KR830002062B1 - Manufacturing method of metal soap - Google Patents

Abstract

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Description

Manufacturing method of metal soap

The present invention provides a metal soap or metal soap mixture prepared by reacting an aliphatic carboxylic acid having about 8-22 carbon atoms with water at least one of metal oxides, hydroxides and carbonates in the presence of water and then removing water. It is about a method.

Conventional metal soaps are known to be produced by a two-step reaction of carboxylic acids. As a first step, an alkali soap is formed by reacting with an appropriate amount of sodium hydroxide solution or potassium hydroxide solution, and in the second step, the alkali soap is mixed with a selected metal salt to precipitate an insoluble metal soap. The reaction takes place at a temperature of 60-70 ° C. using water about 20 times the weight of the carboxylic acid used. Separation of the precipitated metal soap is separated by, for example, filtration or centrifugation, and the resulting alkaline salt is reduced to a content ratio of less than 1% by washing. The metal soap is then pulverized dry. The final product has been considered to be bulky at very low densities and in particular releases excess dust. Another disadvantage of this method is that it requires many process steps.

Another known method is a method of advancing in a molten state when the carboxylic acid is reacted with an oxide, hydroxide or carbonate of a metal. In this method oxides, hydroxides or carbonates of the metal are added to the molten carboxylic acid at temperatures above the expected melting point of the final product and the water of the resulting hydrate is removed by evaporation. The anhydrous melt is then solidified using a cooling tower, cooling cylinder or cooling bath and then milled. The disadvantage of this method is that it produces a lot of dust and produces a dark colored final product. These coarse particles interfere with the production process and do not have satisfactory results.

Also described in German Patent No. 1068238 is a method of producing acid salt lead salt. This method proceeds the reaction of microparticle fatty acid with lead oxide in an aqueous suspension at a temperature slightly below the melting point of the acid. After the reaction, insoluble lead soap is produced and dried. A disadvantage of this method is that excess water, ie about 6-13 times the amount of carboxylic acid used, is required to make the fatty acids of the microparticles into aqueous suspensions. In this way the final product is not directly granular.

The present invention provides an improved process for the preparation of metal soaps or metal soap mixtures, i.e., to directly produce dust-free granular metal soaps or metal soap mixtures in a simple and economical way without additional processing steps by eliminating the disadvantages of known methods. The purpose is to provide a method.

In order to achieve the above object by the method described above, the present invention adds 1-5% of water to the carboxylic acid and then heats it to the temperature required for the reaction to cause an exothermic reaction to proceed under a closed pressure condition that does not supply external heat. The pressure is lowered and the water obtained from the reaction mixture is removed.

The method according to the present invention provides the following advantages over known methods.

The major disadvantages of the known methods were that the final product contained excessive dust and that the color was often black.

The process according to the invention leads directly to the final product in granular form. This product therefore does not spill excess dust and shows improved properties compared to metal soaps obtained by two-step reactions in aqueous phase or direct reactions in the molten state.

The distribution of the particle size of the final product obtained in the form of granules by the process of the present invention is particularly useful since about 80% of the total amount is within the desired particle size range. For example, it is possible to obtain a product in which about 80% of the metal soap is within the particle size range 0.2-2 mm.

Another advantage of the process of the present invention is that it is more economical than the known process, as energy is cut in the reaction and drying processes. This is due to the energy required to incidentally heat about 20 times the amount of water, based on the amount of carboxylic acid used in the reaction, in known methods. This is due to the fact that the amount of heat contained in the reactor at the time of discharge is sufficient to completely evaporate the water and thus does not require an additional energy supply.

Furthermore, in the two known methods mentioned above, the drying of the metal soap is carried out by a conventional drying technique such as a belt dryer fluid flow dryer, a tray dryer, a cylindrical dryer or a cascade dryer. It causes pollution.

The production of the metal soap or metal soap mixture from the reaction step to the final product by the process of the invention is carried out in a closed vessel. Thus, it is simpler than usual and consumes less time.

An advantageous embodiment of the method according to the invention is described as follows.

Aliphatic carboxylic acid having about 8-22 carbon atoms or a mixture of such carboxylic acids is added to at least one of the metal oxide hydroxides or carbonates in a pressure reaction vessel and 1-5% of water based on the total weight of the carboxylic acids is added. After mixing, it is heated to the temperature necessary to cause the reaction. The exothermic reaction proceeds at a temperature of about 90-110 ° C. and stirring of the reaction mixture is continued while a pressure of about 1.1-1.3 bar is formed in about 10-15 minutes. After completion of the reaction, the elevated pressure is reduced and the added water and the resulting water are discharged under reduced pressure conditions and the stirring speed is appropriately increased. This results in a rapid lowering of the temperature of the reaction product to about 50-55 ° C., whereby the final product is obtained in granular form. The granular material obtained is classified as a sieve and unwanted coarse and very fine particles corresponding to about 10% of the total amount are mixed again in the next reaction mixture.

The amount of water added in the process of the present invention is suitable for 2-4% of the total weight of the carboxylic acid, and this amount leads to an optimum result.

Initiation of the exothermic reaction in the process of the present invention requires an initial activated edger entering in the form of heat. It has thus been found to be particularly advantageous to heat the reaction mixture to at least the melting point of the carboxylic acid used or the melting temperature range of the carboxylic acid mixture used, ie generally to a temperature of about 50-60 ° C.

Aliphatic carboxylic acids having about 8-22 carbon atoms are selected from chain carboxylic acids having a hydroxyl group.

In order to obtain a white final product, the process of the present invention comprises at least one of oxides, hydroxides and carbonates of metals selected from bases including lithium, sodium, potassium, magnesium, calcium, strontium, barium, tin, lead and zinc Use It is also possible to use oxides, hydroxides and carbonates of selected metals from groups including copper, iron, nicap, manganese and chromium, but the metal soaps thus produced are generally less suitable as they are colored.

The amount of use of the oxides, hydroxides and carbonates of the metal is preferably at least equal to the amount of acid. In particular, at least one amount of oxides, hydroxides and carbonates of the metal should be slightly above about 2% of the amount of acid in order to prevent the formation of unnecessary free acid groups after the reaction.

The known method required more processing steps that had to be granulated in a device in which a high speed mixer or granulating additive was added at a temperature above the melting point of the additive when it was necessary to make the prepared metal soap into granular form. However, in the method of the present invention, a soft granular product which is easily coagulated and weighed is obtained by a uniform method. If necessary, the granular product of the metal soap can be coated with known lubricants, such as paraffin in fat, which are commonly used as granulation additives in the same reactor after the water has been removed.

An embodiment of the present invention will be described in detail as follows.

Example 1

Preparation of Calcium Soap

25 kg of an industrial carboxylic acid mixture having a chain length of C ₁₄ -C ₂₀ (C ₂₀ 2%, C ₁₈ 64%, C ₁₇ 2%, C ₁₆ 28%, C ₁₄ 4%) with an average molecular weight of 273 was 0.5 l of water and It is placed in a pressure reactor of capacity 130l with a stirrer with 3.5 kg of calcium hydroxide. Heating the reaction mixture to 50-60 ° C. causes exothermic reactions and no further heat input is required. The reaction proceeds with stirring the mixture in a closed reactor where pressure rises to 1.1-1.3 bar. The reaction is complete when pressure or temperature begins to decrease, respectively. After emptying the reactor, distilled under dilute agitation and reduced pressure, dust-free calcium soap produced in the form of granules is obtained directly as the final product.

The following embodiments proceed in the same manner as in Example 1.

Example 2

Production of Lead Soap

25 kg of the same carboxylic acid mixture as in Example 1 is reacted with 0.5 l of water and 10.6 kg of lead monoxide.

Example 3

Preparation of Zinc Soap

25 kg of the same carboxylic acid mixture as in Example 1 is reacted with 0.5 l of water and 3.75 kg of zinc oxide.

Example 4

Preparation of Barium-Calcium Soap

25 kg of industrial carboxylic acid mixtures with C ₁₀ -C ₁₄ and chain length (C ₁₀ 1%, C ₁₂ 93%, C ₁₄ 6%) with an average molecular weight of 200 l of water, 40.0 kg of calcium oxide and 5.4 kg of barium hydroxide React together.

Example 5

Preparation of Barium-Cadmium Soap

25 kg of the same carboxylic acid mixture as in Example 1 is reacted with 0.5 l of water, 2.95 kg of cadmium oxide and 2.95 kg of barium hydroxide.

Example 6

Preparation of Sodium Soap

30 kg of the same carboxylic acid mixture as in Example 1 is reacted with 0.5 l of water and 4.4 kg (100% pure) of sodium hydroxide.

Example 7

Preparation of Barium Soap

30 kg of the same carboxylic acid mixture as in Example 1 is reacted with 0.5 l of water and 9.5 kg of barium hydroxide.

The products obtained in Examples 2-7 were equally directly granulated, dust free metal soaps.

Claims (1)

At least one of the aliphatic carboxylic acids having about 8-22 carbon atoms is reacted with at least one of the oxides, hydroxides, and carbonates of the metal in the presence of water in a stirred state to remove water, and the carboxylic acid is a straight chain and a hydroxyl group. Oxides, hydroxides and carbonates of carboxylic acids, including metals, and metals, selected from groups containing lithium, sodium, potassium, magnesium, calcium, strontium, barium, tin, lead, and zinc in the same amount as carboxylic acids Or at a temperature not exceeding at least 2% and adding 1-5% of water based on the total weight of the carboxylic acid, followed by an exothermic reaction in a closed pressure reaction vessel, That is, the mixture is heated to the melting point of the carboxylic acid used or to the melting range of the carboxylic acid mixture used, The reaction grade that after method of reducing the elevated pressure and the reaction of metal or metal soap to the water characterized by the removal of the mixture obtained in the soap mixture without.