CS199126B1 - Method of producing metallic soaps - Google Patents

Description

The invention relates to a process for the production of metal metal soaps II. % by reacting a fatty acid with metal hydroxides or oxides of this group in the form of an aqueous suspension and optionally in the presence of surfactants and complexing agents at a temperature above the melting point of the fatty acid.

The present invention also provides a granular product suitable for further processing.

Production of metal soaps of higher fatty acids It is a process which finds application mainly in the chemical industry and thus enables to obtain products widely used in the plastics and coating industries, in the production of lubricating oils, in the cosmetics industry, rubber industry, etc.

Prior art methods of making metal soaps are by melting the fatty acid and the oxides or metal hydroxides by treating the molten fatty acid, usually having about twelve to twenty carbon atoms per molecule, to mix with the ground metal oxide or hydroxide, and upon completion of the reaction, the melt is cooled and the product is transferred to a pulverulent farm. According to another known process, metal soaps are prepared by melting alkali aols of aliphatic carbon acids with oxides and metal hydroxides

119 126

189128

II. to IV. of the group with vigorous stirring without external heating, at a temperature below the melting point of the reaction product. Further, a production method based on the conversion of alkali soaps of higher fatty acids with the metal salt in aqueous solution is known. Processes for preparing metal soaps by dispersion techniques directly from fatty acids by reaction with metal hydroxides, carbonates or oxides in an aqueous medium containing surfactants (GDR Pat. 106629) are also described.

The disadvantages of the above processes are that the end products are dark in color and mostly have a higher free fatty acid content. When using the precipitation method, it is necessary to work in dilute solutions, which requires higher equipment requirements and increases production costs due to a greater number of manufacturing operations. The disadvantage of melting processes in production is the high energy consumption.

These deficiencies are eliminated by the method of production of metal soaps of metals II. The reaction of the group comprises the reaction of fatty acids and metal hydroxides or oxides of this group in the form of an aqueous suspension and in the presence of surfactants and complexing agents, at a temperature not melting at the fatty acid. It consists in treating the Group II metal salts with an alkali hydroxide, dispersing them and treating them with a fatty acid, the molar ratio of the fatty acid to the metal hydroxide or oxide being 1: 0.5 to 0, 65.

To metal salts II. Anionic type surfactant, preferably a sodium salt of an alkyl sulfosuccinic acid alkyl of 6 to 8 carbon atoms, is added in an amount of from 0.05 to 0.3 vol% based on the total volume of the reaction mixture. According to a further feature of the invention, the metal salts II. For example, the nitrile triacetic acid sodium salt is added in an amount of from 0.05 to 0.3% by volume, based on the total volume of the reaction mixture.

The dispersing is achieved by stirring at a speed of 4 to 12 / s, preferably 8 / s. This makes it possible to obtain a coarse-grained material with a substantially lower water content and good mechanical stability, which can advantageously be dried in a fluid-bed dryer, which contributes substantially to improved working conditions in the manufacture and handling of the finished product. No less important is a significant reduction in production time, which, while maintaining the same productivity, is up to 5 times that of conventional metal soap production methods. The use of anionic type surfactants will improve the dispersibility of the reactants in the aqueous phase, resulting in increased uniformity of granulation of production, reduction of particulate matter, reduction of free fatty acid content, increase of reaction yield and reduction of water content, thus increasing product quality over prior art technologies to achieve a new and higher effect.

The production method according to the invention is described in more detail below with reference to several exemplary embodiments

199128

Example 1

3750 L of water, 10 L of 30 wt. of a solution of the alkyl ester of sodium sulfosuccinic acid and 10 L (30% by weight of an aqueous solution) of the sodium salt of nitrolotriacetic acid, and the solution was heated to 80 ° C. Stirring at 400 to 450 rpm. 282 L of 45 wt.% sodium hydroxide solution was added. and 503 L of 35% by weight anhydrous calcium chloride solution. To the thus prepared reaction mixture at 80 ° C, preheated stearic acid at a temperature of 90 to 100 ° C in an amount of 750 kg was metered into the upper layer of the reaction mixture while stirring for 15 minutes. After completion of stearic acid dosing, the contents of the boiler were further stirred for 35 min. The reaction mixture contained granules of formed calcium stearate and was pumped to a filter device where the granules were separated from the reaction solution, washed with water and dried. White granules containing 25 wt. water with an average size of 1.2 mm with a predominant proportion (60%) of 1.3 mm particles. The free fatty acid content was 0.5% and the reaction yield 96%.

Example 2

The preparation of calcium stearate was carried out analogously to Example 1 except that the temperature of the reaction mixture was 85 ° C, the amount of anhydrous calcium chloride solution at a concentration of 35% by weight. was 461 L and 45% sodium hydroxide solution. 258 1. 700 kg of stearic acid were metered into the volume of the reaction mixture by means of a perforated tube having a hole diameter of 3 to 5 mm while stirring at a speed of 450 to 500 / min. A product having the same properties as in Example 1 was obtained with an average granule size of 1.0 mm, with a predominant proportion (58%) of 0.9 mm particles. The free fatty acid content was 0.6% and the reaction yield 96%.

Example 3

The preparation of calcium stearate was carried out analogously to Example 1 except that an anionic surfactant of the sodium salt of the alkyl sulfosuccinic acid type was not used. The properties of the product were the same as in Example 1, the free fatty acid content being 2% and the particle size (38%) predominantly being 1.1 mm. The reaction yield was 92

Example 4

The preparation of calcium stearate was performed analogously to Example 1 except that 216 kg of anhydrous calcium sulfate was used instead of calcium chloride. A product with the properties as in Example 1 was obtained with a granule size of 1.4 mm with a predominant proportion (61%) of 1.3 mm particle size. The content of free fatty acids in the product was 0.6 ¢, reaction yield 95%.

199128

Example 5

The preparation of zinc stearate was carried out in the same manner as in Example 1 β except that 398 kg of zinc sulfate heptahydrate and 246 l of 45 wt% sodium hydroxide solution were added instead of calcium chloride solution. Granules having a water content of 28% by weight were obtained. and an average size of 1.3 mm with a predominant proportion (60%) of 1.2 mm. The free fatty acid content was 1.5%, the reaction yield 92%.

Example 6

The preparation of zinc stearate was performed analogously to Example 5 except that the temperature of the reaction mixture was 85 ° C, the amount of zinc sulfate was 417 kg and the sodium hydroxide solution at a concentration of 45% by weight. 1. Stearic acid was fed into the reaction vessel in the same manner as in Example 2. A white product was obtained with a water content of 30% by weight. and an average granule size of 1.2 mm with a predominant particle size of 1.2 mm of 65%. The content of free fatty acids was 1.3%, reaction yield 91%.

Example 7

The preparation of zinc stearate was carried out analogously to Example 5, except that the anionic surfactant of the sodium salt of alkyl sulfosuccinic acid type was not used. The properties of the product were similar to those of Example 6. The free fatty acid content was 2.5%, the predominant proportion (38 particles being 1.3 mm in size) and the reaction yield was 88%.

Example 8

The preparation of zinc ateanate was carried out in the same manner as in Example 5 except that 189 kg of anhydrous zinc chloride was used instead of zinc sulfate. The product properties were similar to Example 5. The free fatty acid content was 1%. The 1.2 mm particles represented the predominant proportion (67%) of the sizes represented. The reaction yield was 94%.

Example 9

The reaction vessel was charged with 3750 L of water, 10 L of 30% sodium aole sulfosuccinic acid alkyl ester solution and 10 L (30% w / w aqueous solution) of sodium nitrolotriacetic acid, 189 kg of anhydrous zinc chloride and 246 L of 45% sodium hydroxide. aqueous solution. The reaction mixture was heated to 80 ° C and 750 kg of stearic cyeeline was added with stirring. The stirrer was 400 to 450 rpm. A white product with a water content of 25% by weight was obtained. The free fatty acid content was 0.2%. The mean granule size was 1.3 mm with a predominant proportion (69%) of the 1.4 mm particles. The reaction yield was 98%.

Example 10

1500 ml of water, 135.6 g of magnesium sulfate heptahydrate, 44 g of sodium hydroxide were charged to the reaction vessel, and the mixture was heated to 80 ° C with stirring. The stirrer speed was maintained at 400-600 rpm. The reaction mixture thus prepared was stirred for 10 min. 300 g of stearic acid was added with stirring. After the stearic acid was dosed, the reaction mixture was further stirred for 70 min. The product formed was white in color and the average granule size was 1 mm with a predominant proportion (30%) of 0.8 mm particles. The free fatty acid content of the product was 2.0% and the reaction yield was 89%. The water content of the product was 30 wt.

Example 11

3500 L of water, 10 L of 30 wt. of an aqueous solution of sodium salt of alkyl sulfosuccinate, 281 L of 45% sodium hydroxide solution. and 389 kg of magnesium sulfate heptahydrate. To the thus prepared reaction mixture heated to 85 ° C, 750 kg of stearic acid was added over 20 minutes at a stirrer speed of 600 to 700 rpm. The resulting product was white in color and the granule size was 1.0 to 1.2 mm. The predominant proportion of particles (60%) was 1.1 mm. The content of free fatty acids was 1.8%, yield 91%. Water content 24%.

Example 12

1,300 ml of water, 120.4 g of cadmium sulfate, 46.2 g of sodium hydroxide were added to the reaction vessel, and the mixture was heated to 90 ° C with stirring. The stirrer speed was maintained at 5400 to 700 / min. 300 g of stearic acid was added to the prepared reaction mixture for 15 minutes. The reaction mixture was further stirred for 80 minutes. The product formed was white in color and the size of the granules ranged from 0.8 to 1.2 mm. 30% wt. The content of free fatty acids in the product was 2%, the reaction yield was 87%. The water content was 30 wt.

Example 13

The preparation of cadmium stearate was carried out in the same manner as in Example 12 except that 143 g of cadmium sulfate and 54.6 g of sodium hydroxide were added to the reaction mixture. The temperature of the reaction mixture was 80 ° C. The product formed had the same properties as in Example 12. The 0.8 mm particle fraction was 38%, the free fatty acid content of the product was 3%, the reaction yield was 87%. The water content of the product was 30%.

Example 14

The preparation of cadmium stearate was carried out in the same manner as in Example 13 except that cadmium chloride was used in place of cadmium sulfate and

19912S anionic surfactant of the sodium salt of sulfosuccinic acid (30% w / w aqueous solution) was used in an amount of 2 ml. Cadmium chloride was used in an amount of 104 g. A product with the same properties as in Example 13 was obtained with a predominant proportion of 0.9 mm particles in an amount of 45% by weight. The free fatty acid content was 1.5 reaction yield 95%. The water content of the product was 28%.

Example 15

The preparation of cadmium ateanate was carried out analogously to Example 14 except that calcium sulfate was used instead of cadmium chloride in an amount of 143 g. The product was white in color, with a mean granule size of 0.9 mm with a predominant proportion (65%) of size 1 particles. 0 mm. The free fatty acid content was 0.5%, the water content of the product was 22% and the reaction yield was 98%.

The method of making the metal soaps according to the invention can be advantageously used for the production of hydrophobizing agents, various plastic stabilizers, vulcanizing compound additives, the production of paints, cosmetics and the like.

Claims (4)

1. Method of production of metal metal soaps II. of a group of fatty acids with metal hydroxides or oxides of this group in the form of an aqueous suspension in the presence of surfactants and complexing agents, at a temperature above the melting point of the fatty acid, characterized in that the metal salts II. and the resulting hydroxides or oxides are dispersed and treated with a fatty acid, the molar ratio of fatty acid to metal hydroxide or oxide being 1: 0.5 to 0.65. 2. A process for producing metal soaps according to claim 1, characterized in that the metal salts II. Anionic type surfactant, preferably sodium sulfosuccinic acid alkyl ester of 6 to 8 carbon atoms, is added in an amount of from 0.05 to 0.3 vol% based on the total volume of the reaction mixture. 3. A process for the production of metal soaps according to claim 1 or 2, characterized in that complexing agents based on nitrogen derivatives of polycarboxylic acids, preferably sodium salts of nitrolotriacetic acid, are added to the salts of the H. group in an amount of 0.05 to 0.3. % by volume, based on the total volume of the reaction mixture. 4. A process for the production of metal soaps according to claims 1 to 3, characterized in that the dispersion is achieved by stirring at a speed of 4 to 12 / s, preferably 8 / s.