KR102584205B1 - fiber having the property of infrared ray radiation, antimicrobial and UV blocking, and method of manufacturing the same - Google Patents

Abstract

The present invention relates to a composite functional fiber that simultaneously exhibits far-infrared radiation, antibacterial, and UV blocking functions, and a method for manufacturing the same.
According to the present invention, it is possible to provide polyester fibers that exhibit various functions by manufacturing fibers by adding a masterbatch that is uniformly mixed at a high content of functional substances for far-infrared radiation, antibacterial and UV blocking to polyethylene terephthalate. It becomes.
In addition, by mixing a resin with a glass transition temperature higher than that of polyethylene terephthalate with polyethylene terephthalate, the running stability of the yarn is improved even during heating, stretching and high-speed running in the spinning process, thereby reducing the occurrence of breakage. Therefore, productivity improves.

Description

Fiber having the properties of far-infrared radiation, antimicrobial and UV blocking, and method of manufacturing the same {fiber having the property of infrared ray radiation, antimicrobial and UV blocking, and method of manufacturing the same}

The present invention relates to a composite functional fiber that simultaneously exhibits far-infrared radiation, antibacterial, and UV blocking functions, and a method for manufacturing the same.

In order to impart various functions such as far-infrared radiation, antibacterial properties, and UV protection to fibers, a method of manufacturing functional fibers by adding organic or inorganic substances with these functions in the form of a masterbatch has been developed.

However, when melt spinning synthetic fibers, there is a problem in that many thread breaks occur and the functional materials are not sufficiently dispersed, resulting in deterioration of physical properties and functionality.

Meanwhile, when melt spinning polyethylene terephthalate, various methods have been developed to improve stability for high-speed spinning.

However, melt spinning of polyethylene terephthalate to which various inorganic additives are added to provide functionality has the problem that winding at high speed during spinning increases the shaking of the yarn and increases the occurrence of broken yarns.

In particular, if the yarn discharged from the spinneret is cooled at a temperature below the glass transition temperature (Tg) of polyethylene terephthalate and then stretched and heat-set in a heat treatment tank to a temperature above Tg, there is a problem in that the breakage increases.

Republic of Korea Patent No. 0591210 (High-strength, low-shrinkage industrial polyester fiber and manufacturing method thereof)

The present invention is intended to solve the problems described above, and is a method for producing a fiber with far-infrared radiation, antibacterial, and UV blocking functions that enables high-speed spinning even when the content of inorganic substances that provide functionality is high when producing polyethylene terephthalate fiber. It is about providing.

In order to solve the above problem, the present invention mixes a multi-functional masterbatch containing a functional material with far-infrared radiation, antibacterial, and UV blocking functions, polyethylene terephthalate, and a resin having a higher glass transition temperature than the polyethylene terephthalate. Obtaining a melt by heating and melting; Obtaining solidified fiber by discharging the melt through a spinneret and cooling it below the glass transition temperature of the polyethylene terephthalate; stretching the solidified fiber by heating it to a temperature equal to or higher than the glass transition temperature; and winding at a speed of 3300 m/min or more. It provides a method for manufacturing a fiber having far-infrared radiation, antibacterial, and UV blocking functions.

According to the present invention, it is possible to provide polyester fibers that exhibit various functions by manufacturing fibers by adding a masterbatch that is uniformly mixed at a high content of functional substances for far-infrared radiation, antibacterial and UV blocking to polyethylene terephthalate. It becomes.

In addition, by mixing a resin with a glass transition temperature higher than that of polyethylene terephthalate with polyethylene terephthalate, the running stability of the yarn is improved even during heating, stretching and high-speed running in the spinning process, thereby reducing the occurrence of breakage. Therefore, productivity improves.

In the present invention, a mixture of a multi-functional masterbatch containing a functional material with far-infrared radiation, antibacterial, and UV blocking functions, polyethylene terephthalate, and a resin having a higher glass transition temperature than the polyethylene terephthalate is discharged through a spinneret. , obtaining a solidified fiber by cooling below the glass transition temperature of the polyethylene terephthalate, heating the solidified fiber to a temperature above the glass transition temperature, stretching, and winding at a speed of 3300 m/min or more, far-infrared radiation, antibacterial and It relates to a method of manufacturing fibers with UV blocking function.

The multi-functional masterbatch contains 60 to 90% by weight of polyethylene terephthalate and 10 to 40% by weight of a functional material, and the functional material includes 15 to 35% by weight of antibacterial zeolite, 15 to 35% by weight of UV blocker, and oxidation agent. It may contain 30 to 70% by weight of aluminum.

The antibacterial zeolite is a zeolite in which an antibacterial material is supported, and a metal having antibacterial properties is preferably supported on the zeolite.

Aluminum oxide is a material that emits far-infrared rays and is an inorganic material that also has UV blocking and antibacterial functions.

The multi-functional masterbatch is manufactured using an extruder divided into a first section, a second section, a third section, a fourth section, and a fifth section, and in the first section, polyester is heated to 100-150°C. A melting step of melting with a passage time of 8 to 15 seconds; In the second section, a first functional material input step in which the antibacterial zeolite with a specific gravity of 2.0 to 3.0 and a UV blocker with a specific gravity of 2.0 to 3.0 are added and heated to 150 to 200 ° C. with a passage time of 3 to 6 seconds; The third section includes a second functional material input step of adding aluminum oxide and heating to 200-240°C with a passing time of 2-4 seconds; The fourth section includes a mixing step of heating to 240 to 270°C and passing through and mixing with a passing time of 1 to 3 seconds; And the fifth section can be manufactured by heating to 240-270°C and extruding.

The multi-functional masterbatch is manufactured by adjusting the specific gravity of antibacterial zeolite and UV blocker to 2.0 to 3.0 and adding it to the second section, and aluminum oxide with a specific gravity of 4.0 to 4.5 is added to the third section, so it has good miscibility and dispersibility. become superior In other words, it becomes a polyester masterbatch containing a high content of functional materials while maintaining a uniform content of functional materials.

It is preferable for the functional material to have an average particle diameter of 0.03 to 1.0 ㎛ for producing fibers. If it is less than 0.03 ㎛, it is added to the fiber and stretched through a heat treatment tank to be described later, and hair is generated in the fiber manufactured by high-speed spinning. The uniformity of the fiber may decrease, and if it exceeds 1.0㎛, the extensibility of the fiber may decrease and breakage may occur.

The polyethylene terephthalate is generally used for fibers, and one with an intrinsic viscosity of 0.55 to 0.65 is preferably used.

By using a resin with a higher glass transition temperature than the polyethylene terephthalate, even if the melted and discharged yarn is spun at a high speed of 3,500 m/min or more, the shaking of the yarn is suppressed and spinning can be performed stably.

If a resin with a lower glass transition temperature than polyethylene terephthalate is used, it is difficult to spin stably at high speeds.

At this time, the resin having a higher glass transition temperature than the polyethylene terephthalate is preferably contained in an amount of 0.1 to 1.0% by weight. If it is less than 0.1% by weight, shaking of the melted and discharged yarn is not suppressed, making it difficult to spin stably at high speeds. If it exceeds 1.0% by weight, miscibility decreases, mechanical strength decreases, and it is economically undesirable.

In the present invention, polyethylene naphthalate can be used as a resin with a higher glass transition temperature than polyethylene terephthalate. The polyethylene naphthalate preferably has a high molecular weight, and the weight average molecular weight is preferably 50,000 or more.

In the spinning process of the present invention, the yarn discharged from the spinneret and solidified by cooling is stretched and heat-set by running it through a heat treatment tank, and after applying an emulsion with an emulsion application device, it is transferred to a winding roller at a predetermined winding speed. It can be carried out by winding.

The cooling can form a solidified thread by cooling wind blown by a radiant cooling device, and the solidified thread formed in this way is cooled to a temperature below the glass transition temperature, more preferably at a temperature 10° C. lower than the glass transition temperature. It is better to cool it down.

The heat treatment tank is preferably located 0.5 to 1.5 m away from the spinneret.

The temperature of the heat treatment tank can be adjusted by arbitrarily selecting optimal conditions below 300°C.

If the temperature is below Tg, stretching is not possible or cold stretching results in a high-orientation, low-specific-gravity yarn with high orientation but low specific gravity. Since uniform stretching is not achieved, dyeing stains are likely to occur. If it exceeds 250℃, the stretching becomes stronger, so the yarn fineness on the upstream side increases, which lowers the spinning tension near the entrance, making it easy for the yarn to shake.

For this reason, it is recommended that the temperature of the heat treatment tank is 150~220℃.

Even after passing through the heat treatment tank, the deterioration of the polyethylene terephthalate fiber is suppressed by the inorganic substances that make up the composite functional masterbatch, and stable driving can be achieved.

After applying the emulsion, it is better to set the winding speed of the winding roller to 3,500 m/min or more because the mechanical properties are improved.

If the winding speed is less than 3,500 m/min, the stretching of the fiber in the heat treatment tank may not be sufficient and the mechanical properties may deteriorate, and tension fluctuations and overheating may occur in the yarn, resulting in uneven stretching.

Additionally, uniformity may decrease and mush may occur.

Meanwhile, the present invention uses a guide made of high purity (99.99% or more) alumina with a hardness of 15 GPa or more, so that the spinning process can be performed even if it contains a high content of inorganic substances of 1% by weight or more and is melt-spun at a high winding speed of 3,500 m/min or more. Since various guides do not wear out quickly, the occurrence of thread breakage and hair loss can be suppressed.

According to the present invention, by containing 0.1 to 10% by weight of a complex functional inorganic material, it is possible to stretch at high speed without deteriorating the fiber in a heat treatment tank for stretching and heat fixing, and by using a resin with a higher glass transition temperature than polyethylene terephthalate, the stretching is possible. ·When running in a heat treatment tank for heat fixation, shaking is suppressed and stretching at high speed is possible, making it possible to manufacture fibers with improved far-infrared ray radiation, antibacterial and UV blocking functions with improved productivity.

Hereinafter, the present invention will be described in more detail based on the following examples.

However, the following examples are only for illustrating the present invention, and the present invention is not limited by the following examples, and may be substituted or changed to other equivalent examples without departing from the technical spirit of the present invention. It will be clear to those skilled in the art that the present invention pertains.

[Production Example 1]

In the first section of the extruder, polyethylene terephthalate for textiles was introduced and passed at 100-150°C for 11 seconds. In the second section, antibacterial zeolite loaded with silver with a specific gravity of 2.3 and an inorganic UV blocker with a specific gravity of 2.6 were added and processed for 150~150°C. Pass at 200℃ for 4 seconds, add aluminum oxide with a specific gravity of 4.1 in the third section, pass at 200~240℃ for 3 seconds, pass at 240~270℃ for 2 seconds in the fourth section, and pass at 270℃ in the fifth section. The molten mixture was passed at ~290°C and extruded through a die, then cooled and cut to prepare multi-functional masterbatch pellets containing 20% by weight of functional material.

The average particle diameter of the functional material used at this time was about 500 nm.

In addition, the content ratio of the functional materials used was antibacterial zeolite: UV blocker: aluminum oxide in a weight ratio of 25:25:50.

[Production Example 2]

In the first section of the extruder, polyethylene terephthalate for textiles is introduced and passed at 100-150°C for 11 seconds. In the second section, antibacterial zeolite loaded with silver with a specific gravity of 2.3, an inorganic UV blocker with a specific gravity of 2.6, and a specific gravity of 4.1 are added to the second section. Add aluminum oxide and pass at 150-200℃ for 4 seconds, in the third section, pass at 200-240℃ for 3 seconds, in the fourth section, pass at 240-270℃ for 2 seconds, and in the fifth section, pass at 270-290℃. The molten mixture at ℃ was passed and extruded through a die, then cooled and cut to prepare a multi-functional masterbatch pellet containing 20% by weight of the functional material.

The average particle diameter of the functional material used at this time was about 500 nm.

In addition, the content ratio of the functional materials used was antibacterial zeolite: UV blocker: aluminum oxide in a weight ratio of 25:25:50.

[Example 1]

89.5% by weight of polyethylene terephthalate with an intrinsic viscosity of 0.64, 10% by weight of the multi-functional masterbatch of Preparation Example 1, and 0.5% by weight of polyethylene naphthalate (Tg = 123°C), mixed and heated to obtain a molten mixture, 295 At ℃, discharge is made through a spinneret with a discharge hole diameter of 0.2 mmΦ, a land length of 0.8 mm, and the number of holes is 36, and cooling wind with a temperature of 25℃ and a humidity of 65RH% is blown at a speed of 0.5 m/sec, and the discharged and solidified fiber is Cooled to 65°C.

Afterwards, stretching was carried out in an air atmosphere heated to 150°C in a heat treatment tank with a length of 1 m and an inner diameter of 30 mm located 1.5 m below the spinneret, and an emulsion was applied using a guide oiling method, followed by stretching at a speed of 4,500 m/min. Polyester fibers were prepared by winding and stretching them.

At this time, a guide made of 99.99% purity alumina with a hardness of 15.7 GPa was used in the oiling guide part.

The polyester fiber of 75 denier/36 filaments thus obtained was tested and evaluated as follows.

[Comparative Example 1]

Polyester fiber was manufactured using the same method as Example 1, except that in Example 1, the multi-functional masterbatch of Preparation Example 2 was used instead of the multi-functional masterbatch of Preparation Example 1.

[Comparative Example 2]

Polyester fiber was manufactured using the same method as Example 1, except that 90% by weight of the polyethylene terephthalate and 10% by weight of the multi-functional masterbatch of Preparation Example 1 were used.

[Comparative Example 3]

Polyester fiber was manufactured using the same method as Example 1, except that the winding speed was set to 2,800 m/min.

[Comparative Example 4]

Polyester fiber was manufactured using the same method as Example 1, except that a guide made of alumina with 99% purity was used as the oil supply guide part.

The manufacturing process characteristics and physical properties in the examples and comparative examples were evaluated as follows, and the results are shown in Table 1.

1. Radioactivity

100 kg of fiber was spun, the presence or absence of thread breaks during spinning was examined, the presence or absence of fluff in the obtained fiber was visually observed, and evaluated according to the following evaluation criteria.

◎: No thread breakage occurs during spinning, no fluff is generated in the obtained fiber, and spinnability is extremely good.

○: No thread breakage occurs during spinning, and although some fluff occurs in the obtained fiber, spinnability is almost good.

△: When spinning, thread breakage occurs three times or less, and spinnability is poor.

×: During spinning, thread breakage occurs more than three times, and spinnability is very poor.

2. Number of cows

The hair sensor detects the occurrence of hair in a fiber length of 10 ⁷ m or more and converts it to the number of hairs per 10 ⁶ m of fiber length.

3. Lubrication guide abrasion

Melt spinning is performed for one month using a new guide, and the wear state of the guide surface is observed at magnification (X400 times) in the oiling guide (contact section) to evaluate the progress of wear.

○: Almost no wear is observed.

△: Some wear is observed.

×: Large wear is observed.

4. Far-infrared radiation

A plain fabric made of manufactured polyester fiber was used as a sample, and the test method was KFIA-FI-1005 (infrared emissivity and radiant energy of the sample, black body (FT-IR spectrometer) using an infrared spectrophotometer (FT-IR spectrometer) at 37°C. Measured against black body.

5. Antibacterial

A plain fabric made of manufactured polyester fiber was used as a sample, and the antibacterial level was tested bacteriostatically using Staphylococcus aureus (ATCC 6538) and Klebsiella pneumococcus (ATCC 4352) as test strains according to KS K 0693. Evaluated by reduction rate.

6. UV protection

The ultraviolet ray blocking rate is measured using the KS K 0850:2014 test method.

The wavelength range is UV-A (315 ~ 400 nm) and UV-B (290 ~ 315 nm).

Example 1 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 radioactive ◎ △ △ ○ ○ Number of mow 0 0.3 One 0.1 0.05 Strength (g/d) 4.57 3.5 3.8 3.1 4.55 Uniformity (U%) 0.58 1.62 1.85 1.2 0.75 Lubrication guide wear resistance
○ ○ ○ ○ △ far infrared rays
radioactive far infrared rays
emissivity
(5~20㎛ wavelength range) 0.902 0.870 - - - radiant energy
(W/m2·㎛, 37℃) ^{3.48 3.27} - - - antibacterial Staphylococcus aureus 99.9% 99.5% - - - pneumoniae 99.9% 99.5% - - - UV protection UV-A 98.2% 93.8% - - - UV-B 98.1% 93.6% - - -

From the results in Table 1, it is confirmed that the far-infrared radiation, antibacterial, and UV blocking performance of Example 1 is superior to that of Comparative Example 1, and therefore, the use of the multi-functional masterbatch according to the present invention provides improvement in functionality. .

In addition, since the spinnability, strength, and uniformity of Example 1 are superior to those of Comparative Example 2, it is confirmed that adding a resin with a higher glass transition temperature than the polyethylene terephthalate according to the present invention provides improvement in spinning workability. .

Claims (5)

A multi-functional masterbatch containing functional substances with far-infrared radiation, antibacterial and UV blocking functions, mixed and heated to contain 0.1 to 1.0% by weight of polyethylene terephthalate and polyethylene naphthalate, which has a higher glass transition temperature than polyethylene terephthalate. Obtaining a melt by melting;
Obtaining solidified fiber by discharging the melt through a spinneret and cooling it below the glass transition temperature of the polyethylene terephthalate;
stretching the solidified fiber by heating it to a temperature equal to or higher than the glass transition temperature;
Applying an emulsion by passing it through an oil supply guide provided with a guide made of alumina with a hardness of 15.7 GPa and a purity of 99.99%; and
A method of manufacturing a fiber having far-infrared radiation, antibacterial, and UV blocking functions, including the step of winding at a speed of 3300 m/min or more. According to clause 1,
The multi-functional masterbatch contains 60-90% by weight of polyester and 10-40% by weight of functional material, and the functional material includes 15-35% by weight of antibacterial zeolite, 15-35% by weight of UV blocker, and aluminum oxide. A method of manufacturing a fiber with far-infrared radiation, antibacterial and UV blocking functions, characterized in that it contains 30 to 70% by weight. According to clause 2,
The multi-functional masterbatch is manufactured using an extruder divided into a first section, a second section, a third section, a fourth section, and a fifth section,
In the first section, a melting step of heating polyester to 100-150°C and melting it with a passage time of 8-15 seconds;
In the second section, a first functional material input step in which the antibacterial zeolite with a specific gravity of 2.0 to 3.0 and a UV blocker with a specific gravity of 2.0 to 3.0 are added and heated to 150 to 200 ° C. with a passage time of 3 to 6 seconds;
The third section includes a second functional material input step of adding aluminum oxide and heating to 200-240°C with a passing time of 2-4 seconds;
The fourth section includes a mixing step of heating to 240 to 270°C and passing through and mixing with a passing time of 1 to 3 seconds; and
The fifth section is a method of manufacturing a fiber having far-infrared radiation, antibacterial, and UV blocking functions, comprising the step of heating and extruding at 240 to 270°C. delete delete