KR101797810B1 - Method for manufacturing mixed liquid for colorimetric sensor and method for manufacturing colorimetric sensor using the same and colorimetric sensor thereof - Google Patents

Method for manufacturing mixed liquid for colorimetric sensor and method for manufacturing colorimetric sensor using the same and colorimetric sensor thereof Download PDF

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KR101797810B1
KR101797810B1 KR1020150082380A KR20150082380A KR101797810B1 KR 101797810 B1 KR101797810 B1 KR 101797810B1 KR 1020150082380 A KR1020150082380 A KR 1020150082380A KR 20150082380 A KR20150082380 A KR 20150082380A KR 101797810 B1 KR101797810 B1 KR 101797810B1
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color conversion
color
mixed solution
mixture
manufacturing
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KR20160145959A (en
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이정헌
조희훈
허준혁
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성균관대학교산학협력단
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B11/00Preparation of cellulose ethers
    • C08B11/02Alkyl or cycloalkyl ethers
    • C08B11/04Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
    • C08B11/08Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals with hydroxylated hydrocarbon radicals; Esters, ethers, or acetals thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F26/00Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
    • C08F26/06Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a heterocyclic ring containing nitrogen
    • C08F26/08N-Vinyl-pyrrolidine
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

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Abstract

A method for producing a color conversion mixed liquid is disclosed. A method for preparing a color conversion mixed solution includes: heating distilled water; Adding a dye to the distilled water to prepare a first mixed solution; Adding a water-soluble polymer and an amphipathic polymer to the first mixed solution to prepare a second mixed solution; Adding an aliphatic hydrocarbon derivative to the second mixed liquid to prepare a third mixed liquid; And preparing a color conversion mixture by adding an indicator having a complementary color to the color of the dye, the color of which changes depending on the presence or absence of analytes in the third mixture liquid.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method of manufacturing a color conversion liquid using a color conversion liquid mixture and a color conversion sensor using the color conversion liquid mixture,

The present invention relates to a color conversion sensor manufacturing method using a color conversion mixture prepared by the color conversion mixture manufacturing method and the color conversion mixture manufacturing method and a color conversion sensor manufactured by the color conversion sensor manufacturing method, A method of manufacturing a color conversion mixed solution capable of producing a solid state color conversion sensor by absorbing a color conversion mixed liquid in a liquid state into an absorption plate in a solid state and a color conversion method using the color conversion mixture prepared through the color conversion mixed solution production method A sensor manufacturing method, and a color conversion sensor manufactured through the color conversion sensor manufacturing method.

Korean Patent No. 10-1502277 relates to a color conversion sensor in a liquid state and relates to a color conversion sensor capable of easily determining whether an analyte exists in the naked eye. Such a color conversion sensor is a color conversion sensor that can be effectively used to detect the presence or absence of volatile organic compounds (VOCs), gas or liquid analytes.

However, it is difficult to handle such a color conversion sensor in a daily life or a work area because it is in a liquid state, and it is difficult to make the surface area that can contact the analyte larger than a solid state sensor. Therefore, There is a limit in that the adsorption and the reaction of the catalyst are slow. In addition, in the case of a conventional color sensor, an indicator and various dyes are mixed and used. However, when the dye is simply transferred onto a solid surface, problems that are not seen in a liquid state arise. Typical examples thereof include color separation ), Decrease in reactivity with analytes and decrease in color contrast effect. The present inventor intends to solve the above problems.

Korean Patent No. 10-1502277

Disclosure of Invention Technical Problem [8] The present invention provides a color conversion liquid preparation method capable of producing a solid state color conversion sensor by absorbing a color conversion liquid mixture in a liquid state into a solid absorption plate, A color conversion sensor manufacturing method using the manufactured color conversion mixed liquid, and a color conversion sensor manufactured through the color conversion sensor manufacturing method.

According to an aspect of the present invention, there is provided a method of preparing a color conversion mixed solution, comprising: heating distilled water; Adding a dye to the distilled water to prepare a first mixed solution; Adding a water-soluble polymer and an amphipathic polymer to the first mixed solution to prepare a second mixed solution; Adding an aliphatic hydrocarbon derivative to the second mixed liquid to prepare a third mixed liquid; And preparing a color conversion mixture by adding an indicator having a color and a complementary color to the color of the dye according to the presence or absence of analytes in the third mixture.

In one embodiment, the water-soluble polymer may be hydroxyethylcellulose.

In one embodiment, the amphipathic polymer may be polyvinylpyrrolidone (PVP).

In one embodiment, the aliphatic hydrocarbon derivative may be ethanol (C 2 H 5 OH).

The method for producing a color conversion mixed solution according to an embodiment of the present invention may further include a step of adding the aliphatic hydrocarbon derivative to the second mixed solution to prepare the third mixed solution so that the water soluble polymer is dissolved in the first mixed solution, And stirring the second mixed solution to which the second mixed solution is added for a predetermined period of time.

The method of producing a color conversion mixed solution according to an embodiment of the present invention may further include sonication of the color conversion mixed solution.

In one embodiment, the volume ratio of the distilled water to the aliphatic hydrocarbon derivative may be 1: 1, since the indicator is well soluble in the aliphatic hydrocarbon derivative and the dye is well soluble in water, It is for this reason.

A method of manufacturing a color conversion sensor using a color conversion mixed liquid according to an embodiment of the present invention includes the steps of: receiving a color conversion mixed solution prepared through the color conversion mixed solution production method in a container; Allowing the color conversion mixed liquid to be absorbed by the absorption plate by contacting one surface of the absorption plate capable of absorbing the color conversion mixture to the surface of the color conversion mixture; And drying the absorber absorbing the color conversion mixed solution.

In one embodiment, the step of drying the absorption plate absorbing the color conversion mixed solution may include: a first drying step of applying electromagnetic waves to the absorption plate absorbing the color conversion mixture to dry; And a second drying step of heating and drying the absorption plate absorbing the color conversion mixed solution.

A color conversion sensor according to an embodiment of the present invention can be manufactured through a color conversion sensor manufacturing method using a color conversion mixed liquid according to an embodiment of the present invention.

In the present invention as described above, even when the liquid-state color-converting mixed liquid is absorbed in the solid-state absorbing plate, color separation of the color-changing mixed liquid does not occur in the absorbing plate, and the color of the color- There is an effect that can be.

By using such a color conversion mixed liquid, it is possible to manufacture a solid state color conversion sensor in which uniform color is distributed throughout without color separation. In addition, by providing a solid state color conversion sensor, convenience of portability, storage, and use can be enhanced as compared with a liquid state color conversion sensor.

When the color conversion mixed liquid is absorbed on the plate-shaped absorption plate, the surface area that can be in contact with the analytes can be increased as compared with the color conversion liquid mixture in the liquid state, so that the reactivity can be improved.

1 is a flowchart illustrating a method of manufacturing a color conversion mixed solution according to an embodiment of the present invention.
2 is a flowchart illustrating a method of manufacturing a color conversion sensor using a color conversion mixed solution according to an embodiment of the present invention.
FIG. 3 is a photograph of a color conversion mixture prepared by the method of producing a color conversion mixed solution according to an embodiment of the present invention.
4A is a photograph showing Comparative Example 1.
4B is a photograph showing Comparative Example 2. Fig.
4C is a photograph showing the second embodiment.
5A is a photograph showing a state where analytes were reacted with Comparative Example 1. Fig.
5B is a photograph showing the state where analytes are reacted with Example 2. Fig.

While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail. It should be understood, however, that the invention is not intended to be limited to the particular embodiments, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

Hereinafter, a preferred embodiment of the present invention will be described in detail with reference to the accompanying drawings. Wherein like reference numerals refer to like elements throughout.

1 is a flowchart illustrating a method of manufacturing a color conversion mixed solution according to an embodiment of the present invention. FIG. 3 is a photograph of a color conversion mixture prepared by the method of producing a color conversion mixed solution according to an embodiment of the present invention.

Referring to FIGS. 1 and 3, a method of manufacturing a color conversion mixed solution according to an embodiment of the present invention includes the steps of heating distilled water (S1100), adding a dye to the distilled water to prepare a first mixed solution (S1200) A step (S1300) of adding a water-soluble polymer and an amphiphilic polymer to the first mixed liquid to prepare a second mixed liquid, a step (S1400) of preparing a third mixed liquid by adding an aliphatic hydrocarbon derivative to the second mixed liquid, (S1500) of changing the color depending on the presence or absence of analytes and adding an indicator having a complementary relation to the color of the dye to prepare a color conversion mixture.

To prepare a color conversion mixed solution, distilled water is heated (S1100). As an example, distilled water may be ultrapure water (di water). The heating of the distilled water is intended to accelerate the reaction rate of the water-soluble polymer added to the distilled water and the amphiphilic polymer to be mixed with the distilled water.

Next, a dye is added to the heated distilled water to prepare a first mixed solution (S1200). Dyes are also called pigments, and these dyes are unaffected by the presence of an analyte and have the inherent color of the material. In the present invention, a dye in which the dye has a complementary color relation with the color of the indicator is used. This is because if you mix two colors that are complementary to each other, you get an achromatic black color due to the complementary relationship. This is because the mixed indicator absorbs most of the light in the visible light region. According to one embodiment of the present invention, dyes having a complementary color to the color of the indicator can be made by combining three primary dyes of magenta, yellow and cyan, You can also make a complementary dye for the indicator.

Next, a water-soluble polymer and an amphipathic polymer are added to the first mixed solution to prepare a second mixed solution (S1300). For example, the water-soluble polymer added may be hydroxyethylcellulose, and a water-soluble polymer having a property of holding water well and a property of high viscosity may be used. Such hydroxyethylcellulose can prevent the color separation of the color conversion mixture when the color conversion mixture is absorbed by the absorption plate described below. As an example, the amphipathic polymer added may be polyvinylpyrrolidone (PVP). The amphiphilic polymer may be such that the hydrophilic dye added in step S 1200 of FIG. 1 and the hydrophobic indicator added in step S 1500 can be evenly mixed and the color conversion mixture can be uniformly absorbed on the absorption plate And can be used as a main material for preventing the color separation of the color conversion mixed solution.

Also, a water-soluble polymer must be added after adding a dye or an amphipathic polymer because the viscosity of the water-soluble polymer may not allow the dye or amphipathic polymer to mix well with the distilled water.

Next, an aliphatic hydrocarbon derivative is added to the second mixed solution to prepare a third mixed solution (S1400). For example, the aliphatic hydrocarbon derivative may be ethanol (C 2 H 5 OH). By adding ethanol, the color conversion mixture can be dried in a short period of time, and through this, it is possible to induce the color conversion mixture to be quickly absorbed and adhered to the absorption plate to be described below to prevent color separation of the color conversion mixture have.

Finally, a color conversion mixture is prepared by adding an indicator having a complementary color relation to the color of the dye, depending on the presence or absence of analytes in the third mixture liquid (S1500). For example, the indicator may be added to the third mixture and stirred to produce a color-changing mixture. The prepared color conversion mixture may be black, but the color conversion mixture prepared according to the change of the dye and indicator may be an achromatic color other than black. For example, it may be gray.

In addition, the method for producing a color conversion mixed solution according to an embodiment of the present invention may further include a step of preparing a third mixed solution by adding an aliphatic hydrocarbon derivative to the second mixed solution (S1400). The water soluble polymer may be dissolved in the first mixed solution, (S1350) stirring the second mixed solution to which the polymer is added for a predetermined period of time.

In addition, the method of producing a color conversion mixed solution according to an embodiment of the present invention may further include a step (S1600) of sonicating the color conversion mixed solution. This is to remove all bubbles present in the color conversion mixture by stirring performed in steps S1350 and S1500.

2 is a flowchart illustrating a method of manufacturing a color conversion sensor using a color conversion mixed solution according to an embodiment of the present invention.

Referring to FIG. 2, a method of manufacturing a color conversion sensor using a color conversion mixed liquid according to an exemplary embodiment of the present invention includes the steps of accommodating the color conversion mixed liquid described with reference to FIG. 1 in a container (S2100) (S2200) of causing the color conversion mixed liquid to be absorbed by the absorption plate by contacting one surface of the absorption plate and the surface of the color conversion mixture to each other, and drying the absorption plate (S2300) absorbing the color conversion mixture Step < / RTI >

In order to manufacture the color conversion sensor, the color conversion mixed solution is accommodated in the container (S2100).

Next, one surface of the absorption plate capable of absorbing the color conversion mixed liquid and the surface of the color conversion mixture liquid are brought into contact with each other to allow the color conversion mixture to be absorbed by the absorption plate (S2200). For example, the absorption plate capable of absorbing the color conversion mixed solution may be a plate-like low dust-proof fabric, a fabric made of a nonwoven fabric or a polymer material, but is not limited thereto.

For example, when a fabric or the like is used as an absorbing plate, the color conversion mixed liquid may be absorbed into a fabric having a large surface area, so that the surface area by which the color conversion mixed liquid can be contacted with the analytes may be increased.

For example, one surface of the absorption plate and the surface of the color conversion mixture should be in contact with each other so that the color conversion mixture can be absorbed into the absorption plate. This is because when the absorption plate is immersed in the color conversion mixture, the surface area of the absorption plate may be reduced, which may degrade the reactivity with the analytes.

Finally, the absorbing plate which absorbs the color conversion mixed liquid is dried (S2300). For example, the electromagnetic wave is first applied to the absorption plate absorbing the color conversion mixed solution (S2320), and the absorption plate absorbing the color conversion mixture is heated and dried (S2340). The first drying can be performed by exposing the absorption plate to electromagnetic waves having microwaves through the microwave oven, and the absorption plate can be rapidly dried by electromagnetic waves. This rapid drying can prevent color separation from occurring in the color conversion mixed solution absorbed in the absorption plate. Next, the color conversion sensor according to the embodiment of the present invention can be manufactured by completely drying the absorption plate through the second drying. Through this process, it is possible to manufacture a solid state color conversion sensor having the same color as that of the color conversion mixture and without color separation of the color conversion mixture.

Example  One: Color conversion  Mixed liquid manufacturing

200 ml of di-water was placed in a 500 ml media bottle and heated to about 70 캜. Then, 75.03 mg of tartrazine and 96.39 mg of direct red 80 were added to the distilled water heated and stirred. Next, 2 g of hydroxyethylcellulose and 1 g of polyvinylpyrrolidone (PVP) were further added and stirred for about 20 minutes. Next, 200 ml of ethanol (EtOH) of 99.9% purity anhydrous ethanol was added. Next, 75.82 mg of Bromocresol green sodium salt (BCG SS) was added to ethanol (EtOH) on distilled water, and the medium bottle was stirred while being sealed to prepare a color conversion mixture (Example 1) .

Example  2: Color conversion  Sensor Manufacturing

The color conversion mixed solution (Example 1) was placed in a container, and the upper surface of the low-emission nonwoven fabric was brought into contact with the surface of the color conversion mixed solution so that the color conversion mixed solution was absorbed into the nonwoven fabric. The nonwoven fabric absorbing the color conversion mixed solution was placed in an empty container, charged into a microwave oven, and rapidly dried by applying electromagnetic waves for about 1 minute and 30 seconds. Finally, the rapidly dried nonwoven fabric was put into an oven and dried for about 5 minutes to prepare a color conversion sensor (Example 2).

Comparative Example  One

Comparative Example 1 was prepared in the same manner as in Example 2 except that a color conversion mixture solution containing no hydroxyethylcellulose was used.

Comparative Example  2

Comparative Example 2 was prepared in the same manner as in Example 2 except that a color conversion mixture solution containing no polyvinylpyrrolidone (PVP) was used.

4A is a photograph showing Comparative Example 1, FIG. 4B is a photograph showing Comparative Example 2, and FIG. 4C is a photograph showing Example 2.

Referring to FIGS. 4A and 4C, in the case of Comparative Example 1, the black color is not uniformly distributed throughout, and the color separation can be confirmed. On the other hand, in Example 2, the black color is uniformly distributed Can be confirmed. It can be seen that the color conversion mixture solution including hydroxyethyl cellulose is used to reproduce the color of the color conversion mixture even without color separation.

Referring to FIGS. 4B and 4C, it can be seen that in the case of the comparative example 2, the color is changed to the red color rather than the black color. In the case of the embodiment 2, the black color is uniformly distributed. Through this, it can be confirmed that the color of the color conversion mixture is reproduced in the absorption plate only if a color conversion mixture containing polyvinylpyrrolidone (PVP) is used.

FIG. 5A is a photograph showing the state in which analytes are reacted with Comparative Example 1, and FIG. 5B is a photograph showing a state in which analytes are reacted with Example 2. FIG.

Referring to FIGS. 5A and 5B, it can be seen that, in the case of Comparative Example 1, even when reacted with gas or liquid analytes, the color conversion is changed from an achromatic color to an achromatic color, Slowly. On the contrary, in Example 2, achromatic color changed into a chromatic color (red color). Therefore, it was recognized that the color easily changed at a glance, and the color conversion speed was much faster than that of Comparative Example 1. As a result, the color conversion sensor according to the embodiment of the present invention has the effect of easily confirming visually whether the analyte exists or not.

While the invention has been shown and described with reference to certain preferred embodiments thereof, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims. Accordingly, the true scope of the present invention should be determined by the following claims.

Claims (10)

Receiving a color conversion mixed solution in a vessel;
Allowing the color conversion mixed liquid to be absorbed by the absorption plate by contacting one surface of the absorption plate capable of absorbing the color conversion mixture to the surface of the color conversion mixture; And
And drying the absorbing plate that has absorbed the color conversion mixed liquid,
The method for producing the color conversion mixed solution may comprise:
Heating the distilled water;
Adding a dye to the distilled water to prepare a first mixed solution;
Preparing a second mixed solution by adding a water-soluble polymer and an amphipathic polymer to the first mixed solution to prepare a second mixed solution, wherein the second mixed solution is prepared by first adding an amphipathic polymer and then adding a water-soluble polymer;
Stirring the second mixed solution so that the water-soluble polymer is dissolved in the first mixed solution;
Adding an aliphatic hydrocarbon derivative to the second mixed liquid to prepare a third mixed liquid; And
Preparing a color conversion mixed solution by adding an indicator having a color complementary to the color of the dye to the color of the third mixed liquid depending on the presence or absence of analytes,
Wherein the step of drying the absorption plate absorbing the color conversion mixed liquid comprises:
A first drying step of applying electromagnetic waves to the absorption plate absorbing the color conversion mixed solution to dry the absorption plate; And
And a second drying step of heating and drying the absorption plate absorbing the color conversion mixed liquid,
By mixing the dye and the indicator in the complementary color relationship, the color conversion mixture can change color from achromatic color to chromatic color depending on the presence or absence of the analyte,
(Method for manufacturing color conversion sensor using color conversion mixture).
The method according to claim 1,
Wherein the water-soluble polymer is hydroxyethylcellulose,
(Method for manufacturing color conversion sensor using color conversion mixture).
The method according to claim 1,
Wherein the amphipathic polymer is polyvinylpyrrolidone (PVP)
(Method for manufacturing color conversion sensor using color conversion mixture).
The method according to claim 1,
Wherein the aliphatic hydrocarbon derivative is ethanol (C 2 H 5 OH)
(Method for manufacturing color conversion sensor using color conversion mixture).
delete The method according to claim 1,
Further comprising the step of subjecting the color conversion mixed solution to sonication,
(Method for manufacturing color conversion sensor using color conversion mixture).
The method according to claim 1,
Wherein the volume ratio of the distilled water and the aliphatic hydrocarbon derivative is 1:
(Method for manufacturing color conversion sensor using color conversion mixture).
delete delete A color conversion sensor, manufactured by the method of any one of claims 1 to 4, 6 and 7.
KR1020150082380A 2015-06-11 2015-06-11 Method for manufacturing mixed liquid for colorimetric sensor and method for manufacturing colorimetric sensor using the same and colorimetric sensor thereof KR101797810B1 (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080295581A1 (en) * 2007-05-31 2008-12-04 General Electric Company Method for the determination of aqueous polymer concentration in water systems
KR101502277B1 (en) * 2014-05-15 2015-03-12 성균관대학교산학협력단 Colorimetric sensor detecting analytes with visual examination

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080295581A1 (en) * 2007-05-31 2008-12-04 General Electric Company Method for the determination of aqueous polymer concentration in water systems
KR101502277B1 (en) * 2014-05-15 2015-03-12 성균관대학교산학협력단 Colorimetric sensor detecting analytes with visual examination

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Acta Chimica Slovaca, Vol.6, ,pp. 100-105, 2013*

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