DE1668600C - Ethylxanthogen 1 propane 2 sulfonic acid and its potassium salts as well as their use as brighteners in acidic galvanic copper plating baths - Google Patents

Description

1 2

It is known that the gloss and the weight are preferably between 5 and 10 mg / l. In the creation of copper deposits, work is generally carried out at room temperature and current densities of the number of sulfur-containing compounds vary from 0.5 to 2 A. Dns can be invented. In the case of these sulfur-containing compounds, moderate additives can, together with known ones, play a role in the content of sulfonic acid groups as water-wetting agents and leveling agents for all common metal-solubilizing groups; on the other hand, additional documents can be used. Copper ores are obtained, but also the derivatives of esters of the SuI coatings, which adhere very firmly and have excellent fothioic or trithiocarbonic acid or dithiocarb luster and which do not need to be polished amic acid, which need the grouping at least once.
- CS - S - included (see German patent specification io example

888 493), as well as those connections which at least "," ·. · ,, .. ■,

two production of Ethylxanthogcn-1-propan-

Carbon atoms, each of which has at least one 2-potassium suitonate

is a sulfur atom (cf. German patent 16.0 g of potassium ethyl xanthate (Vio Mol) were

1 007 592), a gloss-increasing effect. 15, dissolved in 100 ml of anhydrous ethanol in the heat, are therefore often added to mixtures of these hetero compounds and 12.2 g of unpurified propylene _{sulfonylide (V 2} mol) with the compounds containing sulfonic acid groups. The reaction mixture was left on the galvanic copper baths for 1 hour. It is also known to be steam-cooked. After just a few minutes it is advantageous to combine these two active ingredient components with each other, forming a brownish-browned reaction mixture, a yellow, microcrystalline substance almost completely solid, as described in German patents 1,053,274. Therefore, 100 ml Ethanol is added, and 1,062,514 is described. As sulfonic acid groups- After cooling, it was suctioned off, generally only those containing little additives were washed with ethanol, the substance was turned in a little hot, in which the sulfonic acid group was finally dissolved in water, heated with activated charcoal, filtered and that was bound, and for the Production of such Ver 25 ester sulfonate with four times the amount of concentrated bonds, which both the heterocomplex and potassium acetate solution precipitated and cooled. The sulfonic acid-yellow crystalline precipitate bound via a sulfur bridge was filtered off with suction, contained three groups combined, used for washing with a little anhydrous ethanol and preferably drying the sultones such as propane vacuum desiccator in the sulfoalkylation,
or butane sultone. For all of these additives there is 30,, ", ~", ",. ^,

the problem with the application is that the glossy yield: 6.3 g, d. ^ s. 22.4% of theory

producing effect only then in the desired manner. Melting point: 225 ° C (decomp.).

comes to the training if the other bathing. ,,. . .

conditions such as temperature, bath movement and the like in an application example

exact limits were kept. There is therefore 35 in a normal copper bath containing 220 g / l copper sulphate, Interest in finding useful brighteners, 60 g / l sulfuric acid and 2 g / l wetting agent alkvlarylbei to which modified conditions were observed, polyglycol ethers contained 5 to 10 mg of ethyldene be able. xanthogenic-1-propane-2-potassium sulfonate introduced.

The subject of the invention is accordingly one galvanized in this bath iron, brass from ethylxanthogen-l-propane-2-sulfonic acid and its 4 ° or copper sheets at room temperature using potassium salt and their use as a brightening agent with an average current density of 2 A / dm ² and in acidic galvanic copper plating baths. received high-gloss copper coatings that cannot be

Ethylxanthogen-1-propane-2-sulfonic acid has to be polished.

Formula Compared to comparable, constitutional ones

45 and earlier in the same area of application

CH ₃ —CH ₂ —O — C — S — CH ₂ —CH — CH ₃ products shows the essential

! I I improve the gloss effect and the depth scattering

S SO ₁₁ H comparing the results in the Hull cell.

It were in a bath with an addition of

The compounds according to the invention can be 5 ° 5 mg / 1 ethyl xanthogen-1-propane-2-potassium sulfonate, which can easily be prepared by sulfoalkylation of ethyl xanthate otherwise the composition of the specified, if you had the sulfoalkylation of the sulfur example, Hullzellbleche with a medium felatoms with propylene sulfonylide, which electroplates from a current density of 1 A / dm ² for 10 minutes at Manecke in Chemischeberichte, 85 (1952), to room temperature. For comparison, pages 160 to 162 have been described. The presentation of the compounds is carried out in such a way that used; In this example, too, the two reactants are used in equimolar amounts of 220 ε / l of crystallized copper sulfate and 60 g / l of amounts at room temperature or below in aqueous sulfuric acid as the basic bath. This bath was mixed with medium or in many cases in an organic 1.0 g / l of the additional ^preparation solvent mentioned in this example with a pronounced dipole character, 6o rates, namely the sodium salt of 1,3,5-triazine. B. methanol, can act on each other. 2,4,6-tri-mercantopropane-l'-sulfonic acid is added, generally achieving good yields. The so also in this bath were Hull cell sheets with a obtained sulfonic acids or their potassium salts are average current density of 1 A / dm ^a during a, with a suitable choice of solvent, good to iso duration of 10 minutes at room temperature, as they easily ⁶ 5 fert. In both experiments one used as a wetting agent for crystallization. these copper baths are more commonly available commercially

The use concentration of the inventive alkylaryl polyglycol ester in an amount of 2 g / l moderate additive is between 1 and 20 mg / l used.

The following results were obtained:

a) The Hull cell sheet copper-plated with the bath according to the invention showed over the entire area an even shine;

b) that with the known active ingredient according to German Auslegeschrift 1 053 274 in its optimal Applied concentration under otherwise identical conditions, copper-plated comparison sheet proved in the lower current density range as dark red, in the medium current density range there were areas with gloss formation, and in the high current density range the copper deposit was streaky and dark.

If the comparative experiment was carried out in such a way that also of the known additional substance according to the German Auslegeschrift 1 053 274 only 5 mg / 1

Baddüssigkcit were used, the copper-plated Hull cell sheet turned out to be completely lackluster.

The comparison shows that the brightener according to the invention is already used in a much smaller amount has a gloss-producing effect than is required for the comparable gloss agent known so far had to, and that when using the optimum concentration in each case, the permissible current density range is widened considerably.

Claims (2)

Patent claims: 1. Ethylxanthogen-1-propane-2-sulfonic acid and their potassium salt. 2. Use of the compounds according to claim 1 as brighteners in acidic electroplating Copper plating baths.