KR102026086B1 - Composition for preparing febrific synthetic cotton and preparation of the febrific synthetic cotton by using it - Google Patents

Abstract

The present invention relates to a composition for manufacturing pyrogenic synthetic cotton and a method for manufacturing pyrogenic synthetic cotton. More particularly, the present invention relates to a composition for manufacturing pyrogenic synthetic cotton, which comprises 20-30 wt% of a porous binding material composed of silicon dioxide and zeolite; 10-20 wt% of graphene suspension; 50-65 wt% of a fiber spinning polyester resin; and 2-5 wt% of an auxiliary additive, and to a method for manufacturing pyrogenic synthetic cotton having an effect of generating low temperature heat by itself using the composition.

Description

Composition for preparing pyrogenic synthetic cotton and method for preparing pyrogenic synthetic cotton using the same {composition for preparing febrific synthetic cotton and preparation of the febrific synthetic cotton by using it}

The present invention relates to a composition for producing a pyrogenic synthetic cotton and a method for producing a pyrogenic synthetic cotton using the same. More specifically, 20 to 30% by weight of a porous binder composed of silicon dioxide and zeolite, and a graphene suspension of 10 to A composition for preparing a pyrogenic synthetic cotton comprising 20 wt%, 50 to 65 wt% of a fiber spinning polyester resin, and 2 to 5 wt% of an auxiliary additive, and an exotherm having an effect of generating lukewarm heat by using the composition It relates to a method for producing a synthetic synthetic cotton.

Cotton is a fibrous material extracted from cotton, and is widely used as a cotton wool for textiles, textiles, duvets, clothes, quilting, hygiene or medical. And synthetic cotton (synthetic cotton) is used as a substitute for the natural cotton as a cotton prepared using a variety of synthetic fibers, such as polyester fibers.

Conventionally, techniques for adding various functions to synthetic cotton have been introduced. For example, Japanese Patent Application Laid-open No. 10-1999-70911 (September 15, 1999) discloses a polyester chip obtained by mixing an illite processed with a fine powder in a polyester chip at a ratio of 2 to 5% by weight and stirring it with heat. A method for producing a functional illite synthetic cotton having excellent antibacterial and noxious gas adsorption properties has been introduced by obtaining a master batch with an aluminate powder and melt spinning the master batch with a polyester chip for fiber production.

In Patent Publication No. 10-2007-47258 (May 04, 2007), pegmatite powder, chitosan powder, pine calcite powder, and cotton regenerated chip synthetic resin are mixed together to form a powdered resin, and 30% by weight of the powdered resin And a method for producing a functional synthetic cotton that emits far infrared rays by mixing and spinning 70% by weight of a separate cotton finished chip synthetic resin.

Lastly, Korean Patent Publication No. 10-2015-57818 (May 28, 2015) includes 45-55% by weight of natural ginseng fiber processed, 40-45% by weight of multipurpose functional cotton, and low-melting thermoplastic synthetic resin fiber of wave shape. By uniformly mixing and burning 5 to 10% by weight, there is no loosening or slipping between fibers, so that the original shape can be maintained continuously and dimensional stability is introduced.

On the other hand, graphene is a two-dimensional plate-shaped material in which carbon atoms are arranged in a hexagonal shape, and not only has excellent mechanical properties such as elasticity and strength, but also is chemically safe and has thermal conductivity, electrical conductivity, and antibacterial properties. This is one of the very good new materials. Therefore, studies are being actively conducted to apply the excellent physical properties of graphene to fibers.

For example, Patent Registration No. 10-1238667 (February 25, 2013) incorporates liquid graphene as a filler in carbon fiber as a heating source to improve the electrical conductivity of carbon fiber and at the same time improve durability and heat generation. The method for producing a planar heating element using the graphene carbon fiber heating paper is introduced.

In addition, Patent Publication No. 10-2016-132551 (November 21, 2016), a graphene sheet is laminated on a woven fabric or a non-woven fabric structure, graphene gel comprising a porous pore between the graphene sheet This formed graphene fiber composite is introduced. The graphene fiber composite can be used as a heat generating material because it generates heat when a current flows, it is possible to quickly control the amount of heat generated quickly.

Finally, Patent Registration No. 10-1782725 (September 21, 2017), by adjusting the concentration and spinning rate of the aqueous solution of graphene oxide to prepare a graphene fiber of porous structure that can control the elongation rate, high mechanical strength It relates to a graphene fiber having a good elongation at the same time and a method for producing the same.

Patent Publication No. 10-1999-70911 (September 15, 1999) Patent Publication No. 10-2007-47258 (May 04, 2007) Patent Publication No. 10-2015-57818 (May 28, 2015) Patent Registration No. 10-1238667 (February 25, 2013) Patent Publication No. 10-2016-132551 (November 21, 2016) Patent Registration No. 10-1782725 (September 21, 2017)

An object of the present invention is a new material containing graphene has the effect of generating heat of itself by itself, it emits far-infrared rays to promote blood circulation and metabolism of the human body, and furthermore, pyrogenic with antibacterial and odor removal effect It is to provide a composition for producing synthetic cotton and a method for producing a pyrogenic synthetic cotton using the same.

Composition for producing a pyrogenic synthetic cotton wool according to the present invention, 20 to 30% by weight of a porous binder composed of silicon dioxide and zeolite; 10-20 wt% of graphene suspension; 50 to 65% by weight of a fiber spinning polyester resin; 2 to 5 weight percent auxiliary additives; Characterized in that consisting of.

The graphene suspension is characterized by consisting of 20 to 35% by weight of graphene powder having a particle diameter of 220 to 350 nm and 65 to 80% by weight of purified water.

The auxiliary additive includes 45% by weight of acrylic stearic acid, 9% by weight of fatty acid ester calcium, 13.5% by weight of water-soluble calcium solution, 18.9% by weight of amine, 4.6% by weight of hydroxymagnesium silicate, and 9% by weight of fatty acid amine polyoxyester. It is characterized by consisting of%.

Method for producing a pyrogenic synthetic cotton wool according to the invention, A) preparing a composition for producing a pyrogenic synthetic cotton of any one of claims 1 to 5; B) The composition was put into a hermetic mixer, and the internal pressure was pressurized to 100 MPa at a rate of 5 MPa / min, and extruded while decompressing at a rate of 2 MPa / min until the pressure again reached atmospheric pressure. Preparing a mixed polyester chip; C) heating the polyester chip at a temperature of 500 to 600 ° C. for 20 to 30 minutes to obtain a melt; D) The melt is put in a sealed container, and the internal pressure is increased to 400 to 450 MPa at a rate of 5 to 8 MPa / min and maintained for 4 to 5 hours, and then at a rate of 2 to 4 MPa / min. Depressurizing to atmospheric pressure; E) spinning the melt passed through step D) at a speed of 1,220 ~ 1,310 m / min to obtain a fiber, and burning the fiber To obtain a synthetic cotton; Characterized in that it is prepared to include.

Pyrogenic synthetic cotton prepared according to the present invention can be usefully used as a substitute for natural cotton or synthetic cotton, such as quilting cotton, cloth, quilting cotton, etc., has the following effects.

First, it emits far-infrared rays, promotes blood circulation and metabolism in the human body, and further helps to generate and activate cellular tissues.

Second, due to the thermal conductivity of graphene more than twice as high as diamond, the body temperature is continuously maintained, and furthermore, it is effective in generating lukewarm heat by itself.

Third, due to the antimicrobial properties of graphene, there is an effect of blocking the growth of bacteria on their own, and removes the odor even if the antibacterial treatment is not otherwise.

1 is a real photograph of a pyrogenic synthetic cotton prepared according to the present invention,
Figure 2 is a photograph of the infrared radiation energy for the pyrogenic synthetic cotton of the present invention using an infrared thermal imager,
3 is a photograph of the infrared radiation energy for natural cotton using an infrared thermal imager,
Figure 4 is a photograph of the infrared radiation energy for a conventional polyester synthetic cotton using an infrared thermal imager,
5 is a photograph of the antimicrobial test results for Staphylococcus aureus against the pyrogenic synthetic cotton of the present invention,
Figure 6 is a photograph of the antimicrobial test results for pneumococcus against the pyrogenic synthetic cotton of the present invention,
Figure 7 is a photograph of the antimicrobial test results for Pseudomonas aeruginosa for the pyrogenic synthetic cotton of the present invention.

EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail. However, even if necessary matters for carrying out the present invention, a detailed description thereof will be omitted for matters belonging to the known art or easily implemented by those skilled in the art.

Composition for producing a pyrogenic synthetic cotton wool according to the present invention, 20 to 30% by weight porous binder made of silicon dioxide and zeolite, 10 to 20% by weight graphene suspension, 50 to 65% by weight of fiber spinning polyester resin, auxiliary It consists of 2 to 5% by weight of the additive.

First, the porous binder has a function of suppressing the generation of precipitates and bubbles, and if the content is less than 20% by weight, there is a problem in preventing the generation of precipitates and bubbles, and if the content exceeds 30% by weight, graphene There is a problem with component adhesion.

The porous binder is composed of 80 to 95% by weight of silicon dioxide and 5 to 20% by weight of zeolite, having a particle diameter of 3 to 3.5 µm and a porosity of 60 to 80%.

Next, the graphene suspension preferably comprises 20 to 35 wt% of graphene powder having a particle diameter of 220 to 350 nm and 65 to 80 wt% of purified water. When the content of the graphene suspension is less than 20% by weight, there is a problem in the exothermic and thermal effects of the addition of graphene. On the contrary, when the content of the graphene suspension exceeds 35% by weight, it is difficult to extrude the fiber because it affects the strength of the polyester resin. have. The graphene suspension is prepared by injecting graphene powder having a particle diameter of 220 to 350 nm into a kneader with purified water and stirring it at 10,000 to 12,000 rpm for 2 to 3 hours.

The fiber spinning polyester resin is a synthetic resin for producing a conventional synthetic cotton, particularly preferably a polyethylene terephthalate (PET) resin. If the content of the polyester resin is less than 50% by weight, there is a problem in extruding the lowdenia fiber due to the flexibility of the polyester resin, on the contrary, if the content of the polyester resin exceeds 65% by weight, the graphene component content is relatively low to achieve the object of the present invention. There is a problem that is difficult to do.

Lastly, the auxiliary additives have an auxiliary function such as adsorption function, coating function, lubricant function, and impurity removal function of the graphene suspension and polyester resin, and their content includes 2 to 5% by weight. According to a preferred embodiment of the present invention, the auxiliary additive includes 45% by weight of acrylic stearic acid, 9% by weight of fatty acid ester calcium, 13.5% by weight of water-soluble calcium solution, 18.9% by weight of amine, 4.6% by weight of hydroxy magnesium silicate, It is preferred to consist of 9% by weight of fatty acid amine polyoxyester.

In the auxiliary additive, acrylic stearic acid has a function of preventing stickiness, that is, the spinning material does not stick to the machine during graphene fiber extrusion spinning, and the fatty acid ester calcium is a preservative to stably maintain and preserve the polyester resin and graphene components. The function of water-soluble calcium solution to prevent bubbles. And the amine has an adsorption function, the hydroxy magnesium silicate removes impurities, and the fatty acid amine polyoxyester has a function of improving the flexibility of the polyester resin.

Next, the method for preparing a pyrogenic synthetic cotton according to the present invention comprises the following steps A) to E). First step A) to prepare a composition for producing a pyrogenic synthetic cotton of the present invention described above.

In the next step B), the composition is put into a hermetic mixer, and the composition is kneaded well to press the internal pressure up to 100 MPa at a rate of 5 MPa / min in order to keep the mixing ratio constant, and then to facilitate injection again. In order to extrude under reduced pressure at a rate of 2 MPa / min until the atmospheric pressure in order to prepare a polyester chip mixed with graphene. It is preferable that the said polyester chip is about 0.5 * 1 * 1.3cm in size.

In the next step C), the polyester chip is heated at a temperature of 500 to 600 ° C. for 20 to 30 minutes to obtain a melt having 1.5 to 2.0% by weight of graphene contained in the melt. At this time, if the temperature is less than 500 ℃ melt state of the polyester chip is not intact, if it exceeds 600 ℃, the function of the auxiliary additive is inferior.

The content of graphene contained in the melt affects the strength and function of the fibers obtained in the last step E). In other words, if the graphene content is less than 1.5% by weight, the strength and function of the fiber are too weak. On the contrary, if the graphene content is higher than 2.0% by weight, the strength and function of the fiber are increased, but the strength is strong, which is not preferable because of the problem of flexibility. .

In the next step D), the melt is put into a sealed container, the internal pressure is increased to 400 to 450 MPa at a rate of 5 to 8 MPa / min, and maintained for 4 to 5 hours, and then 2 to 4 MPa / min. Reduce pressure to atmospheric pressure at

In the final step E), the melt passed through step D) is spun at a speed of 1,220 to 1,310 m / min to obtain a fiber, and the fiber is burned. To obtain a synthetic cotton. At this time, if the spinning speed of the melt is less than 1,220 m / min, the thickness of the fiber is increased, on the contrary, if it exceeds 1,310 m / min, the thickness of the fiber is thinned.

The fiber obtained in the step E) is preferably 1.5 to 2 denier in thickness. And the other side using the fiber The method is the same as the conventional method for producing synthetic cotton.

EXAMPLE

1) Preparation of the Composition

Next, the composition for preparing the exothermic synthetic cotton of the present invention was prepared according to the components and composition ratios as shown in Table 1.

Ingredient Content (% by weight) Example 1 Example 2 Example 3 Porosity
Binding substance Silicon dioxide 25 30 27 Zeolite Graphene suspension 10 15 20 Polyethylene Terephthalate Resin 62 52 50 Auxiliary additives 45% by weight of acrylic stearic acid 3 3 3 9% by weight of fatty acid ester calcium Water Soluble Calcium Solution 13.5 wt% Amine 18.9 wt% 4.6% by weight of hydroxy magnesium silicate 9% by weight of fatty acid amine polyoxyester Sum 100 100 100

2) Preparation of Synthetic Cotton

Each of the compositions of Examples 1 to 3 was introduced into a hermetic mixer, and the internal pressure was pressurized to 100 MPa at a rate of 5 MPa / min, and then decompressed at a rate of 2 MPa / min until the atmospheric pressure was again reached. Extrusion produced a polyester chip mixed with graphene.

The polyester chip was heated at a temperature of 580 ° C. for 25 minutes to obtain a melt, the melt was put into a sealed container, and the internal pressure was increased to reach 430 MPa at a rate of 7 MPa / min and maintained for 4 hours and 30 minutes. After that, the pressure was reduced to atmospheric pressure at a rate of 3 MPa / min.

Finally, the melt is spun at 1,280 m / min to obtain a fiber, and when the fiber is burned To prepare a synthetic cotton according to the present invention. 1 is a photograph of a pyrogenic synthetic cotton prepared according to Example 1;

[Performance Test]

1) pyrogenic test

Comparative test for pyrogenicity at Korea Far Infrared Applied Evaluation Institute (KFIA) affiliated with the Korea Far Infrared Association (KFIA), respectively, for the goose (polyester) and polyester synthetic cotton purchased commercially as the comparative example of the pyrogenic synthetic cotton of Example 1 Was carried out.

The test method was conducted under the condition of room temperature of 28 ° C. and humidity of 48% using an infrared thermal imager according to “KFIA-FI-1006”. Each sample to be tested was irradiated with heat at 40 ° C. for 10 minutes, and after 1 minute, the infrared radiation energy emitted from each sample was treated with images and temperature data, and the results were attached to FIGS. 1 to 3. .

Figure 1 is a test result for the pyrogenic synthetic cotton of the present invention, Figure 2 is a test result for the goose (cotton), Figure 3 is a test result for the polyester synthetic cotton. In each drawing, the red area means that the temperature is relatively high, and the pyrogenic synthetic cotton of the present invention has more red color than the goose (cotton) or polyester synthetic cotton, and thus does not fall to the maximum temperature. It can be seen that the relatively high temperature is maintained.

2) Far Infrared Emissivity and Radiation Energy Test

The far-infrared emissivity and the radiant energy of the pyrogenic synthetic cotton of Example 1 were tested in the Korea Far Infrared Applied Evaluation Institute. The test method was carried out according to 'KFIA-FI-1005', and the experimental equipment was carried out using a FT-IR Spectrometer at a temperature of 37 ° C. which is the body temperature of the human body.

As a result of the test, it was confirmed that the emissivity (5-20 μm) of the synthetic cotton prepared according to the present invention was 89.4%, and the radiation energy (37 ° C.) was 3.45 × 10 ² W / m ^{2 ·} μm.

3) antimicrobial test

The antimicrobial test was carried out on the pyrogenic synthetic cotton of Example 1 in the Korea Far Infrared Applied Evaluation Institute. Test method is KS K 0693; It was carried out according to 2016 (Antibacterial test method of fiber material), and used strains were Staphylococcus aureua ATCC 6538, Pneumococcus ( Klebsiella pneumoniae ATCC 4352), and Pseudomonas aeruginosa ATCC 27853. To the cell solution, 0.05% of the nonionic surfactant TWEEN 80 was added. The test results are shown in Table 2 below.

Use strain division BLANK  Example 1 Staphylococcus aureus Initial bacterial count 1.8 × 10 ⁴ / ml 1.8 × 10 ⁴ / ml After 18 hours 9.2 × 10 ⁶ / ml 1.2 × 10 ⁵ / ml Bacteriostatic rate - 98.7% Pneumococcal Initial bacterial count 1.8 × 10 ⁴ / ml 1.8 × 10 ⁴ / ml After 18 hours 3.8 × 10 ⁷ / ml 2.0 × 10 ⁵ / ml Bacteriostatic rate - 99.5% Pseudomonas aeruginosa Initial bacterial count 1.8 × 10 ⁴ / ml 1.8 × 10 ⁴ / ml After 18 hours 3.8 × 10 ⁷ / ml 6.6 × 10 ⁶ / ml Bacteriostatic rate - 77.4%

As shown in Table 2, the pyrogenic synthetic cotton prepared according to the present invention showed a bacteriostatic reduction rate of 98.7% for Staphylococcus aureus, 99.5% for pneumococci, and 77.4% for Pseudomonas aeruginosa. 5 to 7 are photographs of the antimicrobial test results for Staphylococcus aureus (FIG. 5), Pneumococcus (FIG. 6) and Pseudomonas aeruginosa (FIG. 7), respectively. In each figure, the photograph (A) is the synthetic cotton of Example 1, and the photograph (B) is the photograph about BLANK.

4) Deodorization performance test

The deodorizing performance of the pyrogenic synthetic cotton of Example 1 was tested in the Korea Far Infrared Applied Evaluation Institute. Test methods are described in FITI Test Guide FTM-5-2; It was carried out according to 2004 (Gas Detection Tube Act), and ammonia and formaldehyde were used as test gases.

100 ppm of ammonia and 15 ppm of formaldehyde, and 10 g of the heating batter of Example 1, respectively, were put into a gas bag having a capacity of 5 L, and after 2 hours, the concentration of test gas remaining in the gas bag was measured. Deodorization rate was calculated by.

As a result of the test, the exothermic synthetic cotton of Example 1 exhibited a deodorization rate of 63% for ammonia and 23.3% for formaldehyde. The deodorization rate (%) was calculated as "[(Cb-Cs) / Cb] x 100". Here, Cb means the concentration of the test gas remaining in the gas bag in the BLANK state, Cs means the concentration of the test gas remaining in the gas bag in which the exothermic synthetic cotton of Example 1 is added.

Claims (8)

20-30% by weight of a porous binder composed of silicon dioxide and zeolite;
10-20% by weight graphene suspension;
50 to 65% by weight of fiber spinning polyester resin;
Auxiliary additive consisting of 45% by weight of acrylic stearic acid, 9% by weight of fatty acid ester calcium, 13.5% by weight of water-soluble calcium solution, 18.9% by weight of amine, 4.6% by weight of hydroxymagnesium silicate, and 9% by weight of fatty acid amine polyoxyester 2 to 5 wt%;
Composition for producing a pyrogenic synthetic cotton, characterized in that consisting of.
The method of claim 1, wherein the porous binder is made of 80 to 95% by weight of silicon dioxide and 5 to 20% by weight of zeolite, having a particle diameter of 3 to 3.5㎛, porosity characterized in that the porosity of 60 to 80% Composition for preparing synthetic synthetic cotton.
The method of claim 1, wherein the graphene suspension is 20 to 35% by weight graphene powder having a particle diameter of 220 ~ 350 nm and 65 to 80% by weight purified water composition for producing a pyrogenic synthetic cotton.
The method of claim 1, wherein the fiber spinning polyester resin is a composition for producing pyrogenic synthetic cotton, characterized in that the polyethylene terephthalate (PET) resin.
delete A) preparing a composition for preparing a pyrogenic synthetic cotton of any one of claims 1 to 4;
B) The composition was put into a hermetic mixer, and the internal pressure was pressurized to 100 MPa at a rate of 5 MPa / min, and extruded while decompressing at a rate of 2 MPa / min until the pressure again reached atmospheric pressure. Preparing a mixed polyester chip;
C) heating the polyester chip at a temperature of 500 to 600 ° C. for 20 to 30 minutes to obtain a melt;
D) The melt is put in a sealed container, and the internal pressure is increased to 400 to 450 MPa at a rate of 5 to 8 MPa / min and maintained for 4 to 5 hours, and then at a rate of 2 to 4 MPa / min. Depressurizing to atmospheric pressure;
E) spinning the melt passed through step D) at a speed of 1,220 ~ 1,310 m / min to obtain a fiber, and burning the fiber To obtain a synthetic cotton;
Method for producing a pyrogenic synthetic cotton, characterized in that it is prepared, including.
The method of claim 6, wherein the melt obtained in step C) has a graphene content of 1.5 to 2.0% by weight.
The method of claim 6, wherein the fiber obtained in step E) has a thickness of 1.5 to 2 denier.

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