Patent Application
20070287757
The invention deals with a method for stabilization of a disperse system (e.g. emulsions or suspensions) which normally is not stable against sedimentation or creaming comprising the step of adding to said disperse system at least one network-inducing component. If the disperse system comprises two liquid phases it is stabilized against creaming by adding to said disperse system at least one network-inducing component. If the disperse system comprises one liquid phase and one solid phase it is stabilized against sedimentation by adding to said disperse system at least one network-inducing component.
In a particular embodiment of the invention, 1 to 30%, preferably 1 to 20%, of one or several emulsifiers and/or 1 to 10%, preferably 5 to 10%, especially 7 to 10% of one or several water-soluble polymers are added to said disperse system as network-inducing component. The percentages are always given by weight with respect to the total weight of the composition.
Preferably, 1 to 20%, especially 10 to 20%, of one or several emulsifiers, is added as network-inducing component to said disperse system. The network-inducing component added to said disperse system can also consist of 1 to 10%, especially 5 to 10% of one or several water-soluble polymers. The network-inducing component added to said disperse system can also consist of one or several emulsifiers and one or several water-soluble polymers.
The method for stabilization of a disperse system according to the invention preferably is used when the disperse system comprises two liquid phases (e.g. oil and water; silicone oil/water). The method for stabilization of a disperse system can also be used when the disperse system comprises one liquid phase and one solid phase (e.g. solid impurities and oil).
In a preferred embodiment for stabilization of a disperse system, 1 to 20% of one or several emulsifiers is added as network-inducing component to said disperse system.
In a further embodiment of the invention, 1 to 10% of one or several water-soluble polymers is added as network-inducing component to said disperse system.
In a particular embodiment of the invention, the stabilization of a disperse system is achieved by adding 1 to 20% of one or several emulsifiers and 1 to 5% of one or several water-soluble polymers as network-inducing component to said disperse system.
Preferably, 10 to 20% of one or several emulsifiers are added as network-inducing component to a disperse system.
Alternatively, 1 to 10% of one ore several water-soluble polymers are added as network-inducing component to said disperse system.
The invention furthermore deals with a method for stabilization of a disperse system, wherein a solution of one or several emulsifiers in water is added as network-inducing component to said disperse system.
As network-inducing component one or several emulsifiers from the group of ethoxylates of alkyl polyethylene glycol ethers can be used. Preferred emulsifiers are from the group of non-ionic surfactants Lutensol (producer: BASF AG) which are added as network-inducing component to said disperse system.
As water-soluble polymers, polymers from the group of polyvinyl alcohols, polyvinyl pyrollidones, polyethylene glycols, polyethylacrylates, polyhydantoines, poly(hydroxyacrylic acids), and polyethylene glycols are added as network-inducing component. Also water-soluble copolymers can be used.
The invention also deals with a disperse system which is stabilized against sedimentation or creaming according to the method as described above.
The network-inducing component can preferably consist of one or several emulsifiers from the group of ethoxylates of alkyl polyethylene glycol ethers, particularly one of the commercially available non-ionic surfactants Lutensol (e.g. Lutensol TO3, TO5, TO6, TO7, TO8, TO10 and TO12 produced by BASF, Germany), polyethylene fatty acid esters, polyethylene alkyl ethers, polyethylene polypropylene alkyl ethers and polypropylene glycol ethers.
Preferred network-inducing components are compounds of formula (I)
R—O(CH2—CH2—O)n—H
wherein R is alkyl with 10 to 15 carbon atoms, preferably 12 to 14 carbon atoms, particularly 13 carbon atoms, and
n is from 2 to 30, preferably from 3 to 20.
In a preferred embodiment, R is i-C13H17 and n is 3, 5, 6, 6.5, 7, 8, 10, 12, 15 or 20. These compounds can also be used as mixtures.
The network-inducing component added can also be one or several water-soluble polymers from the group comprising e.g. polyvinyl alcohols, polyvinyl pyrrolidones, polyethylene glycols, polyethyl acrylates, polyhydantoines, poly(hydroxy-acrylic acids), polymethacrylic acids, polypropylene glycols.
According to a preferred embodiment of the invention, a method for stabilization of an oil-in-water emulsion is provided by adding 5 to 20% of an emulsifier and/or 1 to 5% of a water-soluble polymer to this oil-in-water emulsion.
The method for stabilization of disperse systems can be used for the preparation of various food, cosmetic, dermatological or pharmaceutical products. Further co-emulsifiers can also be used (e.g. 0.1 to 1.5% by weight). In principle, emulsifier micelles and/or water-soluble polymers are useful as network-inducing component ac cording to this invention. In order to stabilize the disperse system, the water-soluble polymer induces the formation of a network of the oil-droplets within the system. Whereas in an emulsion for example the small individual droplets are stable against creaming for a certain period of time (depending inter alia on the droplet diameter, the density difference and the viscosity of the system), they tend to become unstable as soon as small clusters (so-called flocs) are formed. With increasing network-inducing component concentration, often the stability of the emulsion first decreases because of the formation of flocs. However, by adding the above mentioned emulsifiers/polymers to the system, the formation of an oil-droplet-network can be induced which stabilizes the emulsion against creaming.
The following water-soluble polymers are particularly useful according to this invention,
polyvinyl alcohols, polyvinyl pyrrolidones, polyethylene glycols, polyethyl acrylates, poly(hydroxy-acrylic acids) and polymethacrylic acids.
The following examples illustrate the present invention. The percentages provided are percentages by weight based on the total weight of the respective preparation.
An oil-in-water-emulsion was prepared at room temperature by using a laboratory homogenizer (Ultra-Turrax T50) with 1 minute of continuous homogenization (10000 rpm). This starting emulsion was prepared by using
28.5 g of silicone oil (plasticizer AK100, producer: Wacker Chemie AG, Munich),
1.5 g of an emulsifier (sodiumdodecylsulfate) and
70 g of water.
For the testing of the stability of the emulsions at room temperature, the following emulsions A, B, C, D, E and F were prepared:
Test A)
50 ml of the emulsion as prepared above and 25 ml of pure water were mixed and homogenized for 3 minutes (800 rmp). The resulting emulsion was transferred in a glass cell for further observation.
Test B)
The same procedure was applied as described under Test A, however, 25 ml of a solution containing 9% of the non-ionic surfactant Lutensol TO8 (producer BASF Aktiengesellschaft, Ludwigshafen) in water was used, such that the final emulsion contains 3% of Lutensol TO8.
Test C)
The same procedure was applied as described under Test A, however, 25 ml of a solution containing 18% of the non-ionic surfactant Lutensol TO8 (producer BASF Aktiengesellschaft, Ludwigshafen) in water was used.
Test D)
The same procedure was applied as described under Test A, however, 25 ml of a solution containing 30% of the non-ionic surfactant Lutensol TO8 (producer: BASF Aktiengesellschaft, Ludwigshafen) in water was used.
Test E)
The same procedure was applied as described under Test A, however, 25 ml of a solution containing 45% of the non-ionic surfactant Lutensol TO8 (producer: BASF Aktiengesellschaft, Ludwigshafen) in water was used.
Test F)
The same procedure was applied as described under Test A, however, 25 ml of a solution containing 60% of the non-ionic surfactant Lutensol TO8 (producer: BASF Aktiengesellschaft, Ludwigshafen) in water was used.
The stability of all six test emulsions was observed for a period of more than 24 hours.
After 1 minute at room temperature all six test emulsions (A. B, C, D, E and F) were stable, no creaming was observed.
After 10 minutes, some creaming was observed for test emulsions A and B.
After 1 hour, considerable creaming was observed in test emulsions A, B, C and D. The test results after 1 hour at room temperature are shown in
After 5 hours at room temperature, creaming was observed for test emulsions A, B, C, D and E, whereas test emulsion F was stable against creaming. The test results after 5 hours are shown in
The instability of the test emulsions can be described by measuring the volume of the water phase every 5 minutes. The results are shown in
As it easily can be seen, the emulsion containing 1% sodiumdodecylsulfate and the highest concentration of Lutensol TO8 was completely stable against creaming for a period of 5 hours.
The emulsion containing 1% of sodiumdodecylsulfate, but containing no network-inducing component was found to be very unstable, whereas the test emulsions B, C, D and E showed some stabilizing effect of the network-inducing component.
An oil-in-water emulsion was prepared at room temperature by using a magnet stirrer (at 800 rpm) for 1 hour of continuous stirring. The starting emulsion was prepared with:
28.5 g paraffin oil (from Roth),
1.5 g Lutensol TO8 (from BASF Aktiengesellschaft) and
70 g of water.
For the testing of the stability of the emulsions at room temperature, the following emulsions A, B, C, D, E, F, were prepared:
Test A)
50 ml of the emulsion as prepared above and 25 ml of pure water were mixed and homogenized for 3 minutes with a magnet stirrer at 800 rpm. The resulting emulsion was transferred in a glass cell for further observation.
Test B)
50 ml of the emulsion as prepared above and 25 ml of solution containing 3% Kollidon 90 F (polyvinyl pyrrolidone; producer BASF Aktiengesellschaft) in water were mixed and homogenized for 3 minutes with a magnet stirrer at 800 rpm, such that the final emulsion contains 1% Kollidon 90 F.
Test C)
50 ml of the emulsion as prepared above and 25 ml of solution containing 9% Kollidon 90 F were mixed and homogenized for 3 minutes with a magnet stirrer at 800 rpm, such that the final emulsion contains 3% Kollidon 90 F.
Test D)
50 ml of the emulsion as prepared above and 25 ml of solution containing 15% Kollidon 90 F were mixed and homogenized for 3 minutes with a magnet stirrer at 800 rpm, such that the final emulsion contains 5% Kollidon 90 F.
Test E)
50 ml of the emulsion as prepared above and 25 ml of solution containing 21% Kollidon 90 F were mixed and homogenized for 3 minutes with a magnet stirrer at 800 rpm, such that the final emulsion contains 7% Kollidon 90 F.
Test F)
50 ml of the emulsion as prepared above and 25 ml of solution containing 30% Kollidon 90 F were mixed and homogenized for 3 minutes with a magnet stirrer at 800 rpm, such that the final emulsion contains 10% Kollidon 90 F.
The stability of all six test emulsions A, B, C, D, E and F was observed for a period of 24 hours.
After 10 minutes creaming was observed in test emulsions A, B, C and D (see
After 2 hours creaming was observed In test emulsions A, B, C and D, emulsions E and F were still stable against creaming (see
The creaming profiles (as described in example 1) for the test emulsions are shown in
