KR20180074901A - Oil gel and the method of manufacturing the same - Google Patents

Abstract

The present invention relates to oil gel, and to a manufacturing method thereof, and more specifically, to oil gel, capable of alleviating stickiness of the oil gel by using an inorganic material having a three-dimensional branch structure such as hydrophilic fumed silica used as a gelling agent, and to a manufacturing method thereof. In addition, according to the present invention, by adjusting the weight ratio between oil and a gelling agent, which are components of the oil gel, shape stability and ease of use of the oil gel can be realized, and at the same time, mixing with other components becomes easy.

Description

FIELD OF THE INVENTION [0001] The present invention relates to an oil gel,

More particularly, the present invention relates to an oil gel using an inorganic material having a three-dimensional branch structure such as hydrophilic fumed silica as a gelling agent, and a method for producing the same.

In recent cosmetic fields, oils having excellent skin lubrication and moisturizing effects have been utilized variously. Since the oil can form a thin protective film on the skin, it is possible to prevent evaporation of moisture from the skin or to block ultraviolet rays or contaminants coming from the outside.

However, since the viscosity of the oil is low, it can not easily be used and handled easily, and when the functional particles are dispersed in the oil, the particles can easily sink and cause problems in dispersion stability.

Generally, as a gelling agent for increasing the viscosity of an oil, a thickening polymer capable of forming a network structure in oil is used. For example, a polymer such as a hydrogenated styrene-isoprene copolymer is a long linear polymer, And can act as a filler when added in oil.

It is an object of the present invention to provide an oil gel having less sticky property by replacing a thickening polymer used as a gelling agent with an inorganic substance having a three-dimensional branch structure such as hydrophilic fumed silica, and a method for producing the same.

It is another object of the present invention to provide an oil gel capable of uniformly mixing with additional components while having excellent shape stability and ease of use by specifying the weight ratio of components contained in the oil gel and a method for producing the same. .

In one embodiment of the invention,

Oil and hydrophilic fumed silica, wherein said oil and said hydrophilic fumed silica provide an oil gel present in a weight ratio of 1: 0.1 to 32: 1.

The hydrophilic fumed silica may be used as an inorganic substance having a three-dimensional branched structure to be used as the gelling agent of the present invention. In particular, the hydrophilic fumed silica serves to increase the viscosity of the liquid phase by forming a hydrogen bond network in the liquid phase .

Since the network of silica bonds by hydrogen bonding is not a complex entangled structure, the prepared oil gel is less sticky.

In another embodiment of the present invention, there is provided an oil gel manufacturing process comprising mixing oil with hydrophilic fumed silica in a weight ratio of 1: 0.1 to 32: 1.

Here, the oil constituting the oil gel and the hydrophilic fumed silica are present in a weight ratio of 1: 0.1 to 32: 1, thereby giving an appropriate viscosity to the oil gel, so that when external force acts on the structure, When the external force is resolved again, the network structure is formed again and the fluidity is reduced.

By using an inorganic material having a three-dimensional branch structure such as hydrophilic fumed silica used as a gelling agent, stickiness of the oil gel can be mitigated.

Further, by appropriately adjusting the weight ratio between the oil and the gelling agent, which are components of the oil gel, the shape stability and ease of use of the oil gel can be realized and at the same time, other components can be added and mixed.

FIG. 1 shows changes in viscosity of oil gels of Example 2 and Comparative Example 2 and Comparative Example 3 as the external force was increased.

Certain terms are hereby defined for convenience in order to facilitate a better understanding of the present invention. Unless otherwise defined herein, scientific and technical terms used in the present invention may have the meanings commonly understood by one of ordinary skill in the art.

Also, unless the context clearly indicates otherwise, the singular form of the term includes plural forms thereof, and the plural forms of terms may include singular forms thereof.

Hereinafter, the oil gel according to the present invention and its production method will be described in detail.

In one embodiment of the present invention, oil and hydrophilic fumed silica are provided, wherein the oil and the hydrophilic fumed silica are present in a weight ratio of 1: 0.1 to 32: 1.

The gelling agent used in the present invention increases the viscosity of the oil and, at the same time, is not tacky, so that it is easy to use and it should be possible to uniformly mix with the additional components.

The oil gel using the thickening polymer has a problem that the tendency to stretch all the time is difficult because the entanglement between the polymer chains is not easily solved even when the force is applied.

In addition, because of the strong tackiness characteristic, the commercial oil gel can feel uncomfortable due to excessive stickiness when applied to the skin, or it can feel uncomfortable weight, and it is difficult to mix uniformly by stickiness when adding new ingredients to the oil gel, There is a problem.

Therefore, it is possible to form a three-dimensional network structure in the oil, but it is not entangled with the polymer such as a thickening polymer, so that it should have a low sticky property.

Accordingly, the gelling agent used in the present invention may be a fumed silica unless otherwise defined.

Fumed silica is amorphous silicon dioxide, a very light powder of white color. The average diameter of the base particles is from about several nanometers to several tens of nanometers, has a large specific surface area, and can range from 50 to 400 m ² / g.

Here, the fumed silica is produced by hydrolysis in a spark over 1000 ° C. formed with oxygen and hydrogen, as shown in the following reaction formula (1).

 [Reaction Scheme 1]

SiCl4 + 2H2 + O2? SiO2 + 4HCl

The basic particles made from flame are connected to each other due to the collision with each other in the state where the surface is still melted, so that they form a linear branch shape, which can be connected to form a three-dimensional branch structure.

More specifically, in fumed silica, primary particles are fired to form secondary aggregates through primary aggregates. In primary aggregates, primary particles aggregate to form a branch structure. In the secondary aggregates, primary aggregates contact each other As it extends, it becomes the above-mentioned three-dimensional branch structure inorganic form, and it can be said to be a kind of grape clusters.

Fumed silica is classified into hydrophobic fumed silica and hydrophilic fumed silica, and hydrophilic fumed silica has a hydroxyl group (-OH) in the molecule.

Thus, hydrophobic fumed silica increases the viscosity of the liquid phase simply by physically entanglement in the oil. Hydrophilic fumed silica enables the formation of a network structure more easily due to the hydrogen bonding between hydroxyl group (-OH) groups as well as the above-described structural entanglement.

Accordingly, in one embodiment, the gelling agent for making the oil gel is a hydrophilic fumed silica.

There is no limitation on the kind of the oil of the present invention.

For example, there may be mentioned plant-derived argan oil, camellia oil, castor oil, coconut oil, corn oil, jojoba oil, cottonseed oil, soybean oil, walnut oil, wheat germ oil, peach seed oil, olive oil, peanut oil, sunflower seed oil , Palm kernel oil, Karen dura oil, or any one selected from the group consisting of unrefined butter, shea butter, petroleum-derived mineral oil, caprylic / capric triglyceride, and combinations thereof Do.

Here, the oil constituting the oil gel and the hydrophilic fumed silica are present in a weight ratio of 1: 0.1 to 32: 1.

When the weight ratio of the two components is less than 1: 0.1, there is a problem that the viscosity of the oil gel becomes excessively high due to a large amount of the hydrophilic fumed silica, so that the stickiness becomes severe or the structure can not be easily released by external force.

On the other hand, when the weight ratio is more than 32: 1, the liquid component due to the oil becomes excessively large, so that the silica particles become very sticky and particles are formed excessively.

The oil gel component may further comprise additives in addition to the oil and the hydrophilic fumed silica.

The additive acts as a crosslinking agent for forming a hydrogen bond with silica, so that the bonding between the silica particles is facilitated.

For example, a compound having at least two functional groups selected from a thiol group, an amine group, a phosphonate group, a carboxyl group, a hydroxyl group, an imidazole group and a diol group, It can be applied as a material of structure.

Specifically, the additive is a linear or branched compound having two or more functional groups selected from the group consisting of a thiol group, an amine group, a phosphonate group, a carboxyl group, a hydroxyl group, an imidazole group, a diol group, .

Additives such as the above-mentioned structures include functional groups capable of hydrogen bonding at both ends of the molecule.

Therefore, it is possible to perform a cross-linking function between silica particles more easily than a compound having a functional group capable of only hydrogen bonding only in the hydrophilic group such as a surfactant.

In this case, the hydrophilic fumed silica and additives in the oil gel are present in a weight ratio of 1: 0.6 to 120: 1.

The oil gel contains the hydrophilic fumed silica and the additive in the above-mentioned range, so that the viscosity of the oil gel can be adjusted to an appropriate level, so that there is convenience of handling and even mixing with the additional component is possible.

The oil gel components may be present in an amount of 86 to 96% by weight of oil, 3 to 12% by weight of hydrophilic fumed silica and 0.1 to 2% by weight of additives.

 Each weight percent of the oil, hydrophilic fumed silica and additives present in the oil gel provides the effect of the present invention, i.e., ease of handling and uniform further mixing of the other ingredients, while producing less sticky oil gels Is determined within a range that does not impair the effect.

When the weight percentage of the oil is out of the above-mentioned range, the liquid component present in the oil gel becomes excessively small or becomes excessively large, and the handling of the oil gel becomes inconvenient.

When the weight percentage of the hydrophilic fumed silica is out of the above-mentioned range, there is a problem that the viscosity of the oil gel becomes excessively low or high, thereby making it difficult to deform the structure.

Further, when the weight percentage of the additive is out of the above-mentioned range, it is difficult to change the structure bond by significantly reducing or excessively bonding the silica.

 Particularly, when the content of the additive is less than 0.1% by weight, a distant silica network can not be formed easily and the viscosity of the oil gel becomes lower than that of the oil liquid.

According to another aspect of the present invention, there is provided a method for preparing an oil gel, comprising mixing oil with hydrophilic fumed silica in a weight ratio of 1: 0.1 to 32: 1.

When the weight ratio of the oil and the hydrophilic fumed silica is less than 1: 0.1, since the viscosity of the oil gel becomes excessively high due to the large amount of the hydrophilic fumed silica, there arises a problem that the stickiness becomes worse or a structure difficult to be released by external force may be formed do.

On the other hand, when the weight ratio is more than 32: 1, the liquid component due to the oil becomes excessively large, which leads to the problem that the silica particles are concentrated and the particle formation proceeds excessively.

At this time, the oil is stirred at a rate of 100 to 300 rpm for 10 to 15 minutes while introducing the hydrophilic fumed silica.

In addition, when a large amount of hydrophilic fumed silica is added for a short time, the mixture is not easily released, so a small amount of the hydrophilic fumed silica is slowly added to the dispersion to confirm that the hydrophilic fumed silica is well dispersed in the oil.

Especially, as the hydrophilic fumed silica content increases, the viscosity increases and becomes stiff.

Therefore, when the oil and the hydrophilic fumed silica are mixed, the hydrophilic fumed silica is added to the oil at a rate of 0.3 to 1.2 g / min relative to 100 g of the oil.

Next, the above oil gel manufacturing method includes a step of mixing the above-mentioned oil gel with an additive.

The above-mentioned structured additive can perform cross-linking action between silica over a wider range than a compound containing a functional group capable of hydrogen bonding at only one end of the molecule.

In addition, the oil gel manufacturing method may further include removing the bubbles in the oil gel by reducing the pressure of the oil gel at a pressure of 1.5 to 7.5 psi.

At this time, the produced oil gel is decompressed to the above-mentioned range to sufficiently remove the air bubbles generated during the mixing, so that the oil gel which is opaque due to air bubbles can be completed transparently.

Hereinafter, specific embodiments of the present invention will be described. However, the embodiments described below are only intended to illustrate or explain the present invention, and thus the present invention should not be limited thereto.

Example  One

The homomixer was gradually added with 6 wt% of hydrophilic fumed silica while stirring the oil at 8000 RPM for 10 minutes. When a large amount of hydrophilic fumed silica was added for a short period of time, a small amount of the hydrophilic fumed silica was gradually introduced into the oil so that the hydrophilic fumed silica was well dispersed in the oil.

When the hydrophilic fumed silica was added, 0.1 wt% of polyethylene glycol was further added, and mixing was continued until uniformly mixed.

Immediately after completion of the mixing, the oil gel was observed under a reduced pressure for 5 hours under a pressure of 5 psi to remove air bubbles generated during the mixing to finally produce a transparent oil gel.

0.2 ml of the prepared oil gel was placed on a 45-degree inclined surface to measure the length of the oil flowing down for 1 minute.

Example  2

9% by weight of hydrophilic fumed silica was slowly added to the homomixer while stirring the oil at 8000 RPM for 10 minutes. When a large amount of hydrophilic fumed silica was added for a short period of time, a small amount of the hydrophilic fumed silica was gradually introduced into the oil so that the hydrophilic fumed silica was well dispersed in the oil.

When the hydrophilic fumed silica was added, 0.1 wt% of polyethylene glycol was further added, and mixing was continued until uniformly mixed.

Immediately after completion of the mixing, the oil gel was observed under a reduced pressure for 5 hours under a pressure of 5 psi to remove air bubbles generated during the mixing to finally produce a transparent oil gel.

0.2 ml of the prepared oil gel was placed on a 45-degree inclined surface to measure the length of the oil flowing down for 1 minute.

In addition, the external force was applied to the prepared oil gel to measure a change in viscosity which changes as the external force increases.

Comparative Example  One

6% by weight of hydrophobic fumed silica was slowly added to the homomixer while stirring the oil at 8000 RPM for 10 minutes. When a large amount of hydrophobic fumed silica was added for a short period of time, a small amount of the hydrophobic fumed silica was slowly added to the oil so that the hydrophobic fumed silica was well dispersed in the oil.

After the addition of the hydrophobic fumed silica, 0.1 wt% of polyethylene glycol was further added, and mixing was continued until uniformly mixed.

Immediately after completion of the mixing, the oil gel was observed under a reduced pressure for 5 hours under a pressure of 5 psi to remove air bubbles generated during the mixing to finally produce a transparent oil gel.

0.2 ml of the prepared oil gel was placed on a 45-degree inclined surface to measure the length of the oil flowing down for 1 minute.

Comparative Example  2

A 9% by weight hydrophobic fumed silica was slowly added to the homomixer while stirring the oil at 8000 RPM for 10 minutes. When a large amount of hydrophobic fumed silica was added for a short period of time, a small amount of the hydrophobic fumed silica was slowly added to the oil so that the hydrophobic fumed silica was well dispersed in the oil.

After the addition of the hydrophobic fumed silica, 0.1 wt% of polyethylene glycol was further added, and mixing was continued until uniformly mixed.

Immediately after completion of the mixing, the oil gel was observed under a reduced pressure for 5 hours under a pressure of 5 psi to remove air bubbles generated during the mixing to finally produce a transparent oil gel.

0.2 ml of the prepared oil gel was placed on a 45-degree inclined surface to measure the length of the oil flowing down for 1 minute.

In addition, the external force was applied to the prepared oil gel to measure a change in viscosity which changes as the external force increases.

Comparative Example  3

The homomixer was stirred at 8000 RPM for 10 minutes, and 9 wt% of a copolymer of hydrogenated styrene and isoprene, which is a thickening polymer, was added.

Immediately after completion of mixing, the oil gel was observed under a reduced pressure of 5 psi under a pressure of 5 psi to remove air bubbles generated during mixing to finally produce a transparent oil gel.

The external force was applied to the prepared oil gel to measure the change in viscosity as the external force increased.

Results 1

The lengths of the oil gels prepared according to Examples 1 and 2 and the oil gels prepared according to Comparative Examples 1 and 2 were measured on the slopes and the results of the measurements were as shown in Table 1 below .

Fumed silica Run length 6 wt% Example 1 7.0 cm Comparative Example 1 Run down 9 wt% Example 2 2.0 cm Comparative Example 2 Run down

Through the above experiment, it was confirmed that, in the oil gel composed of the hydrophilic fumed silica of Examples 1 and 2 and the hydrophobic fumed silica of Comparative Example 1 and Comparative Example 2, depending on the nature of the fumed silica, The viscosity of the gel was comparable.

Table 1 shows that as the hydrophilic fumed silica content increases, the viscosity can be easily adjusted from a soft gel to a hard gel and that hydrophilic fumed silica can form an oil gel even with a small amount of hydrophilic fumed silica compared to hydrophobic fumed silica .

Experimental Result 2

The external force was applied to the oil gel prepared according to Example 2, Comparative Example 2 and Comparative Example 3 to measure a change in viscosity which changes with increasing external force. The results are shown in a thick solid line in Example 2, Example 2 is shown by a thin solid line and Comparative Example 3 is shown by a dotted line in the graph of Fig.

Through the above experiment, the copolymer of hydrophilic fumed silica as the oil gel of Example 2, the oil gel of the hydrophobic fumed silica of Comparative Example 2 and the hydrogenated styrene and isoprene of Comparative Example 3 as Component The degree of ease of the structure was easily solved by the external force.

Referring to the graph of FIG. 1, SHEAR RATE is a numerical value indicating how much the rotation is performed per hour. The larger the value, the larger the external force is.

The initial viscosity of the oil gel of Example 2 was the highest, but as the external force was larger, the viscosity of the oil gel rapidly decreased as compared with Comparative Example 2 and Comparative Example 3.

In addition, Comparative Example 2, which is a hydrophobic fumed silica component, did not show a significant difference in the rate of decrease in viscosity as compared with Comparative Example 3 in which the commercialized thickening polymer was used as a component.

The oil gel of Example 2 containing 9% by weight of hydrophilic fumed silica as the component was compared with the oil of Comparative Example 2 containing 9% by weight of hydrophobic fumed silica as the component and the thickening polymer of Comparative Example 3, And it was confirmed that the oil gel could be easily mixed by adding other ingredients to the oil gel.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit of the invention as set forth in the appended claims. The present invention can be variously modified and changed by those skilled in the art, and it is also within the scope of the present invention.

Claims (9)

Oil and hydrophilic fumed silica wherein the oil and the hydrophilic fumed silica are present in a weight ratio of 1: 0.1 to 32: 1.
The method according to claim 1,
The oil may be selected from the group consisting of argan oil, camellia oil, castor oil, coconut oil, corn oil, jojoba oil, cottonseed oil, soybean oil, walnut oil, wheat germ oil, peach seed oil, olive oil, peanut oil, sunflower seed oil, Kelendula oil, one leaf butter, shea butter, mineral oil extracted from petroleum, caprylic / capric triglyceride, and combinations thereof.
Oil gel.
The method according to claim 1,
The oil gel further comprises an additive, and the additive includes two or more functional groups selected from the group consisting of a thiol group, an amine group, a phosphonate group, a carboxyl group, a hydroxyl group, an imidazole group, a diol group, Compound
Oil gel.
The method of claim 3,
Wherein the hydrophilic fumed silica and the additive are present in a weight ratio of 1: 0.6 to 120: 1
Oil gel.
The method of claim 3,
Said oil gel comprising from 86 to 96% by weight of oil, from 3 to 12% by weight of hydrophilic fumed silica and from 0.1 to 2% by weight of additives
Oil gel.
And mixing the oil with hydrophilic fumed silica in a weight ratio of 1: 0.1 to 32: 1.
The method according to claim 6,
The hydrophilic fumed silica is added at a rate of 0.3 to 1.2 g / min relative to 100 g of the oil
Oil gel manufacturing method.
The method according to claim 6,
Further comprising the step of mixing the additive with the oil gel, wherein the additive is selected from the group consisting of a thiol group, an amine group, a phosphonate group, a carboxyl group, a hydroxyl group, an imidazole group, a diol group, Lt; RTI ID = 0.0 >
Oil gel manufacturing method.
The method according to claim 6,
And removing the air bubbles inside the oil gel by reducing the pressure of the oil gel
Oil gel manufacturing method.

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