Electrolysis: processes – compositions used therein – and methods – Electrolytic coating – Depositing predominantly single metal coating
Reexamination Certificate
1999-09-13
2001-05-29
Gorgos, Kathryn (Department: 1741)
Electrolysis: processes, compositions used therein, and methods
Electrolytic coating
Depositing predominantly single metal coating
C205S244000
Reexamination Certificate
active
06238542
ABSTRACT:
BACKGROUND
FIELD OF THE INVENTION
The invention concerns a process for the galvanic precipitation of zinc deposits and/or zinc-alloy deposits on a metallic surface, working with an aqueous acid electrolyte which contains at least one zinc salt and at least one high-gloss agent.
Different processes for the galvanic precipitation of zinc deposits and zinc alloy deposits are known from in practice. To this extent, comparable acid zinc electrolytes or zinc-alloy electrolytes are also known. Coating of metallic surfaces is usually carried out on the basis on the good anti-corrosion effect achieved by the zinc or zinc-alloy layers. It is often also desirable for the zinc or zinc-alloy coats to have a glossy surface and fulfil ornamental purposes. High-gloss agents are added to the electrolytes for this purpose, which, interacting as needed with other electrolytic components, produce the gloss on the zinc or zinc-alloy coats. In the processes mentioned above known in practice, aromatic carbonyl compounds, particularly benzylacetone or benzophenone as well as o-chlorobenzaldehyde, are used. The high-gloss agents are usually employed in a solution of alcohol, particularly methanol. Special safety precautions are necessary in the manufacture, transportation and storage of these solutions, because of their high flammability and toxicity. The disadvantage is unnecessary expense. The high-gloss agents are also used in higher boiling solvents, in butyl glycol for example, which bring disadvantages of a physiological nature. Since the solubility of the familiar high-gloss agents mentioned is very low, they must be solubilized with high concentrations of wetting agents in the aqueous electrolytes. This is also complicated and costly.
SUMMARY OF THE INVENTION
By contrast, the invention starts with the technical problem of describing a process as described above which works with water-soluble high-gloss agents which produce optimal gloss on the zinc and zinc-alloy coats in a simple and safe way.
DETAILED DESCRIPTION OF THE INVENTION
To solve this technical problem, the invention defines a process as described above whose characteristic is that a heterocyclic aromatic compound, with at least one alkylated nitrogen atom as the heteroatom, is added to the electrolyte as the high-gloss agent. Heterocyclic aromatic compounds are also called heteroaromatics. According to the invention, the heterocyclic aromatic compounds used have at least one nitrogen atom as the heteroatom, to which an alkyl group is bonded. To this extent, they are n-alkylated heterocyclic aromatic compounds. The heterocyclic aromatic compound used as the high-gloss agent can also have several alkylated nitrogen atoms as heteroatoms. It is within the scope of the invention that the alkyl groups bonded to the nitrogen atom are straight-chain, branched or cyclic. The alkyl groups can also contain double bonds and/or triple bonds. In one version of the invention, hydrogen atoms in the alkyl groups are replaced by functional groups. So the hydrogen atoms in the alkyl groups can be replaced by hydroxyl groups and or ether groups and/or carboxyl groups and/or ester groups and/or halogen atoms and/or sulfonate groups and/or aromatic rings and/or amino groups.
It is within the scope of the invention that the heterocyclic aromatic compound used as the high-gloss agent has additional heteroatoms besides one or several alkylated nitrogen atoms. They can be non-alkylated nitrogen atoms to which, depending on the bonding conditions, a hydrogen atom can also be bonded. But in this case, it can also be other heteroatoms, such as oxygen or sulfur atoms. In one version of the invention, the heterocyclic aromatic compound can have at least one additional nitrogen atom as the heteroatom; no alkyl group is bonded to this nitrogen atom. It is within the scope of the invention that other substitutes are bonded to the carbon atoms of the heterocyclic aromatic compound in place of hydrogen atoms. For example, alkyl groups and/or ether groups and/or carboxyl groups and/or halogen atoms and/or sulfonate groups and/or amino groups and/or hydroxyl groups can be bound to these carbon atoms. In one version of the invention, a condensed ring system is used as a heterocyclic aromatic compound, which contains aromatic and/or non-aromatic rings. In this version, one ring alone, or several rings, or all the rings can each have at least one heteroatom.
Preferably at least one N-alkylated 5-ring heteroaromatic and/or at least one N-alkylated 6-ring heteroaromatic is added to the electrolyte as the heterocyclic aromatic compound. These 5-ring heteroaromatics and/or 6-ring heteroaromatics are particularly suitable as high-gloss agents for zinc and/or zinc-alloy precipitation. In the preferred version, which has is a particularly important part of the invention, at least one N-alkylated pyridine is added as a heterocyclic aromatic compound. N-hexadecylpyridine chloride as the high-gloss agent is the preferred additive. Furthermore, the use of dodecylpyridine chloride and/or N-benzylpyridinium-3-carboxylate is preferred. In this context, it must be pointed out that it is part of the invention that the heterocyclic aromatic compound can be used in the form of quaternary salt as a high-gloss agent. Then the electrolyte has an assigned inorganic or organic anion, which is advantageously compatible with the other electrolyte components. As a matter of preference, they are halides, sulfations, hydrogen sulfations, tetrafluoride borates or acetates. In principal, the invention involves, for example, the use of N-alkylated pyrroles and/or N-alkylated pyrazolenes and/or N-alkylated imidazoles and/or N-alkylated quinolines as high-gloss agents.
In a preferred version of the invention, the heterocyclic aromatic compound is used in a concentration of 0.001 g/l to 100 g/l, preferably 0.005 g/l to 10 g/l, referenced to the electrolyte. It is within the scope of the invention that other known high-gloss agents are used in addition to the heterocyclic aromatic compound. The total concentration of the high-gloss agent added to the electrolyte in this case is 0.001 g/l to 100 g/l, preferably 0.005 g/l to 10 g/l, referenced to the electrolyte.
Different types of electrolyte are known for the precipitation of zinc deposits and/or zinc-alloy deposits. The preferred method is to use a zinc electrolyte on a zinc chloride base to precipitate zinc deposits. The zinc electrolyte contains 5 g/l to 500 g/l of zinc salt, preferably zinc chloride. To precipitate zinc-cobalt alloys, the electrolyte contains a zinc salt, preferably 50 g/l to 150 g/l zinc salt, preferably zinc chloride, as well as a cobalt salt, preferably cobaltous chloride. A zinc salt in the amount of 5 g/l to 500 g/l, preferably 50 g/l to 150 g/l, and cobaltous salt in the amount of 0.01 g/l to 150 g/l, preferably 1 g/l. to 50 g/l is used. To precipitate zinc-nickel alloys, a zinc salt, preferably zinc chloride, as well as a nickel salt, preferably nickel chloride, is added to the electrolyte. The concentration of zinc salt in the electrolyte is 5 g/l to 500 g/l, preferably 50 g/l to 150 g/l, and the concentration of nickel salt in the electrolyte is 0.01 g/l to 150 g/l, preferably 1 g/l to 50 g/l. The electrolyte is preferably adjusted to mildly acidic. For practical purposes, the electrolyte has a pH of 4 to 6. It is within the scope of the invention that the electrolyte contains conducting salt. The preferred conductive salt used is ammonium chloride and/or potassium chloride and/or sodium chloride. For practical purposes, the electrolyte has of 5 g/l to 250 g/l of conducting salt by volume.
In the preferred version of the invention, at least one sufactant is added to the electrolyte. The preferred choice is a sufactant concentration of 0.001 g/l to 100 g/l, preferably 0.5 g/l to 20 g/l, referenced in each case to the electrolyte. In one version of the invention, at least one non-ionic sufactant from the “alkyl alcoxyl, aryl alcoxyl, alkylaryl alcoxyl” group is added to the electrolyte. In another version of the invention, at l
Gorgos Kathryn
Keehan Christopher M.
Warn, Burgess & Hoffmann, P.C.
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