DED0013648MA - - Google Patents

Description

FEDERAL REPUBLIC OF GERMANY

Registration date: November 21, 1952. Advertised January 5, 1956

GERMAN PATENT OFFICE

It has been found that the surface properties of powdery substances, in particular of substances that are known in technology under the term "pigments" in a wide variety of fields of application brings to use, can improve significantly if these substances are anionic Mixtures of salts of acidic organic sulfuric acid derivatives, such as. B. alkyl sulfates, Impregnated alkyl sulfonates or alkylbenzenesulfonates that act as basic components on the one hand inorganic bases, such as. B. alkali, alkaline earth or earth metals and on the other hand ammonia or contain organic bases.

The impregnation increases the wettability of the powdery substances and their distributability significantly improved in liquid, highly viscous or plastic organic materials, furthermore their ability to float in the. Suspension in liquids, as well as their adhesiveness and their Pourability. ,

Pigments impregnated in this way are of particular practical interest, for example for paintwork and paints in which they are excellent in floatability or as fillers for Natural and synthetic rubber, regenerated rubber and rubber substitutes.

509 627/26

D 13648 IVa / 12g

Powdered substances that come into consideration here can be inorganic or organic Be nature, e.g. B. inorganic oxides, hydroxides and salts, such as those used, for. B. used as color pigments become, like-. ocher, iron oxide red, red lead, Titanium dioxide, zinc sulfide, barium sulfate, potassium carbonate and the like, also soot, zinc oxide, finely divided silica anhydride, silica gel, calcium silicate or aluminum silicate dispersions

ίο and the like, as they are used as fillers for rubber and Reclaimed rubber come into consideration. Powder bases such as talc, Rice flour, starch and the like, bleaching earth, kaolin, pumice stone powder, clay, also activated carbon, cork flour, Wood flour, as well as other well-known inorganic. niche or organic powdery substances.

The impregnation of these powdery substances with the anion-active mixtures of salts of acidic organic sulfuric acid derivatives is carried out in the usual way by stirring the powdery substances into solutions of the salt mixtures in water or an organic solvent, separating them and then drying them, or adding the solutions to the dry pigments appropriately sprayed or misted on. In suitable cases, the salt mixtures can also be applied directly to the powdery substances by grinding or mulling, whereby both components can be used both dry and in the moistened state ¹ . The amounts in which the salts of acidic organic sulfuric acid derivatives are applied to the powdery substances depend on the working conditions used and the respective intended use. These amounts are between 0.05 to 10% and more, preferably from 0.1 to 5%, calculated on the powdery substances.

Among organic sulfuric acid derivatives, as used in the context of the present invention as Components for the salt mixtures used in. Sulfuric acid esters will primarily be considered aliphatic, cycloaliphatic! · and fatty aromatic alcohols and sulfonic acids with Understood aliphatically or aromatically bonded sulfonic acid group, for which the following examples to be mentioned are: hexylsulfuric acid esters, octylsulfuric acid esters; dodecylsulfuric acid esters, Oleylsulfuric acid esters or mixtures of alkylsulfuric acid esters, Sulfuric acid esters of naphthenic or resin alcohols, hexylsulphonic acid, cyclohexylsulphonic acid, Octylsulphonic acid, mixtures of alkylsulphonic acids such as those produced by the action of sulfur dioxide and chlorine on hydrocarbon mixtures such as diesel oil; further Octylbenzenesulfonic acid, dodecylbenzenesulfonic acid or other alkylbenzenesulfonic acids or mixtures thereof, like them, e.g. B. by condensation of unsaturated gasoline hydrocarbons with benzene in the presence obtained from aluminum oxide and subsequent sulfonation, and also tetrahydronaphthalene sulfonic acid and the like

The alkyl radicals of these sulfuric acid derivatives can also be heteroatoms, such as oxygen or sulfur or nitrogen or atomic groups derived therefrom, as well as substituents. Inorganic Niche bases which are used to form the salt mixtures according to the invention are for example Sodium, potassium, calcium, magnesium, aluminum and the like come as organic bases primary, secondary or tertiary bases into consideration, such as. B. octylamine, dioctylamine, cyclohexylamine, Diethylcyclohexylamine, Monomethylaniline, Diethylaniline, Monoethanolamine, Triethanolamine, Morphö-Hn, Piperidine, pyridine, quinoline and the like.

The impregnations of the powdery substances or pigments are for the most diverse technical Areas of application suitable. Apart from the already mentioned production of pigmented Paints and varnishes and their use in the rubber industry, they can are used, for example, when mixing in pulverulent opacifying agents, coloring agents or fillers in plastics or plastic masses. In the manufacture of powders for dusting Rubber or synthetic resin skins, also in the production of coatings containing pigments for Paper, cardboard and the like, or as a filler for paper and cardboard, as a matting agent for Artificial silk and shaped structures as filling, weighting or finishing agents in the textile industry etc. -

The impregnation process according to the invention can accordingly be used in all cases which are an improvement of the surface properties of the powdery substances,. Increasing their coverage in use, improving the stability of their state of distribution and the improvement of the performance properties of the products manufactured with it.

Clays capable of base exchange have already been treated with cation-active onium compounds, about their surface properties with regard to their applicability as fillers for. Improve rubber. These onium compounds are used to react with the base-exchanging ones Toning enabled. It was therefore surprising that one is anionactive with compounds Character as used in the context of the present invention, in particular A valuable pigment impregnation is also obtained with the claimed mixtures can, especially since the substances according to the invention are much more easily accessible than the onium compounds of the state of the art.

Examples

i. In a ball mill, 500 parts by weight of red iron oxide with 5 parts by weight of a sulfonate mixture of 20% of the diethylcyclohexylamine salts of an alkyl sulfate mixture with alkyl radicals C ₄ to C ₁₁ and 80% of the magnesium salts of an alkyl sulfate _{mixture with alkyl radicals C 10} to C _{18 are} processed until the mixture is evenly distributed is achieved on the iron oxide red. The iron oxide red shows no change in its coloring character, is stable in storage and can be easily removed

509 627/26

D 13648 IVa / 12 g

and incorporate homogeneously into varnishes and paints.

The pigment can e.g. B. with a rosin ester linseed oil varnish (i: i) in the ratio 50 parts of pigment 50 parts of lacquer incorporated on a funnel mill. be rubbed. The grinding shows after 6 months Observation time no sediment, but at most an accumulation of pigment below the top third of the contents of the vessel, which can easily be evenly distributed can bring. The sedimentation, measured according to the method of Boiler-Licht hardt (»Color und Lack ", vol. 58, pp. 441 to 443) was so small that the test cone with a load of only 9 g reached the bottom of the jar. A grinding of the same binder with the same, however untreated iron oxide red, in the same proportions, was obtained after a month's observation period a strong, viscous sediment, which was very difficult to stir up again. According to the above test method, this rubbing required a cone load of 150 g in order to avoid the To reach the bottom of the jar.

2. In a pan mill 500 parts by weight of iron oxide red were treated with 5 parts by weight of a solution which consists of 10% diethylcyclohexylamine salt of an alkyl sulfate mixture with alkyl radicals C ₄ to C ₁₁ , 40% magnesium salt of an alkyl sulfate mixture with alkyl radicals C ₁₀ to C ₁₈ , 40% water, 10% Hexalin consists. The collapse continues until the alkyl sulfate mixture is evenly distributed and the water has evaporated. The iron oxide red shows no change in its color properties and has good distribution and suspension properties in paints.

Rubbing of this iron oxide red in a rosin ester linseed oil varnish (1: 1), rubbed in proportion 50:50, required according to the same test method like example ί a cone load of 21g, while the same grinding with unhandled Pigment required a cone load of 150 g in the same ratio.

3. To improve the surface properties of a calcium silicate pigment, as it is used in the rubber industry as a mineral filler, to 1000 parts by weight of a paste containing about 70% water of this pigment, 12 parts by weight of a salt mixture, which consists of an alkylbenzenesulfonic acid mixture (alkyl radicals C ₁₂ to C ₁₆ ) was obtained by neutralization with magnesium oxide and triethanolamine in the ratio ι: ι. The mixture is homogenized in a kneader, dried in the usual way at about 100 ° and then ground.

Kind of place of calcium silicate can also be used in the same. Way one made of water glass with Use mineral acid precipitated silica pigment.

Claims (6)

PATENT CLAIMS: 1. Process for improving surface properties water-insoluble, powdery substances, characterized in that the powdery substances are mixed with anion-active Mixtures of salts of acidic organic sulfuric acid derivatives of inorganic or impregnated with organic bases. 2. The method according to claim 1, characterized in that, for the impregnation, mixtures of salts of alkyl sulfates, alkyl sulfonates or alkylbenzene sulfonates are used which ^{contain alkali, alkaline earth or earth metals as basic components on the one hand and ammonia or organic 1} bases. 3. The method according to claim 1 and 2, characterized characterized in that the mixtures of salts of acidic organic sulfuric acid derivatives in amounts from 0.05 to 10%, preferably from 0.1 to 5%, with the dry, powdered substances processed homogeneously. 4. The method according to claim 1 and 2, characterized characterized in that one solutions of the mixtures of salts of acidic organic sulfuric acid derivatives Processed homogeneously with the powdery substances in water or organic solvents. 5. The method according to claim 1 to 4, characterized characterized in that to improve the surface properties of powdery Color pigments and the like for paints, lacquer paints, oil paints, synthetic resin paints and the like with mixtures of salts of acidic organic sulfuric acid derivatives, such as. B. alkyl sulfates, Alkyl sulfonates or alkylbenzenesulfonates, which are used as basic components on the one hand inorganic bases such as alkali, alkaline earth or earth metals and on the other hand Containing ammonia or organic bases, impregnated. 6. The method nach.Anspruch 1 to 4, thereby characterized in that to improve the ■ surface properties of powdery Substances for natural or synthetic rubber or rubber substitutes are used with mixtures from salts of acidic organic sulfuric acid derivatives, such as. B. alkyl sulfates, alkyl sulfonates or Alkylbenzolsu'lfonaten, the basic components on the one hand inorganic Bases such as alkali, alkaline earth or earth metals and on the other hand ammonia or organic Contains bases, impregnated. Referred publications: U.S. Patent Nos. 2531396, 2519622; French Patent No. 963,737;
German patent specifications No. 485 054, 569842. 509 627/26 12.55