KR20100087526A - Method for preparing cotton fabric using nano silica particle and water-repellent agent - Google Patents

Method for preparing cotton fabric using nano silica particle and water-repellent agent Download PDF

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Publication number
KR20100087526A
KR20100087526A KR1020090006581A KR20090006581A KR20100087526A KR 20100087526 A KR20100087526 A KR 20100087526A KR 1020090006581 A KR1020090006581 A KR 1020090006581A KR 20090006581 A KR20090006581 A KR 20090006581A KR 20100087526 A KR20100087526 A KR 20100087526A
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South Korea
Prior art keywords
water
water repellent
cotton fabric
fluorine
repellent
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KR1020090006581A
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Korean (ko)
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민병길
배근열
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금오공과대학교 산학협력단
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Priority to KR1020090006581A priority Critical patent/KR20100087526A/en
Publication of KR20100087526A publication Critical patent/KR20100087526A/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D06M23/10—Processes in which the treating agent is dissolved or dispersed in organic solvents; Processes for the recovery of organic solvents thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
    • D06M2200/12—Hydrophobic properties
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/01—Natural vegetable fibres
    • D10B2201/02—Cotton
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/02—Moisture-responsive characteristics
    • D10B2401/021—Moisture-responsive characteristics hydrophobic

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Textile Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The present invention relates to the water-repellent processing of fabrics using nano-silica particles and fluorine-based water repellents already commercially available. More specifically, the nano-silica particles are adhered to the surface of the fiber to form spherical protrusions and the surface is coated with a fluorine-based water repellent agent. The present invention relates to a method of imparting water repellency to cotton fabrics.

According to the present invention, by using a commercially available fluorine-based water repellent, it is possible to improve the cost efficiency due to cost reduction and process shortening than the water-repellent imparting method using fluorinated silane or alkylated silane that has been studied a lot. In addition, by reducing the amount of fluorine-based polymers, fluorine-based water repellents, which are being tightened around the world, potential risks to the human body can be reduced.

Description

Method for preparing cotton fabric using nano silica particles and water-repellent agent

The Lotus-effect, already widely applied in everyday life such as automobile glass, leisure textiles, and pipes, refers to the self-cleaning observed in the leaves of lotus leaves or insects. It means to keep the spherical shape and to roll off to remove contaminants on the surface. This is due to the micro- and nano-sized projections of the substrate surface and the hydrophobicity of the substrate surface, including the projections. It is common to introduce nano-sized inorganic particles (TiO 2 , SiO 2 , ZnO) prepared by the sol-gel method onto the substrate surface in order to give the surface roughness, that is, the protrusion structure.

Many existing studies have used fluorinated silanes, alkylated silanes to hydrophobically modify the substrate surface including protrusions. Recently, the necessity of a water repellent fabric is increasing due to the expansion of leisure, outdoor and sports apparel markets, and research on the implementation of water repellency using nano particles and nano structures is actively being conducted. Cotton is a natural fiber with many advantages such as softness, comfort, warmth, biodegradability and low cost, but it has a lot of -OH groups on the surface, so it is less resistant to contaminants.

An object of the present invention is to provide a relatively inexpensive and easy-to-apply alternative material that can replace fluorinated silanes, alkylated silanes that are expensive and have difficulty in providing hydrophobicity of the fiber surface using nanotechnology. It is to provide a simple manufacturing process.

In order to solve the above problems, according to a preferred embodiment of the present invention, a cotton woven fabric characterized in that the silica sol is applied to the cotton fabric and heated to fix the particles on the surface of the cotton fabric, and then the cotton fabric having the silica particles fixed thereon is treated with a water repellent agent. Provides a water repellent method.

According to another suitable embodiment of the present invention, the particle size of the silica sol is preferably 50 to 1000 nm.

According to another suitable embodiment of the present invention, the average particle size of the silica sol is more preferably 378 ± 17 nm.

According to another suitable embodiment of the present invention, the water repellent is preferably a fluorine-based water repellent.

According to another suitable embodiment of the present invention, the silica sol is a mixture of 1) tetraethyl orthosilicate (TEOS) and ethanol (Ethanol) and stirred and 2) ammonium oxide (NH 4 OH) and water (H It is a spherical silica sol obtained by mixing and stirring 20).

According to another suitable embodiment of the present invention, the concentration of the water repellent is preferably 0.1% by weight.

As described above, the water repellent process using the fluorine-based water repellent agent commercialized with the nano-silica particles of the present invention not only solves problems such as difficulty in application due to expensive and complicated processes, but also compared to the water repellent process using only the fluorine-based water repellent agent. A much smaller amount can provide a water repellent fabric with good water repellency.

In addition, the water-repellent processing of the cotton fabric using the water repellent agent compatible with the nano-silica particles of the present invention exhibits excellent water repellency as a lean solution of the commercially available water repellent agent, resulting in high production cost, which is a problem when fluorinated silane and alkylated silane are used. In addition to solving problems such as difficulties in the process, the use of fluorine-based water repellents is greatly reduced, which greatly reduces the potential risk of fluorine-based compounds.

By applying fluorine-based water repellent, which is already commercially available, to the fiber surface containing protrusions, it provides a relatively inexpensive, easy-to-apply substitute material and a simple manufacturing process to replace the existing fluorinated silane and alkylated silanes. .

Hereinafter, the present invention will be described in detail.

The present invention relates to a water-repellent process characterized by applying a silica sol prepared by the sol-gel method to a cotton fabric and applying heat to fix the particles on the surface of the fiber, then applying a fluorine-based water repellent to the treated fabric, drying and fixing.

The particle size of the silica sol of the present invention is preferably 50 to 1000 nm. If the particle size of the silica sol is less than 50nm, when the sol-gel method is used, it takes much time for particle generation, and thus the industrial economics are inferior.

The present invention used nano-silica particles prepared by the sol-gel method to give a projection structure, it is also possible to introduce the projection structure on the surface using other inorganic particles (TiO 2 , SiO 2 , ZnO).

It is preferable that the water repellent used in this invention is a fluorine-type water repellent. Examples of the water repellent are as follows, but the water repellent of the present invention is not limited to the following examples.

Nika korea KF GUARD 2000)

DAIKIN Dongin TEXCHEM UNIDYNE TG-580, UNIDYNE TG-581, UNIDYNE TG-658, UNIDYNE TG-995, UNIDYNE TG-996)

Hereinafter, the present invention will be described in detail with reference to Examples, but the present invention is not limited by Examples.

≪ Example 1 >

Water repellent was attempted on the cotton fabric using a fluorine-based water repellent diluent (0.1 wt%) commercialized with nano silica particles having an average diameter of 378 ± 17 nm, and the characteristics of the water-repellent cotton fabric were evaluated.

Preparation of 1-1 Nano Silica Sol

Solution No. 1: TEOS 0.39 mol and Ethanol 2.35 mol were mixed and stirred at 400 rpm at 30 ° C for 1 hour.

No. 2 solution: 0.18 mol of NH4OH, 2.94 mol of H20, and 2.35 mol of Ethanol were mixed and stirred at 400rpm at 30 ° C for 1 hour.

By mixing solution 1 and solution 2 and stirring at 400 rpm at 30 ° C. for 24 hours, a sol having spherical nano silica particles having an average diameter of 378 ± 17 nm can be prepared.

Silica Particles Fixing and Water Repellent Process of 1-2 Cotton Fibers

(1) The fabric used was refined and bleached plain weave cotton fabric (60 males).

(2) The cotton fiber was immersed in the prepared silica sol described in Example 1-1 and fixed at 70% padding ratio (WPU) using a laboratory mangle (DL-2005H, Daelim Starlet, Korea). Thereafter, the resultant was dried at 80 degrees for 3 minutes with a laboratory tenter and then cured at 160 degrees for 3 minutes. A laboratory laundering machine (DL-2002, Daelim Engineering, Korea) was used to remove particles that did not adhere to the fiber surface by the ISO 105-A01 method. The treated cotton was immersed in a diluent (0.1%) of a commercial water repellent (KF255, Nicca Korea) and dried again at 180 degrees for 3 minutes.

1-3 Changes in Surface Structure and Surface Chemical Composition of Cotton Fibers Treated

(1) Referring to FIG. 1, it is easy to distinguish between an untreated surface and a surface on which silica particles are fixed. As a result of analyzing the chemical composition of the surface to determine the identity of the hemispherical protrusions (Fig. 2), it was confirmed that the nano-silica particles (SiO 2 ).

(2) When the diluent (0.1%) of the water repellent commercialized on the cotton fabric to which the nano-silica particles are fixed, it was confirmed that the surface structure was changed as shown in FIG. In addition, as a result of analyzing the chemical composition of the surface (Fig. 4), it was confirmed that the fluorine-based water repellent was coated on the surface, and compared with the surface structure before the water-repellent imparting process (Fig. 2), the size of the protrusions was noticeably increased. It was confirmed that the water repellent was coated not only on the surface of the cotton fiber but also on the surface of the nano silica particles fixed to the fiber.

1-4 Water repellency evaluation of cotton fabric after water repellent

After dropping 3.3 ml of water droplets on the cotton fabric subjected to the water repellent provision process, the contact angle and the measured photograph after 30 seconds are shown in FIG. 5. The synergy of the hydrophobic surface imparted by the projections and fluorine-based water repellents generated by the nano-silica particles prevents water droplets from penetrating into the cotton fabric and remains stationary on the surface in a nearly perfect sphere shape.

<Example 2>

Water repellent was applied to the cotton fabric using a fluorine-based water repellent diluent (0.1%) compatible with nano silica particles having an average diameter of 142.5 ± 9.6 nm, and the characteristics of the water-repellent cotton fabric were evaluated.

Preparation of 2-1 Nano Silica Sol

Particles of different sizes could be produced by reducing the ammonia water as a catalyst in Example 1-1.

Solution No. 1: TEOS 0.39 mol and Ethanol 2.35 mol were mixed and stirred at 400 rpm at 30 ° C for 1 hour.

Solution No. 2: NH4OH 0.05 mol, H20 2.94 mol and Ethanol 2.35 mol were mixed and stirred at 400 rpm at 30 degrees for 1 hour.

By mixing solution 1 and solution 2 and stirring at 400 rpm at 30 ° C. for 24 hours, a sol having spherical nano silica particles having an average diameter of 142.5 ± 9.6 nm can be prepared.

2-2 Silica Particles Bonding and Water Repellent Process

It is the same as Example 1-2.

2-3 Changes in Surface Structure and Surface Chemical Composition of Cotton Fibers Treated

(1) It was confirmed that the same as the SiO 2 particles in Example 1-3 and through Figure 6 it was confirmed that the size of the particles fixed on the surface is significantly reduced compared to Example 1.

(2) As a result of analyzing the chemical composition of the surface treated with the diluent (0.1%) of the water repellent commercialized on the cotton fabric to which the nano-silica particles of Example 2-1 were fixed (Fig. 7), the fluorine-based water repellent was coated on the surface. I could confirm that

2-4 Water repellency evaluation of cotton fabric after water repellent

After dropping 3.3 ml of water droplets on the cotton fabric subjected to the water repellent provision process, the contact angle and the measured photograph after 30 seconds are shown in FIG. 8. This resulted in the reduction of the size of the particles fixed on the fiber surface, the degree of surface roughness (roughness) due to the water repellency is reduced to give a lower synergistic effect than Example 1 showed a lower contact angle than that of Example 1 .

<Example 3>

Using a fluorine-based water repellent (0.5%) commercialized with the same size nano-silica particles used in Example 1 was tried to water-repellent cotton fabric and evaluated the characteristics of the water-repellent cotton fabric.

Preparation of 3-1 Nano Silica Sol

It is the same as Example 1-1.

3-2 Silica Particles Fixing and Water Repellent Process of Cotton Fiber

(1) The fabric used was refined and bleached plain weave cotton fabric (60 males).

(2) The cotton fiber was immersed in the silica sol prepared in Example 1-1, and the padding ratio (WPU) was fixed at 70% using a laboratory mangle (DL-2005H, Daelim Starlet, Korea). Thereafter, the resultant was dried at 80 degrees for 3 minutes with a laboratory tenter and then cured at 160 degrees for 3 minutes. A laboratory laundering machine (DL-2002, Daelim Engineering, Korea) was used to remove particles that did not adhere to the fiber surface by the ISO 105-A01 method. The treated cotton was immersed in a diluted solution (0.5%) of a commercial water repellent (KF255, Nicca Korea) and dried again at 180 degrees for 3 minutes.

3-3 Changes in Surface Structure and Surface Chemical Composition of Treated Cotton Fibers

(1) The structure in which the silica particles were fixed on the surface fiber surface and the chemical component (SiO 2 ) of the projections were the same as in Example 1-3.

(2) When the diluent (0.5%) of the water repellent commercialized on the cotton fabric to which the nano-silica particles are fixed, it was confirmed that the surface structure was changed as shown in FIG. In addition, as a result of analyzing the chemical composition of the surface (Fig. 10), it was confirmed that the fluorine-based water repellent is coated on the surface and compared to Figure 4 treated in the 1-3 compared to the commercialized water repellent treated with the strength of fluorine (F) It was found to be strong in proportion to the concentration of. Compared with the surface structure before the water repellent imparting process (Fig. 2), the size of the protrusions was remarkably increased, indicating that the water repellent was coated not only on the surface of the cotton fiber but also on the surface of the nano silica particles adhered to the fiber.

3-4 Water repellency evaluation of cotton fabric after water repellent

After dropping 3.3 ml of water droplets on the cotton fabric subjected to the water repellent provision process, the contact angle and the measured photograph after 30 seconds are shown in FIG. 11. This can be explained through FIGS. 12A and 12B. As the concentration of commercialized water repellent increases, the thickness of the fluorinated polymer coated on the surface increases, thereby filling the valleys between the projections and the projections with the fluorine-based polymer, thereby reducing the surface roughness and thereby the projections due to the water repellency. It was confirmed that the improvement of the contact angle was inferior to that of Example 1 because of the disappearance and only the fluorine-based water repellent exhibited water repellency.

Comparative Example 1

The characteristics of the untreated cotton fabric were evaluated. (FIGS. 13 and 14).

Comparative Example 2

Water repellency was evaluated by treating only the diluent (0.1%) of the water repellent commercialized on the untreated cotton fabric. (FIG. 15, FIG. 16).

Comparative Example 3

Water repellency was evaluated by treating only the diluent (0.5%) of the water repellent commercialized on the untreated cotton fabric. (FIGS. 17 and 18).

Comparative Example 4

Only the nano silica particles were fixed to the untreated cotton fabric without the water repellent treatment to evaluate the water repellency (FIG. 19).

1 is a SEM photograph of the surface to which the nano silica particles having a diameter of 378 ± 17 nm is fixed.

2 is a chemical composition analysis (XPS) of a cotton fabric surface to which nano silica particles having a diameter of 378 ± 17 nm are fixed.

FIG. 3 is a SEM photograph of a cotton fabric after water repellent processing using a fluorine-based water repellent diluent (0.1%) compatible with nano silica particles having a diameter of 378 ± 17 nm.

Figure 4 is a photograph of the analysis of the chemical composition (XPS) of the surface of the cotton fabric after water repellent using a fluorine-based water-repellent diluent (0.1%) commercialized with nano silica particles having a diameter of 378 ± 17 nm.

5 is a measurement of the contact angle of the cotton fabric after water-repellent process using a fluorine-based water repellent diluent (0.1%) compatible with nano silica particles having a diameter of 378 ± 17 nm.

6 is a SEM photograph of the surface to which the nano-silica particles having a diameter of 142.5 ± 9.6 nm is fixed.

7 is a chemical analysis (XPS) of the surface of the cotton fabric to which the nano silica particles having a diameter of 142.5 ± 9.6 nm is fixed.

8 is a measurement of the contact angle of the cotton fabric after water-repellent process using a fluorine-based water repellent diluent (0.1%) compatible with nano silica particles having a diameter of 142.5 ± 9.6 nm.

FIG. 9 is a SEM photograph of a cotton fabric after water repellent treatment using a fluorine-based water repellent diluent (0.5%) compatible with nano silica particles having a diameter of 378 ± 17 nm.

10 is a chemical analysis (XPS) of the surface of the surface of the cotton fabric after water repellent using a fluorine-based water repellent diluent (0.5%) and commercialized nano silica particles having a diameter of 378 ± 17 nm.

11 is a measurement of the contact angle of the cotton fabric after water repellent process using a fluorine-based water repellent diluent (0.5%) compatible with nano silica particles having a diameter of 378 ± 17 nm.

FIG. 12A is a surface structure (AFM) when treated with a fluorine-based water repellent diluent (0.1%) commercially applied to a cotton fabric having nano-silica particles having a diameter of 378 ± 17 nm.

12B is a surface structure (AFM) when treated with a commercially available fluorine-based water repellent diluent (0.5%) on a cotton fabric having nano silica particles having a diameter of 378 ± 17 nm.

13 is an SEM photograph of an untreated cotton fabric.

Figure 14 measures the contact angle of the untreated cotton fabric.

FIG. 15 is a SEM photograph of a cotton fabric when treated with a fluorine-based water repellent diluent (0.1%) commercially applied to the untreated cotton fabric.

16 is a measurement of the contact angle of the cotton fabric when treated with a fluorine-based water repellent diluent (0.1%) commercially available to the untreated cotton fabric.

FIG. 17 is a SEM photograph of a cotton fabric when treated with a fluorine-based water repellent diluent (0.5%) commercially applied to the untreated cotton fabric.

18 is a measurement of the contact angle of the cotton fabric when treated with a fluorine-based water repellent diluent (0.5%) commercially available to the untreated cotton fabric.

19 is a measurement of the contact angle of the cotton fabric in which the nano-silica particles having a diameter of 378 ± 17 nm fixed to the untreated cotton fabric.

Claims (6)

A method of water repelling cotton fabrics, comprising applying a silica sol to a cotton fabric, applying heat to fix the particles to the surface of the cotton fabric, and then treating the cotton fabric to which the silica particles are fixed with a water repellent. The method of claim 1, An average particle size of the silica sol is 50 to 1000nm, characterized in that the water repellent of the cotton fabric. The method of claim 1, An average particle size of the silica sol is 378 ± 17nm, characterized in that the water repellent of the cotton fabric. The method of claim 1, And said water repellent is a fluorine-based water repellent. The method of claim 1, The silica sol is a mixture of 1) tetraethyl orthosilicate (TEOS) and ethanol (Ethanol) and agitation and 2) a mixture of ammonium hydroxide (NH 4 OH) and water (H 2 0) to stir And a spherical silica sol obtained by stirring. The method of claim 4, wherein The water-repellent method of the cotton fabric, characterized in that the concentration of the water repellent is 0.1% by weight.
KR1020090006581A 2009-01-28 2009-01-28 Method for preparing cotton fabric using nano silica particle and water-repellent agent KR20100087526A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101251814B1 (en) * 2011-07-28 2013-04-12 다이텍연구원 Process Of Producing Organic―Inorganic Hybrid Finishing Agent For Fabrics Having High Durability
WO2013058843A3 (en) * 2011-07-05 2013-08-22 Luna Innovations Incorporated Fluid-resistant textile fabrics and methods

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013058843A3 (en) * 2011-07-05 2013-08-22 Luna Innovations Incorporated Fluid-resistant textile fabrics and methods
US9708755B2 (en) 2011-07-05 2017-07-18 Luna Innovations Incorporated Fluid-resistant textile fabrics and methods
KR101251814B1 (en) * 2011-07-28 2013-04-12 다이텍연구원 Process Of Producing Organic―Inorganic Hybrid Finishing Agent For Fabrics Having High Durability

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