KR20190085364A - Method for fabrication of emulsion containing cellulose nanofiber and emulsion prepared by the method - Google Patents

Abstract

The present invention provides a manufacturing method of an emulsion containing cellulose nanofibers (CNF), which comprises: a step (a) of supplying a suspension containing water and cellulose ingredients, and oil to a fluid collision device; a step (b) of injecting the suspension and the oil supplied from the step (a) at a high pressure towards one collision point through a plurality of nozzles provided in the fluid collision device; a step (c) of minutely fibrillating the cellulose contained in the suspension by collision energy generated when the fluid collides at the one collision point, and micronizing particles of the oil; and a step (d) of coupling particles of micronized oil to the fibrillated cellulose to be dispersed in water and emulsified. In addition, the present invention provides an emulsion manufactured by the method. Accordingly, the present invention can maintain emulsion stability for a long term without emulsifiers.

Description

TECHNICAL FIELD The present invention relates to a method for producing an emulsion containing cellulose nanofibers and an emulsion prepared by using the same. BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an emulsion containing cellulose nanofibers,

The present invention relates to a method for producing an emulsion containing cellulose nanofibers and an emulsion produced using the same.

Emulsion or emulsion (hereinafter referred to as "emulsion") collectively refers to a state in which one of two liquids which do not mix with each other is dispersed in a small particle state on the other side. At this time, the two liquids which are not mixed with each other may be water and oil, and water and oil are difficult to mix with each other as their polarities are different from each other.

Here, it is necessary to add a surfactant or an emulsifier (hereinafter referred to as "emulsifier") as a third component in order to mix two liquids which are not mixed with each other or to maintain the mixed state continuously. At this time, the added emulsifier is oriented adsorption on the interface between oil and water to lower the interfacial free energy, thereby facilitating the operation of emulsification, while suppressing the phase separation rate of water and oil to maintain the emulsion state do.

The technique for manufacturing such an emulsion is disclosed in Korean Patent Publication No. 10-2001-0103463 (filed on May 10, 2000, published on November 23, 2001), Korean Patent Publication No. 10-2001-0038746 1999, October 27, 2001, May 15, 2001).

At this time, the emulsion is generally used as a base for manufacturing cosmetics. Conventional emulsions are prepared by adding a separate emulsifier to disperse the aqueous liquid phase and the oily liquid phase particles uniformly and without agglomeration, followed by stirring. Here, the conventional emulsion could weaken the emulsifying property after a certain period of time, and the emulsifying agent added separately could cause skin irritation and allergic stimulation of the user depending on the chemical components thereof.

Thus, emulsions that maintain emulsion stability without the addition of chemical additives such as emulsifiers are required.

It is an object of the present invention to provide a technique capable of producing an emulsion in which emulsion stability is maintained without any chemical additives.

In order to accomplish this object, a method for producing an emulsion containing cellulose nanofibers according to an embodiment of the present invention comprises the steps of: (a) supplying a suspension and oil containing water and a cellulose component to a fluid collision apparatus; ; (b) injecting the suspension and the oil supplied in the step (a) through the plurality of nozzles provided in the fluid impact device at a high pressure toward one impact point; (c) the cellulose contained in the suspension is finely divided and fibrillated by the impact energy generated when the fluid collides at one collision point, and the particles of the oil are refined; And (d) emulsifying the dispersed oil particles while dispersing the particles of the oil microfined in the shredded cellulose.

Here, in the step (a), the cellulose is extracted from a woody or non-woody system.

At this time, in the step (a), the cellulose may be extracted from bamboo.

In the step (d), the content of the oil may be within 50 wt% of the total weight of the emulsion.

In addition, an emulsion can be produced by the above-described production method.

As described above, the present invention has the following effects.

First, even if an additional chemical additive for emulsifying oil and water or an emulsifier such as a surfactant is not added, the size of the cellulose contained in the suspension tends to be reduced due to the fluid collision. At this time, It is possible to prepare an emulsion in which oil and water are emulsified in the hydrophobic part exposed to the emulsion, and emulsion stability of the emulsion can be maintained in the long term even without emulsifying agent.

Secondly, it is possible to prepare an emulsion in which oil and water are emulsified using cellulose extracted from nature without adding an additional emulsifier, and in addition to the cellulose nano fiber produced by the above-described cellulosic shrinkage, It is possible to manufacture an environmentally friendly emulsion for application of oil, and it is possible to minimize the occurrence of skin irritation and allergies of the user.

Third, when cellulose nano fiber (CNF) alone is applied to cosmetics, medicines, and the like, it is able to take away the moisture of the skin by the hydrophilic component when it is used in contact with the human body. However, Can be increased.

1 is a schematic view schematically showing a fluid impact device used for producing an emulsion of the present invention.
Fig. 2 illustrates the emulsion (A) according to one embodiment of the present invention produced using the manufacturing method of Fig. 1 and the comparative emulsion (B) of the comparative example with the present invention.

The preferred embodiments of the present invention will be described in more detail with reference to the accompanying drawings, in which the technical parts already known will be omitted or compressed for simplicity of explanation.

≪ Description of fluid collision device >

Before describing the method of manufacturing an emulsion, a brief description will be given of a fluid impact device used for manufacturing an emulsion or an Aqueous Counter Collision (ACC) device (hereinafter referred to as a 'fluid impact device').

1 is a schematic view schematically showing a fluid impact device used for producing an emulsion of the present invention.

1, the fluid impact device ACC includes a storage tank ST, a plunger P, a fluid impingement unit FC, and a cooling unit C, .

Here, the storage tank ST stores a fluid F, such as a suspension containing a cellulose component, and a fluid F 'containing fine particles passing through the cooling unit C through a process to be described later, ) Is also introduced.

The plunger P is a pressurizing means for generating pressure such that the fluid F moved from the storage tank ST can be moved to a high pressure state and the fluid F discharged by the plunger P in a high pressure state Is introduced into the chamber body of the fluid collision unit FC. At this time, a collision section is provided in the chamber body of the fluid collision unit (FC), and the high-pressure fluid (F) introduced into the chamber main body passes through two to three or more injection nozzles (JN) The fluid F collides with the particles colliding with one collision point in the collision section, and the size of particles contained in the fluid F can be reduced by the fluid collision.

A separate hopper is provided on the upper side of the chamber body for introducing the fluid F discharged from the plunger P in a high pressure state. The hopper is connected to each of the injection nozzles JN located in the chamber by a fluid path A fluid supply piping unit may be provided.

Thereafter, cooling is performed by a heat exchange method in order to recover the temperature level of the fluid F 'including the micronized particles which become high temperature by the heat generated in the process of fluid collision, and then the fluid F' ) Moves into the storage tank.

That is, the fluid collision device ACC can be finely dispersed to a small size by reducing the particle size included in the fluid F due to the collision energy generated by the collision of the fluid F injected from the injection nozzle JN.

For reference, the collision pressure and the number of collisions of the fluid collision device ACC are controllable, and the particle size included in the fluid F 'containing the particles after the collision after the collision can be changed depending on the controlled conditions .

≪ Explanation of Method for Manufacturing Emulsion Containing Cellulose Nanofibers >

1. Step (a)

(a) is a step of supplying a suspension and oil containing water and a cellulose component to a fluid collision device (ACC). At this time, the suspension in fluid state and the oil are stored together in the storage tank ST of the fluid collision device ACC and can be moved to the injection nozzle JN.

Here, the cellulose contained in the suspension may be extracted from woody or non-woody systems. For example, cellulose can be extracted from herbaceous systems such as bamboo and cotton, which correspond to the non-woody system.

At this time, since the characteristics of specific cellulose vary depending on where cellulose is extracted, the ratio of suspension to oil supplied to the fluid collision device (ACC) and the ratio of water to cellulose contained in the suspension may vary.

The oil contained in the emulsion of the present invention may be an oil extracted from plants such as olive, soybean, sunflower, grape seed and the like.

At this time, the content of the oil may be within 0.001 wt% to 50 wt% of the total weight of the emulsion, and the content of the suspension may be within 50 wt% to 99.999 wt% of the total weight of the emulsion. At this time, the ratio of water to cellulose contained in the suspension may be 9: 1, wherein the content of cellulose may be 1 wt% to 10 wt% of the total weight of the suspension. Here, when the content of cellulose is out of the above-mentioned range or the content of oil is higher than the above-mentioned value, the dispersion stability is lowered and the emulsion stability is lowered and layer separation may occur between oil and water. If the oil content is less than 0.001 wt%, the moisture resistance of the emulsion produced may be lowered.

As another example, it is also possible to supply the fluid collision device (ACC) with cellulose nanofibers (CNF) and oil dispersed in water, thereby preparing an emulsion through the steps described below. That is, since the cellulose component of the suspension supplied to the fluid collision device (ACC) can be any one of cellulose and cellulosic nanofibers (CNF) before being nanoized, the cellulose referred to in the present invention is limited to the cellulose before being nano- But also the above-described cellulose nanofibers (CNF).

For reference, it is stable that cellulose is dispersed in water. Thus, the cellulose nanofibers (CNF) nanofibrated through the fluid collision device (ACC) can be produced by dispersing in water. In this case, the cellulose nanofiber (CNF) alone is applied to cosmetics, medicines, and the like, and when it is used in contact with the human body, it can take away the moisture of the skin by the hydrophilic component. However, Can be increased.

2. Step (b)

(b) is a step of injecting the suspension and the oil supplied in the step (a) through the plurality of injection nozzles JN provided in the fluid collision device ACC toward the one collision point CP.

Here, it is preferable that the plurality of injection nozzles JN inject the injected fluid at a high pressure of 10 bar to 2000 bar.

In this case, if the pressure is too low, the emulsion stability of water and oil can not be expected, so that it may be difficult to produce emulsion of stable formulation. If the pressure is too high, a fluid impact device (ACC) . ≪ / RTI >

3. Step (c)

In step (c), the cellulose contained in the suspension finely fibrillates by the collision energy generated when the fluid collides at one collision point, and the particles of the oil are refined.

the suspension and the oil supplied in the step (a) are sprayed to one point inside the chamber in the fluid collision unit FC through the injection nozzle JN, and at this time, the shear stress applied to the fluid through the injection nozzle JN And the collision energy generated when the ejected fluid collides with the cavitation at the end of each of the plurality of injection nozzles JN. That is, due to the fluid-to-fluid collision, the cellulose may be torn into a small size, and the hydrophobic portion may be exposed at the torn portion.

Further, the oil is dispersed in a small size while passing through the injection nozzle JN.

4. Step (d)

In the step (d), the particles of the oil that has been micronized in the pulverized cellulose are combined and emulsified while being dispersed in water.

In step (C), the oil dispersed in a small size while passing through the spray nozzle JN, that is, the micronized oil is defatted and bonded to the hydrophobic part of the expressed cellulose, and the cellulose and the oil pass through the spray nozzle JN , An emulsion in which water and oil are emulsified by means of a shattered cellulose can be produced.

That is, the present invention can produce an environmentally friendly emulsion in which water and oil are emulsified by containing cellulose nanofibers, without adding an additional emulsifying agent such as a surfactant or a chemical additive for emulsifying oil and water.

In addition, since the cellulosic nanofibers act as thickeners in the emulsion containing the cellulose nanofibers prepared by the above-described production method, the viscosity can be controlled by controlling the content of the cellulose nanofibers. By adjusting the composition ratio of the emulsions, May be provided. That is, the emulsion of the present invention can be used for a human body such as skin, mucous membrane, scalp, hair and the like, and can be used for a body lotion such as a lotion, a cleanser, a skin lotion, a makeup base, a foundation, a cream, a pack, a shampoo, a rinse, a body cleanser, , Ointments, gels, and the like.

At this time, the emulsion of the present invention can be further added with a perfume, a sunscreen agent, a dye, a pigment and the like as well known in the above-mentioned application fields, and the kind and amount thereof can be appropriately selected and contained by a person skilled in the art .

Meanwhile, an emulsion can be prepared through the above-mentioned production method, and examples and comparative examples will be described in order to facilitate understanding of the present invention. However, the following embodiments are merely preferred embodiments of the present invention, and the present invention is not limited to the following embodiments.

FIG. 2 illustrates an emulsion (A) according to one embodiment of the present invention produced using the manufacturing method of FIG. 1 and an emulsion (B) of a comparative example with the present invention.

Example

After supplying a suspension and oil containing water and a cellulose component to the fluid collision device (ACC), the suspension and oil are injected at high pressure toward one collision point (CP) through two injection nozzles (JN) An emulsion (A) in which the oil was properly emulsified was prepared.

To describe the manufacturing process of the embodiment of the present invention in more detail, 4 kg of a 2 wt% bamboo cellulose suspension is injected into the hopper located at the top of the chamber of the fluid collision unit (FC) in the fluid collision device (ACC). The final pressure of the spray nozzle (JN) of the fluid collision unit (FC) was 2000 bar and the temperature of the cellulosic suspension was controlled between 28 and 30 ° C through the setting of the cooling device. The discharge amount per minute in the fluid collision device (ACC) was set at 3L. When 4 kg of the cellulosic suspension passed through the fluid impingement unit (FC) 5 times, the syringe was placed inside the hopper and 1 kg of olive oil was added. When the initial olive oil is injected, yellow olive oil is found in the form of a bundle, but it is confirmed that the fluid collision unit (FC) is uniformly dispersed when it is repeatedly passed through several times. After the oil was added, 5 kg of the water + cellulose + oil mixture was circulated 25 times, and the emulsion (A) as the emulsified solution was recovered. In the final emulsified solution, the content of cellulose, water and oil in the emulsion (A) is 1.6 wt% (80 g) of cellulose, 78.4 wt% of water (3920 g) and 20 wt% of oil (1000 g).

Comparative Example

First, water and oil were supplied to the fluid collision device ACC and then injected at high pressure toward one collision point (CP) through at least two injection nozzles JN to obtain a mixture of water and oil. Thereafter, the cellulose nanofibers (CNF) were added and then stirred for a predetermined period of time by a conventional method to prepare a comparative emulsion (B).

Here, the manufacturing process of the comparative example will be described in more detail. 3 kg of pure water is injected into the hopper located at the top of the chamber of the fluid collision unit (FC) of the fluid impact device (ACC) fluid collision device (ACC). The final pressure of the spray nozzle (JN) of the fluid collision unit (FC) was 2000 bar and the temperature of the water was controlled between 28 and 30 ° C through the cooling device setting. The discharge amount per minute in the fluid collision device (ACC) was set at 3L.

First, when 3 kg of water passed through the fluid collision unit (FC) 5 times, the syringe was placed inside the hopper and 2 kg of olive oil was added. When the olive oil is injected into the hopper without a syringe, the oil floats on the water and sticks to the hopper wall and does not enter the fluid impingement unit. After the oil was added, 5 kg of water + oil mixture was circulated 25 times to collect the mixed solution.

Thereafter, 1 kg of the previously prepared water + oil mixture and 1 kg of the previously prepared 3.2 wt% cellulosic nanofiber suspension were stirred at a high speed for 5 minutes in a homomixer to prepare an emulsified comparative emulsion (B) . In a total of 2 kg of the emulsified solution, the content of cellulose, water and oil in the comparative emulsion (B) is 1.6 wt% (32 g), water 78.4 wt% (1568 g) and oil 20 wt% (400 g) respectively.

Comparative and analysis of the above-described embodiment and the comparative example with reference to FIG. 2 revealed that, in the case of the emulsion (A), a white flow was easily formed. At this time, it can be confirmed that water, cellulose nanofibers, and oil are evenly dispersed and emulsified in the emulsion (A) without the separated sections. In addition, the formulation did not change even after a certain period of time, and it was confirmed that the emulsion stability was maintained for a long time.

In the case of the comparative emulsion (B), since the oil and water are not properly emulsified, the color thereof is similar to the yellow added to the oil added to the comparative emulsion (B), and is made into a formulation close to the jelly formulation, It is not a formulation. In addition, the existence of a section with layer separation is also found.

As a result, the addition of cellulose nanofibers to a solution of water and oil to simply emulsify water and oil does not result in emulsified emulsions, but because of the fluid collision, the cellulose contained in the suspension is revealed by tearing It can be confirmed that the oil and water are emulsified due to the hydrophobic part.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. And the scope of the present invention should be understood as the scope of the following claims and their equivalents.

ACC: Fluid collision device
ST: Storage tank
P: plunger
FC: Fluid impact unit
JN: injection nozzle
C: Cooling unit
CP: crash point

Claims (5)

(a) feeding a suspension and oil containing water and a cellulose component to a fluid impingement device;
(b) high-pressure injection of the suspension and oil supplied in the step (a) through a plurality of injection nozzles provided in the fluid impact device toward one impact point;
(c) the cellulose contained in the suspension is finely divided and fibrillated by the impact energy generated when the fluid collides at one collision point, and the particles of the oil are refined; And
(d) emulsifying while dispersing the particles of the oil that has been micronized in the shredded cellulose into water; and
A method for producing an emulsion containing cellulose nanofibers (CNF).
The method according to claim 1,
In the step (a)
Wherein the cellulose is extracted from a woody or non-woody system
A method for producing an emulsion containing cellulose nanofibers.
3. The method of claim 2,
In the step (a)
Characterized in that the cellulose is extracted from bamboo
A method for producing an emulsion containing cellulose nanofibers.
The method according to claim 1,
In the step (a)
Wherein the content of the oil is 0.001 wt% to 50 wt% of the total weight of the emulsion
A method for producing an emulsion containing cellulose nanofibers.
5. An emulsion prepared by the method according to any one of claims 1 to 4.

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