The method of obtaining stable emulsifiers emulsions of the type oil - in-water

 

(57) Abstract:

Usage: in the field of producing emulsions of organic substances, of the type oil - water for the production of ointments, creams, latex, etc. of the invention: mix water and oil phase to obtain a highly concentrated emulsion with a volume content of the dispersed phase over the ratio of the maximum packing balls - more 0,74%, and then dilute the resulting emulsion water content of the dispersed phase below the ratio of the maximum packing of balls, preferably below 0,66. Droplets of the dispersed phase have a size of less than 0.5-1 μm. 1 C.p. f-crystals.

The invention relates to the field of producing emulsions of organic substances (oil in water emulsion of the type oil-in-water M/C).

This method can be used in a number of industries, for example in the chemical industry in the production of latexes in the pharmaceutical industry in the manufacture of ointments and creams etc.

Almost all known methods of making emulsions M/consists in dispersing the oil phase in water in the presence of surfactants emulsifiers.

To obtain highly stable emulsions, not bit the clock and day, it is necessary that the droplets of the dispersed phase had sizes less than 0.5-1 μm. Otherwise, comes a rapid separation of the phases of the emulsion due to the difference of densities with subsequent coalescence of the dispersed phase. A fairly high degree of dispersion is achieved usually by the use of high-intensity ways dispersion using homogenizers, exposure to ultrasound and other Most closely described in the book of C. S. of Vaskovo. The course of colloid chemistry, M. Chemistry, 1975, S. 317-380.

The application of this method involves using expensive equipment and requires a lot of energy and often does not give reproducible results.

Widespread found methods of preparation of emulsions by mixing oil and water phases, which do not require sophisticated equipment and high energy consumption. However, due to insufficient dispersion typically results in unstable emulsions with droplet size of the dispersed phase than 10 microns (E. A. Vasiliev, V. G. Ushakov. Apparatus for mixing environments. L. 1979, S. 8 prototype).

The problem to be solved in the present invention is to provide a method for producing stable emulsions of the type M/V with high grade is ovat in two stages: first, get highly concentrated (gel) emulsion (VIK) the volumetric content of the dispersed phase (in fractions of a unit), exceeding the maximum coefficient of installation of balls equal to 0.74. Then diluted received VIK water with moderate stirring up the volume content of the oil phase is less 0,74.

The method of obtaining VIK described, for example, in K. J. Lisont, J. Coll. Sci, v 22, R. 462-468. He is gradually added to a concentrated aqueous solution of emulsifier (10-35 wt.) the organic phase under mechanical stirring to achieve a volume ratio of organic and aqueous phases more than 2.9: 1 (the content of oil phase >0,74). Efficient crushing drops occurs when the content of oil phase more 0,74.

We found that subsequent dilution obtained VIK water emulsion is formed with a droplet size of the dispersed phase is less than 0.5 μm.

The resulting emulsion is very stable. Coalescence of the organic phase is not observed within a few weeks. In some cases, when advocating for several hours, there is partial separation (clipcooperativa). However, a slight stirring or shaking the homogeneity of the emulsion is restored.

The reasons for achieving a high degree of dispersion of the organic phase on predlagaemaya phases when the content of the organic phase, the larger the ratio of the maximum packing balls (more 0,74), is due to the fact that the drops, as it follows from geometrical considerations, cannot at this concentration to exist in a spherical shape and start as exceeding the content of 0.74 to take shape, the transition between spherical and polyhedral. As a consequence, the surface tension at different parts of the drops is not the same, which facilitates mechanical dispersion. A high concentration of emulsifier in the aqueous phase used in the preparation of tick-borne encephalitis, provides the adsorption of emulsifier the resulting dispersion droplet surface and thereby helps to prevent the drops merge.

According to modern concepts, tick-borne encephalitis can be represented as a system consisting of "slots" filled the dispersed phase, and "walls" between the "cells" consisting of a dispersion medium. At high content of dispersed phase from (to 0.74 to 0.99) thickness "partitions" is many times smaller than the size of the "cells". When diluted with water, VIK goes into "normal" emulsion, and the volume of the droplets of the dispersed phase corresponds to the amount of "cells" VIK.

Thus VIK allows you to reach the degree DISI in a short time, especially at elevated temperatures, disintegrate emitting organic phase. In addition, VIK offer extremely high viscosity, which makes them unsuitable for the specified application. Subsequent dilution of the tick-borne encephalitis with water to a concentration of the dispersed phase below the maximum ratio of packing balls (preferably below 66% ) leads to the preservation of a high degree of dispersion of the organic phase is reached when receiving VIK while enhancing the stability of the emulsion and lowering its viscosity by several orders of magnitude.

For carrying out the process of producing emulsions according to the present method requires widespread standard mixing device, which distinguishes the claimed method from the currently known methods of obtaining highly dispersed emulsions with the use of homogenizers, sound generators, and other complex and expensive equipment and giving less reproducible results on the properties of emulsions.

Example 1. In a glass reactor with a volume of 250 ml was placed 5 ml of 20% aqueous solution E-30 (sodium alkyl sulphonates C12-C15) and was added 50 ml of styrene for 20 minutes under stirring paddle stirrer phase 10:1. Received VIK was stirred for 15 min and then was added with stirring to 140 ml of water. Received 25% (by volume) emulsion of styrene. The emulsion is not contested within 10 days. Coalescence was not observed for 30 days. The droplet size of the dispersed phase, determined by light scattering method, was 60 nm.

Example 2. Analogously to example 1, but as the aqueous phase used a 15% aqueous solution of lauryl sodium. Coalescence was not observed for 30 days. After 24 h of sedimentation of the emulsion was observed the formation of "cream". With shaking recovered homogeneous emulsion. The droplet size of the dispersed phase, determined by light scattering method, was 77 nm.

Example 3. In a reactor with a volume of 250 ml was placed 5 ml of 33% aqueous solution of emulsifier OP-7 was added with stirring for 30 min, 35 ml of butyl acetate. Formed gel-like tick-borne encephalitis. To the resulting VIK was added under stirring and 47.5 ml of water. Received 40% (by volume) emulsion of butyl acetate in water, not otstaivavshaya within 30 days.

Example 4. Same as 1, but as the water phase used a 15% aqueous solution of laurate potassium, and as the oil phase heptane. Received a 25% emulsion HepB is remesiana for 1 min recovered homogeneous emulsion.

Example 5. Same as 1, but as the oil phase used toluene. Received a 25% emulsion of toluene was not stratified during 5 days. coalescence was not observed within 30 days.

Example 6 (negative). Same as 1 to 10 ml of 20% aqueous solution of emulsifier E-30 was added 20 ml of styrene (which is about 66. to the mixture). Gel highly concentrated emulsion was not formed. After stopping stirring, the emulsion was stratified in several minutes with subsequent coalescence in less than 1 h

Example 7 (negative). Similar to 6, but the resulting emulsion immediately after the addition of styrene was diluted with stirring to 70 ml of water until the content of styrene and about 20. The emulsion obtained was stratified almost immediately after cessation of mixing. Stratification was accompanied by coalescence of droplets of styrene.

Thus, the inventive method allows to obtain a fine stable emulsion type M/V with high sedimentation stability.

1. The method of obtaining stable emulsifiers emulsions of the type oil

water, comprising mixing water and oil phases, characterized in that exercise PE is the ratio of the maximum packing of balls more 0,74, with further dilution obtained highly concentrated emulsions with water until the content of the dispersed phase is less than the ratio of the maximum packing of balls.

2. The method according to p. 1, characterized in that the dilution of highly concentrated emulsions is carried out until the content of the dispersed phase is less 0,66.

 

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