KR102618140B1 - A Method for Producing a Homogeneous Mixture and the Homogeneous Mixture Using the Same - Google Patents

Abstract

The present invention relates to a method for producing a homogeneous mixture and a homogeneous mixture thereby. A method for producing a homogeneous mixture includes the steps of stirring two immiscible liquid components; A step in which two liquid components are mixed and subjected to primary high-pressure homogenization; A step of first ultrasonic treatment on the first homogenized component; Adjusting the component ratio of the first homogeneous solution; A second high-pressure homogenization step for the first homogenized solution with the adjusted component ratio; A second step of ultrasonic treatment on the second homogenized solution; And it includes the step of producing a homogeneous mixture that does not separate layers from each other.

Description

Method for producing a homogeneous mixture and a homogeneous mixture thereby {A Method for Producing a Homogeneous Mixture and the Homogeneous Mixture Using the Same}

The present invention relates to a method for producing a homogeneous mixture and a homogeneous mixture thereby, and specifically to a method for producing a homogeneous mixture in which water and oil components are homogeneously mixed, and to a homogeneous mixture thereby.

An emulsifier or surfactant must be used to uniformly mix the water and oil components without forming a layer. Emulsifiers are compounds with hydrophilic and lipophilic groups and have the function of emulsifying them by binding to hydrophilic and lipophilic compounds. Combining two immiscible compounds using such an emulsifier does not have the characteristics of a uniform or homogeneous mixture. Additionally, emulsifiers themselves can be harmful compounds to the human body. Additionally, if an emulsifier is not used, separation of the water and oil layers may occur over time. Therefore, there is a need to develop a technology that allows water and oil components to be mixed without using emulsifiers. Regarding the homogeneous mixture of water and oil components, Patent Publication No. 10-2002-0032293 discloses an oil-water homogenization device. Additionally, Patent Publication No. 10-2012-0072760 discloses a device for uniform mixing of water and oil. However, the prior art does not disclose a technology in which water and oil components can be uniformly mixed and maintained for a long time. For the use of a homogeneous mixture of water and oil components in the cosmetic field, medical field or similar fields, it is necessary to maintain a homogeneous state for a long period of time, but the prior art or known art does not disclose such technology.

The present invention is intended to solve the problems of the prior art and has the following purposes.

Prior Art 1: Patent Publication No. 10-2002-0032293 (Keum Kyung-moon, published on May 3, 2002) Oil-water homogenization device Prior art 2: Patent publication number 10-2012-0072760 (Kang application, published on July 4, 2012) Water and oil mixing uniform device

The purpose of the present invention is to provide a method for producing a homogeneous mixture in which water and oil are uniformly mixed and the uniform mixing state can be maintained for a long period of time, and to provide a homogeneous mixture thereby.

According to a preferred embodiment of the present invention, a method for producing a homogeneous mixture includes the steps of stirring two immiscible liquid components; A step in which two liquid components are mixed and subjected to primary high-pressure homogenization; A step of first ultrasonic treatment on the first homogenized component; Adjusting the component ratio of the first homogeneous solution; A second high-pressure homogenization step for the first homogenized solution with the adjusted component ratio; A second step of ultrasonic treatment on the second homogenized solution; And it includes the step of producing a homogeneous mixture that does not separate layers from each other.

According to another suitable embodiment of the present invention, the two liquid components are water and oil components.

According to another suitable embodiment of the present invention, the water and oil components are mixed at a weight ratio of 80:10 to 30 in the first homogenization process, and adjusted to a weight ratio of 100:0.1 to 10 in the component ratio adjustment step.

According to another suitable embodiment of the present invention, a pressure of 10,000 to 30,000 psi is applied during the first or second high pressure homogenization process.

According to another suitable embodiment of the present invention, ultrasonic waves of 20 kHz to 30 kHz are applied during the primary or secondary ultrasonic treatment process.

According to another suitable embodiment of the present invention, a homogeneous mixture of water and oil without layer separation is provided while the weight ratio of the water and oil components is 100:0.1 to 5.

The method for producing a homogeneous mixture according to the present invention ensures that two different components that do not mix with each other are uniformly mixed. For example, water and oil components are mixed uniformly without the use of emulsifiers. In addition, this uniform mixing state can be maintained for a long period of time and thereby can be effectively applied to various industrial fields. For example, the homogeneous mixture of water and oil prepared by the production method according to the present invention can be applied to the cosmetics field, food field, medical field, or similar fields, and the present invention is not limited thereto.

Figure 1 shows an example of a method for producing a homogeneous mixture according to the present invention.
Figure 2 shows an example of a homogenizer for the manufacturing method according to the present invention.
3 and 4 show an example of a homogenization module for the homogenization process according to the present invention.
Figure 5 shows an embodiment of a heat exchanger for the manufacturing method according to the present invention.
Figure 6 shows an embodiment of an ultrasonic unit for the manufacturing method according to the present invention.
Figures 7a to 7c show the EDS test results of the water and oil mixture prepared by the production method according to the present invention.
Figures 8a to 8d show FTIR test results of a water and oil mixture prepared by the production method according to the present invention.

Below, the present invention will be described in detail with reference to the embodiments shown in the attached drawings, but the examples are for a clear understanding of the present invention and the present invention is not limited thereto. In the description below, components having the same reference numerals in different drawings have similar functions, so unless necessary for understanding the invention, the description will not be repeated, and well-known components will be briefly described or omitted, but the present invention It should not be understood as being excluded from the embodiments.

Figure 1 shows an example of a method for producing a homogeneous mixture according to the present invention.

Referring to Figure 1, the method for producing a homogeneous mixture includes the step of stirring two liquid components that do not mix with each other (P11); A step in which the two liquid components are mixed and subjected to primary high-pressure homogenization (P12); A step in which the first homogenized component is subjected to first ultrasonic treatment (P13); A step in which the component ratio of the first homogeneous solution is adjusted (P14); A second high-pressure homogenization step (P15) for the first homogenized solution with the adjusted component ratio; A second ultrasonic treatment step for the second homogenized solution (P16); and a step (P17) of generating a homogeneous mixture in which layers are not separated from each other.

Two ingredients that are immiscible with each other may be prepared, and the two ingredients may be, for example, water and an oil ingredient. The oil component may be, but is not limited to, lavender oil, orange oil, phytoncide, pine oil, or similar extracts of natural plants. The two components may separate into layers when mixed unless an ingredient, for example an emulsifier, is added. Once these two ingredients are prepared, they can be mixed and stirred. The two components can be mixed and stirred at a weight ratio of water: oil component = 80: 10 to 30, preferably 80: 15 to 25, preferably 80: 20 (P11). A stirrer can be prepared, water and oil components are stirred in the stirrer (P11), and then high-pressure homogenization can be performed. The high-pressure homogenization process may be performed, for example, in a device such as a homogenizer, and a pressure of 10,000 to 30,000 psi may be applied in the homogenizer to proceed with the high-pressure homogenization process. In the homogenization process, two components can be made into a primary homogeneous solution through collision, mixing, shearing, and cavitation processes (P12). The created first homogeneous solution can be moved to a heat exchanger and cooled, and can be subjected to first ultrasonic treatment in this process (P13). For example, the primary ultrasonic treatment may be performed by an ultrasonic transducer with an output of 500 to 2,500 W at a temperature of 10 to 25° C., and the applied ultrasonic frequency may be 20 kHz to 30 kHz. Under these conditions, when the first ultrasonic treatment is performed (P13), a first mixed solution or a first homogeneous solution can be created. The first homogeneous solution can be diluted to adjust the component ratio of water and oil components (P14), and by adjusting the component ratio, the water and oil components can be water: oil component = 100: 0.1 to 10 in weight ratio. If the ingredient ratio is adjusted in this way, the second high-pressure homogenization process can proceed (P14). The secondary homogenization process may be performed in the same or similar manner as the primary homogenization process, and the secondary homogenization process may be performed with a pressure of 10,000 to 30,000 psi (P14). A secondary homogenized solution may be generated as the secondary homogenization process progresses, and the secondary homogenized solution may be transferred to a heat exchanger. Afterwards, the second ultrasonic treatment can be performed in the heat exchanger under the same or similar conditions as the first ultrasonic treatment (P16). And through this secondary ultrasonic treatment, a homogeneous mixture can be created (P17). For example, a homogeneous mixture of water and oil components may be created. The homogeneous mixture prepared in this way can be maintained in a homogeneously mixed state without layer separation even when stored for a long period of time. The first and second homogenization processes can be carried out in a homogenizer, and the homogenizer for the homogenization process is explained below.

Figure 2 shows an example of a homogenizer for the manufacturing method according to the present invention.

Referring to Figure 2, the homogenizer includes an input container 11 into which the raw material solution is input; A pressurizing module (13) that applies pressure to the input raw material solution; a homogeneous module (15) that turns the raw material solution into a homogeneous solution using the pressure applied by the pressurizing module (13); A heat exchanger (17) that stabilizes and discharges the homogeneous solution; and ultrasonic units 18a, 18b, and 18c that apply ultrasonic waves to the raw material solution or the homogeneous solution.

When the raw material solution stored in the input container 11 is guided to the transfer path 14, the drive unit 12, such as a pressure pump or motor, can operate the pressurizing module 13, such as a plunger capable of reciprocating movement. The raw material solution may be a raw material made homogeneous in a homogenizer, and may be composed of at least one solvent and at least one solute. Raw material solutions can be solutions of various types used in the food field, such as cooking oil, powdered milk, margarine or mayonnaise, or solutions used in the chemical field, such as ink, soap, fuel oil, vitamins, toothpaste, paint or perfume. . Alternatively, the raw material solution may include, but is not limited to, pharmaceuticals, dyes, silicones, resins, or similar substances. As it is pressurized by the pressurizing module 13, it can be moved along the transfer conduit 14 and input into the homogeneous module 15. The homogeneous module 15 may have the function of making a homogeneous solution by colliding the raw material solution and pulverizing and mixing it to a nano size. The homogeneous solution formed by the homogeneous module 15 is guided to the heat exchanger 17 via the guiding conduit 16, is stabilized, and can be discharged to the outside. According to one embodiment of the present invention, ultrasound may be applied to a raw material solution or a homogeneous solution. Specifically, an ultrasonic unit 18a may be placed inside or outside the input container 11 to apply ultrasonic waves to the raw material solution. The ultrasonic unit 18b is installed in the transfer conduit 14 and can apply ultrasonic waves to the flowing raw material solution. Alternatively, the ultrasonic unit 18c may be installed in the heat exchanger 18c. For example, an ultrasonic unit 18c may be installed below the heat exchanger 17 to apply ultrasonic waves to the homogeneous solution moving along the inside of the heat exchanger 14. By applying such ultrasound, the homogeneity and stability of the homogeneous solution can be improved. The ultrasonic units 18a, 18b, and 18c may be installed at various locations in the homogenizer to apply ultrasonic waves to the raw material solution or the homogenized solution. The ultrasonic units 18a, 18b, and 18c may apply ultrasonic waves of various frequencies, for example, ultrasonic waves having a frequency of 20 kHz to 10 MHz. Ultrasonic waves having various frequencies may be applied to the raw material solution or homogeneous solution.

3 and 4 show an example of a homogenization module for the homogenization process according to the present invention.

Referring to FIG. 3, the raw material solution moving along the transfer conduit 14 can be input into the homogeneous module 15, and the homogeneous module 15 includes three protection blocks 21a, 21b, and 21c. Each of the protection blocks 21a, 21b, and 21c may be connected to each other in a cylindrical or drum shape, and the homogenization means shown at the bottom of FIG. 2 may be placed inside the protection blocks 21a, 21b, and 21c. The first and third protection blocks 21a and 21c may have a relatively large length, and the second protection block 21b disposed in the middle may have a relatively small length. The protection blocks 21a, 21b, and 21c may be made of a material with a large specific gravity, such as metal, and may have a structure that prevents external vibration or shock from being transmitted to the homogeneous means disposed inside.

The transfer path 14 and the internal guidance path of the homogeneous module 15 may be connected, and a residence space 22 may be formed in the internal guidance path. The residence space 22 may be cylindrical in shape, extending with a relatively large inner diameter relative to the conveying path 14, and having an inner conveying path 14a extending with the same or similar diameter as the conveying path 14. ) can be connected to. A homogeneous cell (HC) may be connected to the internal transport path 14a. The homogeneous cell HC includes a homogeneous path having a relatively large diameter compared to the internal transport path 14a and a collision inducing block 23a disposed inside the homogeneous path. The raw material solution flowing into the homogeneous cell (HC) from the internal transfer path 14a flows into the inflow space having a relatively large diameter and then collides with the collision inducing block 23a, and then collides with the collision inducing block 23a and the homogeneous cell ( It may flow in a horizontal direction along the gap path 23b formed between HC). Thereafter, it may be moved in the vertical direction at the end of the collision inducing block 23a and flow along the cavitation path 24, which is relatively small compared to the internal transport path 14a. Thereafter, the raw material solution may be guided to the diffusion block 25 in which the diffusion path 25a is formed. The diffusion path 25a may have a fallopian tube shape or a fan shape, and the raw material solution guided along the diffusion path 25a may flow along a homogeneous discharge path 26 connected to the guide path 16. In this way, inside the homogeneous cell (HC), the raw material solution can become a homogeneous solution through collision, mixing, shear, and cavitation processes. Below, the structure of the homogeneous cell (HC) that produces this action is explained in detail.

Referring to FIG. 4, the homogeneous cell (HC) connected to the internal transport path 14a extends in a cylindrical shape with a constant diameter from the inclined inducing portion 31 and the inclined inducing portion 31 whose cross-sectional area gradually increases along the extension direction. It may be composed of a path forming space 32. Additionally, a collision inducing block 23a may be placed inside the path forming space 32. The collision inducing block 23a may have a cylindrical shape with a smaller diameter and length than the diameter and length of the path forming space 32. For example, the diameter of the collision inducing block 23a may be 1/2 to 9/10 of the diameter of the path forming space 32. And the length of the collision inducing block 23a may be 2/5 to 3/4 of the length of the path forming space 32. The collision guidance block 23a may be separated from the rear surface of the path forming space 32 and disposed to form a vertical guidance path 33, and the cross-sectional area of the vertical guidance path 33 may be smaller than that of the gap path 23b. You can. The raw material solution may move in the horizontal direction along the gap path 23b and then flow in the vertical direction along the vertical guide path 33. A cavitation path 24 may be connected to the central portion of the path forming space 32, and the cross-sectional area of the cavitation path 24 may be 1/5 to 1/2 of the cross-sectional area of the internal conveying path 14a, e.g. For example, it may be in the form of a nozzle with a diameter of 60 to 85 ㎛. The raw material solution flowing along the internal transfer path 14a may be guided to the diffusion block 25 in which the diffusion path 25a described above is formed. Afterwards, the raw material solution becomes a homogeneous solution and can flow into the heat exchanger.

Figure 5 shows an embodiment of a heat exchanger for the manufacturing method according to the present invention.

Referring to Figure 5, the heat exchanger 17 includes a housing 41; A heat exchange tube 42 disposed in a coil shape inside the housing 41; an inlet tube (43) delivering the homogeneous solution to the heat exchange tube (42); and a discharge tube 44 that discharges the homogeneous solution from the heat exchange tube 42 to a reservoir of the homogeneous solution, such as a storage tank. A refrigerant tube that guides the flow of refrigerant may be disposed inside the heat exchanger 17. Ultrasonic units 45a, 45b, and 45c may be placed at various positions in the heat exchanger 17 having this structure. The ultrasonic units 45a, 45b, and 45c may be disposed on the peripheral surface of the housing 41, on the cover of the housing 41, or on the lower side of the housing 41. When the ultrasonic unit 45b is disposed on the cover of the housing 41, the ultrasonic transmission member 451 is coupled to the ultrasonic unit 45b to apply ultrasonic waves to the homogeneous solution transported inside the housing 41. When the ultrasonic unit 45c is placed below the housing 41, the ultrasonic transmission plate 452 may be placed below the housing 41. A plurality of vibration elements may be disposed on the ultrasonic transmission plate 452, and ultrasonic waves may be guided in a predetermined direction by the vibration elements. The ultrasonic units 45a, 45b, and 45c are disposed at various positions in the heat exchanger 17 and can apply ultrasonic waves to the homogeneous solution moving along the inside of the heat exchange tube 42. And the ultrasonic unit 45a may have an appropriate structure capable of applying ultrasonic waves to a homogeneous solution.

Figure 6 shows an embodiment of an ultrasonic unit for the manufacturing method according to the present invention.

Referring to FIG. 6, the ultrasonic unit may include a direction forming unit 51 and a plurality of vibration elements 52_1 to 52_N) disposed in the direction forming unit 51. Additionally, the ultrasonic unit may include a limiting attachment unit 55 formed above the direction forming unit 51 and a transmission blocking member 57 formed along the circumferential surface of the limiting attachment unit 55. Additionally, the ultrasonic unit may include a fixing unit 53, and an ultrasonic blocking unit 54 may be disposed along the peripheral surface of the fixing unit 53. Each vibration element (52_1 to 52_N) includes a piezoelectric element and may be made of a transducer structure that converts electrical vibration into mechanical vibration. The direction forming unit 51 may function as an ultrasonic lens that guides the ultrasonic waves generated from the vibration elements 52_1 to 52_N in a predetermined direction, and may be made of a convex lens or concave lens structure to guide the ultrasonic waves in various directions. The limiting attachment unit 55 allows the ultrasonic waves generated from the vibration elements 52_1 to 52_N to be transmitted in a predetermined direction through the ultrasonic transmission member 56 while the ultrasonic unit is disposed inside the input container, transfer path, or heat exchanger. The ultrasonic unit may be coupled to and fixed to the heat exchanger by the fixing unit 53. An ultrasonic blocking unit 45 is disposed along the circumferential surface of the fixing unit 53 to block ultrasonic waves from being transmitted along the housing of the heat exchanger or through other paths. The transmission blocking member 57 or the ultrasonic blocking unit 54 may be made of a porous material or sound-absorbing material that absorbs vibration, and the ultrasonic transmission member 56 may be made of a high-density metal material. A vibration element that receives reflected ultrasonic waves may be disposed in the ultrasonic unit. Since the ultrasonic unit transmits ultrasonic waves to a homogeneous solution and thereby induces dispersion of the dispersoid, it is necessary to transmit the ultrasonic waves in a direction that reduces the reflected ultrasonic waves. Therefore, the transmission direction of ultrasonic waves must be adjusted according to the size or amount of the reflected wave received by the receiving vibration element. Intensity information of the reflected ultrasonic waves received by the receiving vibration element may be transmitted to the control unit, and the control unit may adjust the application direction of the ultrasonic unit according to the received intensity information. The ultrasonic transmission direction of the ultrasonic unit can be adjusted in various ways, for example, by adjusting the radius of curvature of the direction forming unit 51. Application of ultrasound to a homogeneous solution can be accomplished in various ways.

A homogeneous mixture of water and oil was prepared using the homogenizer described above.

Example

A. Water and orange oil were prepared in a weight ratio of water:orange oil = 85:15, stirred in a stirrer, and added to the homogenizer.

B. A pressure of 15,000 psi was applied to the homogenizer to homogenize the mixed solution to create a first homogeneous solution, and ultrasonic treatment was performed by applying ultrasonic waves at 20 kHz with an output of 1,400 W at a temperature of 15°C.

C. The ultrasonicated first homogenized solution is diluted and the ingredient ratio is adjusted to water: orange oil = 95.5: 0.5, and the second homogenized and second ultrasonicated solutions are performed under the same conditions to homogenize 0.5% water and orange oil. The mixture was made.

test

The prepared homogeneous mixture of water and orange oil was subjected to Energy Dispersive Spectroscopy (EDS) and Fourier Transform Infrared Spectroscopy (FTIR) tests. For FTIR analysis ASTM E 1252 was used and for testing an Agilent Cary 670 (with 620 IR microscopy) with an MCT single point detector coupled to FTIR microscopy using a germanium slide-on ATR crystal was used. In the test process, 100% oil and homogeneous mixture were contrasted and presented in Figures 7a to 7c and Figures 8a to 8d.

The left and right sides of Figure 7a show the EDS test results for 100% oil on a Ti-stud, and the left and right sides of Figure 7b show the EDS test results for 100% oil on an Al-stud. And Figure 7c shows the test results on Ti and Al studs of the homogeneous mixture according to the present invention, respectively. As can be seen from FIGS. 7A to 7C, it can be seen that the homogeneous composition according to the present invention does not contain any components other than oil components.

The left and right sides of Figure 8a show the transmission test results of the KBr plate of 100% oil and 0.5% homogeneous mixture, respectively, and the left and right sides of Figure 8b show the platinum (platinum) plate of 100% oil and 0.5% oil mixture, respectively. It shows the test results of reflectance and extraction drying ATR (Attenuated Total Reflection) of the Au) plate. The left and right sides of Figure 8c show the dry ATR test results of the 0.5% homogeneous mixture and the test results of the platinum plate reflective mule, respectively. And the left and right sides of Figure 8d show the test results of liquid ATR of 0.5% homogeneous mixture and liquid ATR of 100% oil, respectively.

From the test results, no non-oil components or non-water components, including surfactants, were detected, and it can be seen that the homogeneous mixture is a mixture of pure water and oil.

Although the present invention has been described in detail above with reference to the presented embodiments, those skilled in the art will be able to make various variations and modifications without departing from the technical spirit of the present invention by referring to the presented embodiments. . The present invention is not limited by such variations and modifications, but is limited by the claims appended below.

11: Insertion container 12: Drive unit
13: Pressurization module 14: Transport path
15: homogeneous module 16: guide conduit
17: heat exchanger 18a, 18b, 18c: ultrasonic unit

Claims (6)

A step in which two liquid components that do not mix with each other are stirred;
A step in which two liquid components are mixed and subjected to primary high-pressure homogenization;
A step of first ultrasonic treatment on the first homogenized component;
Adjusting the component ratio of the first homogeneous solution;
A second high-pressure homogenization step for the first homogenized solution with the adjusted component ratio;
A second step of ultrasonic treatment on the second homogenized solution; and
It includes the step of generating a homogeneous mixture that does not separate layers from each other,
The two liquid components become water and oil components, and the water and oil components are mixed at a weight ratio of 80:10 to 30 in the first high-pressure homogenization process, and adjusted to a weight ratio of 100:0.1 to 10 in the component ratio adjustment step. ,
A method for producing a homogeneous mixture, characterized in that a pressure of 10,000 to 30,000 psi is applied during the first and second high pressure homogenization processes. delete delete delete The method according to claim 1, wherein ultrasound waves of 20 kHz to 30 kHz are applied during the first or second ultrasonic treatment process. delete