml In the resulting electrolyte galvanizing conduct electrolysis at room temperature, cathode current density of 1.0 a/square inch within 18 minutes. As the cathode using pre-fat and potraviny plate of steel grade 10 size 40×50 mm, as anodes using two plates of zinc brand W1 sizes 50×100 mm each. As a result, the cathode get a smooth matte fine crystalline zinc coating light gray, strongly coupled with the base.

Example 5.

To the mixture 187,4 g three-hydrate nitrilotri(methylenephosphonate)(2-) zinc(II) and 20.7 g of three-hydrate nitrilotri(methylenephosphonate)(2-) copper(II) under stirring and cooling parts was added a solution of 148 g of potassium hydroxide in 800 ml of water. After cooling to room temperature, the electrolyte is diluted with water to a volume of 1000 ml In the received electronic is rolite brass plating conduct electrolysis at room temperature, cathode current density of 0.6 A/square inch within 18 minutes. As the cathode using pre-fat and potraviny plate of steel grade 10 size 40×50 mm, as anodes using two plates of stainless steel 12X18H10T sizes 50×·100 mm each. As a result, the cathode get a smooth matte fine crystalline yellow coating, similar to the composition of brass brand L firmly coupled with the base.

Example 6.

Dissolve 41,0 g three-hydrate nitrilotri(methylenephosphonate)(2) Nickel(II) in 900 ml of water containing 9.0 g of sodium hydroxide and 12.6 g of three-hydrate of sodium acetate. The solution is heated to 80±2°C, add with stirring a solution of 31.8 g of the monohydrate of hypophosphite of sodium in 100 ml heated to 80±2°With water. The resulting solution is poured into the glass, which is placed in a thermostat heated to a temperature of 82°C. immersed In a solution of pre-fat and potraviny plate of steel grade 10. The density of the load is 2.7 square inch of surface per 1 l of solution. After 30 minutes, the plate is extracted, washed with water and dried. As a result, the plate get a smooth, shiny Nickel coating is firmly connected with a base, of a thickness of 3.1 μm. The solution is not decomposed and remains transparent, and there are no traces of contributing what I Nickel on the bottom and walls of glass, the sediment at the bottom.

Examples of implementing the claimed invention show the possibility of preparation of electrolytes and fluids given composition and concentration of the crystalline nitrilotri(methylenephosphonate)(2-) copper(II), zinc(II), Nickel(II), cobalt(II)that do not contain other anions besides anion nitrilotri(methylenephosphonic) acid and unwanted impurities, which could degrade the quality of the coating metals and alloys. Improving the processability of the method of preparation of the phosphonate electrolytes and solutions is due to the fact that crystalline nitrilotri(methylenephosphonate)(2) metal(II) quickly moving in aqueous solution under the action of alkalies, this does not result in undesirable foaming. The method according to the claimed invention allows to prepare highly concentrated solutions, which can be used as a ready electrolytes or as a concentrate for subsequent dilution to the concentration specified by the recipe. Electrolytes and solutions, obtained by the claimed method, provide high-quality coatings of metals and alloys and are environmentally safe.

1. The method of preparation of the phosphonate of electrolytes and fluids to obtain galvanic and chemical coatings metals and alloy and, which contain as main components of the metal cations from the group consisting of copper, zinc, Nickel, cobalt, and anions nitrilotri(methylenephosphonic) acid, comprising dissolving in water compounds, which are a source of metal cations, and compounds, which are a source of anion nitrilotri(methylenephosphonic) acid, characterized in that as a source of metal cations and anion nitrilotri(methylenephosphonic) acid using crystal nitrilotri(methylenephosphonate)(2) metals from the group consisting of copper, zinc, Nickel, cobalt.

2. The method according to claim 1, characterized in that for the preparation of phosphonate electrolytes and solutions used to obtain coatings with copper or copper alloys, use crystal nitrilotri(methylenephosphonic)(2-) copper (II).

3. The method according to claim 1, characterized in that for the preparation of phosphonate electrolytes used for obtaining coatings of zinc or zinc alloys, use crystal nitrilotri(methylenephosphonic)(2-) zinc (II).

4. The method according to claim 1, characterized in that for the preparation of phosphonate electrolytes and solutions used to obtain coatings with Nickel or Nickel alloys, use crystal nitrilotri(methylenephosphonic)(2) Nickel (II).

5. The method according to claim 1, characterized in that for the preparation of f is spontanih electrolytes and fluids used for obtaining coatings of cobalt or cobalt alloys, use crystal nitrilotri(methylenephosphonic)(2) cobalt (II).



 

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