KR101989932B1 - Lyocell-like PET multi-functional Master Batch and Preparation method thereof, Polyester fiber using the same - Google Patents

Abstract

The present invention relates to a process for preparing a multifunctional master batch of a PET multifunctional master produced through an extruder divided into a first section, a second section, a third section, a fourth section and a fifth section, An ester master batch is introduced and heated at 100 to 150 DEG C for a passage time of 8 to 15 seconds to melt the polyester; A BBOT feeding step in which BBOT (2,5-bis- (5-t-butylbenzoxazolyl) thiophene) is fed in the second section and is passed at a passage time of 3 to 6 seconds while being heated to 150 to 200 ° C; Barium sulphate and tourmaline in which barium sulphate (BaSO ₄ ) and tourmaline are introduced in the third section and which is passed through at a passage time of 2 to 4 seconds while being heated to 200 to 240 ° C; The fourth section is heated at a temperature of 240 to 270 DEG C for 1 to 3 seconds; And an extrusion step of extruding polyester containing barium sulfate, tourmaline and BBOT as functional materials while heating at 270 to 290 ° C in the fifth section. The multifunctional Lyocellike PET multifunctional master batch and its production ≪ / RTI >

Description

Lyocellike PET multifunctional masterbatch, a method for producing the same, a polyester fiber using the same, a polyester fiber using the same,

The present invention relates to a Lyocellike PET multifunctional masterbatch, a process for preparing the same, a polyester fiber using the same, a Lyocellike PET multifunctional masterbatch imparting multifunctionality to a PET masterbatch, a process for producing the same, a polyester fiber .

As the level of living has improved, it has been expected that fabrics that can produce apparel having functionalities with aesthetic functions in appearance while making the human body more comfortable and comfortable beyond the conventional clothing concept are expected to appear. We are introducing more advanced yarns and fabrics.

Recently, synthetic fibers have become more sophisticated in order to improve the physical properties that complement weaknesses of natural fibers and to maximize the advantages of synthetic fibers. Representative functional materials include sweat-absorbed quick-drying, antistatic, UV-blocking, cold-feeling, antibacterial and deodorizing functions, and secondary textile products thereof.

Conventionally, as a method for imparting functionality to synthetic fibers, a polymer masterbatch containing a functional material is prepared, and then a polymer masterbatch containing a functional substance and a general polymer masterbatch are mixed and fiberized to impart functionality to the fiber have.

Korean Patent Laid-Open No. 1998-033438 discloses a method for producing a polyester fiber having excellent deodorizing and antibacterial properties. A polyester masterbatch containing microparticles of elvan which emits far-infrared rays having an antibacterial and deodorizing function is prepared, And polyester fibers having an antibacterial and deodorizing function through a spinning process in combination with a master batch.

Korean Patent Registration No. 0481358 discloses a method in which a master batch containing zeolite-based inorganic particles having metal ions having antimicrobial and deodorant properties is mixed with a general polyester master batch at a certain ratio and spun to prepare a fiber .

As described above, in the prior art, the polymer masterbatch containing the functional material is formed by extruding the functional material and the polymer masterbatch into an extruder, mixing the mixture in the extruder, forming the strand into a strand, cutting the pellet ).

In the polymer masterbatch containing the functional material prepared as described above, it is very important that the functional material is contained uniformly, and it is preferable that a high content of the functional material is contained for economical efficiency and fairness at the time of fiber production.

However, when a high content of the functional material is contained in the polymer masterbatch, it is difficult to uniformly contain the functional material contained in the masterbatch.

In addition, in order to impart multifunctionality to a fiber, the functional master material has a single function. In order to impart a multifunctionality to the fiber, there is a problem that a polymer masterbatch containing a large number of functional materials must be used. And the physical properties such as strength and elongation are deteriorated.

Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made to solve the above problems of the prior art, and it is an object of the present invention to provide a process for producing a multifunctional Lyocellike PET masterbatch capable of containing a high content of functional materials capable of imparting multi- The purpose.

It is also an object of the present invention to provide a PET multifunctional master batch in the method of manufacturing the above-described Lyocellike PET multifunctional masterbatch.

It is another object of the present invention to provide a lyocell-like PET fiber having a tactile feel similar to a lyocell using the above-mentioned Lyocellike PET multifunctional masterbatch.

The present invention relates to a process for preparing a multifunctional master batch of a PET multifunctional master produced through an extruder divided into a first section, a second section, a third section, a fourth section and a fifth section, An ester master batch is introduced and heated at 100 to 150 DEG C for a passage time of 8 to 15 seconds to melt the polyester; A BBOT feeding step in which BBOT (2,5-bis- (5-t-butylbenzoxazolyl) thiophene) is fed in the second section and is passed at a passage time of 3 to 6 seconds while being heated to 150 to 200 ° C; Barium sulphate and tourmaline in which barium sulphate (BaSO ₄ ) and tourmaline are introduced in the third section and which is passed through at a passage time of 2 to 4 seconds while being heated to 200 to 240 ° C; The fourth section is heated at a temperature of 240 to 270 DEG C for 1 to 3 seconds; And an extrusion step of extruding polyester containing barium sulfate, tourmaline, and BBOT as functional materials while heating at 270 to 290 ° C in the fifth section. The method of manufacturing a multifunctional Lyocellike PET masterbatch according to claim 1, to provide.

Also, the present invention provides a process for preparing a multifunctional master batch of the lyocellike PET characterized in that the functional material is contained in an amount of 40 wt% or more.

Also, the present invention provides a process for preparing a multifunctional master batch of the lyocell-like PET comprising the functional material in an amount of 40 to 55 wt%.

The present invention also provides a process for preparing a multifunctional master batch of a lyocellike PET characterized in that the barium sulfate and tourmaline are contained in a mixing ratio of 1.0: 0.8 to 1.2 and the BBOT is contained in 2 to 8 phr of the master batch.

Also provided is a Lyocellike PET multifunctional masterbatch which is produced by the above process.

Also provided is a Lyocellike PET multifunctional fiber characterized in that it is formed using the Lyocellike PET multifunctional masterbatch.

The present invention also provides a multifunctional Lyocellike PET fiber characterized in that the polyester fiber contains 4 to 6 wt% of barium sulfate, 4 to 6 wt% of tourmaline, and 0.03 to 0.5 wt% of BBOT.

As described above, the method for preparing a multifunctional master batch of the LI-CELL-like PET according to the present invention is a method for preparing multifunctional master batches of biosurfactants such as barium sulfate, tourmaline and BBOT, which are functional materials, There is an effect that a master batch can be manufactured.

Also, there is an effect that it is possible to produce a PET multifunctional master batch containing a functional material with a uniform content of the functional material and a high content of the functional material with a content of 50 wt% or more.

In addition, the lyocellike PET multifunctional fiber of the present invention has a high ultraviolet blocking ratio and excellent antimicrobial activity due to the function of barium sulfate, tourmaline and BBOT which are functional materials.

FIG. 1 is a view showing a process of a process for producing a multifunctional master batch of the Lyocellike PET according to the present invention.
Figure 2 is a schematic illustration of an extruder for producing the Lyocellike PET multifunctional master batch of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. First, it should be noted that, in the drawings, the same components or parts have the same reference numerals as much as possible. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted so as to avoid obscuring the subject matter of the present invention.

As used herein, the terms " about, " " substantially, " " etc. ", when used to refer to a manufacturing or material tolerance inherent in the stated sense, Accurate or absolute numbers are used to help prevent unauthorized exploitation by unauthorized intruders of the referenced disclosure.

FIG. 1 is a process diagram of a method for producing a multifunctional master batch of the Lyocellike PET according to the present invention, and FIG. 2 is a schematic diagram of an extruder for producing the multifunctional master batch of the Lyocellike PET multifunctional masterbatch of the present invention.

The present invention is barium sulfate (BaSO _4), tourmaline and BBOT relates to a method for producing lyocell-like PET multifunctional masterbatch - a (2,5-bis (5-t- butyl-benzoxazolyl) thiophene) as functional material As shown in Fig. 1, is prepared including a melting step, an BBOT introduction step, a barium sulfate and tourmaline introduction step, a mixing step, and an extrusion step.

The barium sulphate is excellent in optical properties and has antimicrobial properties and has a property of blocking ultraviolet rays.

Tourmaline is a crystal belonging to the hexagonal system with crystal structure and promotes the metabolism of the body by generating far infrared rays and anions, activates cell function and immune function, and has strong heat effect and high penetration power to improve blood circulation and purification .

The BBOT acts as a photocatalyst for converting light such as infrared rays and ultraviolet rays into visible light, and acts to increase the antibacterial and UV shielding properties of barium sulfate and tourmaline.

The barium sulfate, tourmaline and BBOT may preferably be those having a particle size of 400 to 500 nm in order to improve workability and ease of dispersion.

The Lyocellike PET multifunctional master batch of the present invention is produced through an extruder divided into a first section, a second section, a third section, a fourth section and a fifth section, and the first section, the second section, The third section, the fourth section, and the fifth section are not distinguished from each other by the heating temperature of the extruder.

As shown in FIG. 2, the extruder used in the present invention is generally a device that is mixed and extruded through a screw. In the present invention, it is preferable to use an extruder having a twin screw.

The temperature of the first section, the second section, the third section, the fourth section, and the fifth section may be increased with an increase in section, and an extruder whose heating temperature is controlled for each section should be used.

The melting step is a step of proceeding in a first section. In the first section, a polyester master master batch is charged, and the polyester is melted by passing at a passage time of 8 to 15 seconds while heating at 100 to 150 ° C.

Generally, a polyester resin has a melting point of about 250 ° C or higher and is not melted when heated at 100 to 150 ° C in a melting step. However, the polyester master batch is squeezed by screw rotation in the extruder, Lt; / RTI >

The general polyester master batch melts at least about 80% while passing through the first section and the second section of the melting step, and is mostly melted in the third section.

The BBOT is carried out in the second section, and BBOT (2,5-bis- (5-t-butylbenzoxazolyl) thiophene) is introduced and heated for 3 to 6 seconds It is a step that passes by time.

The barium sulphate and tourmaline loading step is a step performed in the third section. Barium sulphate (BaSO ₄ ) and tourmaline are charged and passed at a passage time of 2 to 4 seconds while being heated to 200 to 240 ° C.

The mixing step is a step performed in the fourth section, and mixing the barium sulfate, tourmaline, and BBOT added in the second section and the third section so as to be uniformly mixed.

The inventors of the present invention have found from various experiments that the dispensing timing of the functional substance differs depending on the specific gravity of the substance, and the BBOT has a specific gravity of about 1.05 to 1.4, Barium sulfate has a specific gravity of about 4.0 to 4.5 and tourmaline has a specific gravity of 3.0 to 3.5. Thus, it has excellent mixing properties and dispersibility in the third section.

When the barium sulfate and tourmaline are put in the third zone, barium sulfate and tourmaline are precipitated at the lower end of the extruder, and when the barium sulfate and tourmaline are added in the third zone, The mixing property may be deteriorated. If the polyester is put in after the third section, the dispersibility may be lowered and the uniformity of the content contained in the polyester master batch may be lowered.

In addition, the passing time of each section is the time during which the polyester stays in the section. In the first section, it takes a long time for the polyester to pass in the progressing state, but the polyester gradually melts and the polyester heating temperature rises. The passing time is increased accordingly.

The transit time may be an element that keeps the polyester state in the section the same, and if the transit time deviates from the range described above, the uniformity of the functional material content may be lowered.

The passage time per section may control the rotation speed of the extruder screw.

The extruding step is a step of extruding polyester containing barium sulfate, tourmaline and BBOT as functional ingredients while heating to 270 to 290 ° C in the fifth step.

In the extruding step, the polyester containing the functional material is extruded to form a strand. The polyester containing the functional material extruded in the strand form is cut through a cutting step to form a pellet- . ≪ / RTI >

The multifunctional master batch of the present invention, which is prepared as described above, contains a high content of barium sulphate, tourmaline and BBOT as functional materials, and it is preferable that the functional material is contained in an amount of 40 wt% or more, 40 to 55 wt%.

The functional materials barium sulfate and tourmaline are preferably contained in a mixing ratio of 1.0: 0.8-1.2 by weight, and the BBOT is preferably contained in 2 to 8 phr (parts per hundred resin) of the master batch.

The method for preparing a PET masterbatch containing the functional material of the present invention as described above is a method for preparing a functional masterbatch containing functional materials such as barium sulfate, tourmaline, and BBOT, which are functional materials, Containing PET masterbatch can be prepared.

The multifunctional Lyocellike PET multifunctional fiber may be prepared through the Lyocellike PET multifunctional masterbatch of the present invention.

Barium sulphate, tourmaline and BBOT contained in the Lyocellike PET multifunctional fiber may preferably contain 4 to 6 wt% of barium sulfate, 4 to 6 wt% of tourmaline and 0.03 to 0.5 wt% of BBOT in order to exhibit functionality.

The Lyocellike PET multifunctional fiber produced using the Lyocellike PET multifunctional master batch of the present invention has various functions such as UV blocking property, antibacterial property, deodorizing property and the like.

Hereinafter, examples of the method for producing the Lyocellike PET multifunctional master batch according to the present invention are shown, but the present invention is not limited to the examples.

◈ Evaluation of uniformity of content according to the input range of functional material

1. Evaluation of Barium Sulfur Content Uniformity

A polyester masterbatch with a melting point of about 260 deg. C and a twin screw extruder were used to prepare a PET masterbatch.

The temperature and the transit time for each section of the extruder are shown in Table 1. The PET master batch was prepared by forming the temperature for each section to gradually increase as the extrusion proceeded.

- Barium sulphate with a particle size of about 400 nm was injected into each section and the content of barium sulphate was adjusted from 40 to 65 wt% to prepare a PET master batch having different barium sulfate contents. The range of barium sulfate content The results are shown in Table 2.

* The content error range (%) was calculated by the following formula, by measuring 5 g of the prepared PET masterbatch at 500 to 600 ° C. for 30 to 60 minutes to remove the PET resin, and then measuring the weight of the residual ash. The experiment was repeated 30 times to measure the error range.

* Content error range calculation formula: [(Weight of functional material injected-Ash weight) / Weight of functional material injected] * 100

division Temperature (℃) Pass Time (s) Section 1 100 to 150 11 The second section 150 ~ 200 4 Section 3 200 to 240 3 Section 4 240 ~ 270 2 Section 5 270 ~ 290 -

division 40wt% 45wt% 50wt% 55wt% 60wt% 65wt% Section 1 ± 3.1 ± 4.9 ± 6.3 ± 8.2 ± 9.9 ± 11.8 During the second section ± 0.7 ± 1.5 ± 2.7 ± 3.9 ± 5.1 ± 7.2 Section 3 ± 0.2 ± 0.7 ± 1.6 ± 2.5 ± 3.7 ± 5.9 Section 4 ± 2.8 ± 3.9 ± 5.2 ± 6.9 ± 8.2 ± 9.8

As shown in Table 2, when the barium sulphate was added in the third section, the content error range was measured to be the smallest, and it was found that the content uniformity was the best in the PET masterbatch placed in the third section.

2. Evaluation test of homogeneity of content of tourmaline

The same procedure as in the above evaluation of the uniformity of barium sulfate content was carried out using tourmaline having a particle size of about 400 nm and the results are shown in Table 3.

division 40wt% 45wt% 50wt% 55wt% 60wt% 65wt% Section 1 ± 1.9 ± 3.0 ± 4.9 ± 6.4 ± 7.9 ± 10.0 The second section ± 0.2 ± 0.7 ± 1.5 ± 2.4 ± 3.9 ± 5.4 Section 3 ± 0.1 ± 0.4 ± 1.2 ± 2.1 ± 3.0 ± 4.2 Section 4 ± 1.5 ± 2.7 ± 3.9 ± 5.8 ± 7.4 ± 9.0

As shown in Table 3, the content error of the tourmaline was measured to be the smallest when injected in the third zone, and it was found that the content uniformity was the best in the PET master batch placed in the third zone.

◈ Evaluation of uniformity of contents in Examples and Comparative Examples

1. Example

The PET masterbatch was prepared in the same manner as in the evaluation of the content uniformity according to the functional ingredient input period. The BBOT having a particle size of about 410 nm was charged in the second section, and barium sulfate having a particle size of about 400 nm and barium sulfate having a particle size of about 400 nm Tourmaline was injected in the third section to produce the Lyocellike PET multifunctional master batch of the present invention.

The functional materials barium sulfate and tourmaline were contained in a mixing ratio of 1: 1 by weight and BBOT was contained in 3 phr of the masterbatch. By controlling the content of the functional material to 40 ~ 65 wt%, a multifunctional master batch of Lyocellike PET having different functional material contents was prepared.

2. Comparative Examples 1 to 3

BBOT, barium sulfate and tourmaline were added to the first section, Comparative Example 2 was applied to the first section, BBOT and barium sulfate were added to the second section, In Comparative Example 3, the BBOT was charged in the third section, and the barium sulfate and tourmaline in the fourth section to prepare a PET master batch.

3. Above ◈ The content error range of functional materials was measured by the contents of the examples and the comparative examples as in the evaluation of the uniformity of contents according to the intervals of the functional materials, and the results are shown in Table 4.

division 40wt% 45wt% 50wt% 55wt% 60wt% 65wt% Example ± 0.1 ± 0.2 ± 0.6 ± 1.0 ± 2.0 ± 3.5 Comparative Example 1 ± 4.2 ± 6.2 ± 12.1 ± 14.4 ± 17.9 - Comparative Example 2 ± 3.1 ± 4.1 ± 6.4 ± 8.9 ± 10.9 ± 14.4 Comparative Example 3 ± 3.5 ± 4.9 ± 7.7 ± 9.3 ± 11.8 ± 16.5

As shown in Table 4, the Lyocellike PET multifunctional masterbatch of the present invention has a very small content error range of the functional material as compared with the PET masterbatch of the comparative example, and the Lyocellike PET multi- It can be seen that the content uniformity is very excellent.

In addition, when the content of the functional material is 60 wt% or more, the content error range is increased, and the content of the functional material is most preferably 40 to 55 wt%.

◈ Manufacture and functional evaluation of multifunctional fiber of Lyocellike PET

The Lyocellike PET multifunctional master batch and the general polyester master batch having a functional material content of 50 wt% prepared in the above examples were mixed at a weight ratio of 1: 9, and then 75 Denier, 72 Filament In circular cross-linked polyethylene terephthalate (PET) multifunctional fiber.

* Functional evaluation

1. Evaluation of ultraviolet barrier property

The fabrics were prepared from the lyocellike PET multifunctional fibers prepared above, and the ultraviolet blocking rates were measured and are shown in Table 5.

- Measuring instrument: UV-VIS-NIR SPECTROPHOTOMER

- Wavelength range: UV-R: (290-400 nm)

             UV-A: (315-400 nm)

             UV-B: (290-315 nm)

- wavelength interval: 5 nm

UV-rays Blocking rate (%) UV (UV-R) 97.1 Ultraviolet (UV-A) 94.5 Ultraviolet (UV-B) 96.2

As shown in Table 5, the fabrics made of the multifunctional fibers of the present invention showed a UV blocking ratio of 90% or more at all wavelengths, and thus the ultraviolet blocking property was excellent.

2. Evaluation of antimicrobial activity

The antimicrobial activity of the fabric was measured after preparing the fabric with the above-prepared Lyocellike PET multifunctional fiber.

The antimicrobial activity was evaluated by measuring the number of bacteria / Ml and the reduction rate of bacteria.

Staphylococcus aureus Initial number of bacteria 2.0 x 10 ⁴ After 18 hours 2.9 x 10 ³ Bacteriostatic reduction rate 99.9% Pneumococcus Initial number of bacteria 2.2 x 10 ⁴ After 18 hours 2.2 x 10 ³ Bacteriostatic reduction rate 99.9%

As shown in Table 6, it can be seen that the fabric prepared from the Lyocellike PET multifunctional fiber of the present invention has a high antibacterial activity with a reduction ratio of Staphylococcus aureus and Pneumococcus bacteria of 99.9%.

3. Deodorization Evaluation

The fabrics were prepared from the Lyocellike PET multifunctional fibers prepared above and deodorizability was measured and shown in Table 7

The deodorization property was measured by gas detection method.

- Sample amount: 5.0 g

- Test gas: ammonia (NH3)

- Concentration of injected test gas: 500

- Volume of container: 1000 / / mL

- Test environment: temperature 21 캜, humidity 64% R.H.

division 30 minutes 60 minutes 90 minutes 120 minutes Deodorization rate (%) 70 74 80 82

As shown in Table 7, it can be seen that the fabrics made from the Lyocellike PET multifunctional fibers according to the present invention have a high deodorization rate as the deodorization rate increases over time and thus the deodorization property is excellent.

Claims (7)

1. A method for manufacturing a multifunctional master batch of Lyocellike PET manufactured through an extruder divided into a first section, a second section, a third section, a fourth section and a fifth section,
Wherein the first section is a melting step of putting a general polyester master batch and passing the polyester master batch through a passing time of 8 to 15 seconds while heating at 100 to 150 DEG C to melt the polyester;
A BBOT feeding step in which BBOT (2,5-bis- (5-t-butylbenzoxazolyl) thiophene) is fed in the second section and is passed at a passage time of 3 to 6 seconds while being heated to 150 to 200 ° C;
Barium sulphate and tourmaline in which barium sulphate (BaSO ₄ ) and tourmaline are introduced in the third section and which is passed through at a passage time of 2 to 4 seconds while being heated to 200 to 240 ° C;
The fourth section is heated at a temperature of 240 to 270 DEG C for 1 to 3 seconds; And
And an extrusion step of extruding functional materials of barium sulfate, tourmaline and polyester containing BBOT while heating at 270 to 290 ° C in the fifth section,
Wherein the barium sulfate and tourmaline are contained at a mixing ratio of 1.0: 0.8 to 1.2, and the BBOT is contained at 2 to 8 phr of the masterbatch. The method according to claim 1,
Wherein the functional material is contained in an amount of 40 wt% or more. The method according to claim 1,
Wherein the functional material is contained in an amount of 40 to 55 wt%. delete A Lyocellike PET multifunctional master batch produced by the process of any one of claims 1 to 3. 7. A Lyocellike PET multifunctional fiber, characterized in that it is formed using said Lyocellike PET multifunctional masterbatch of claim 5. The method according to claim 6,
Characterized in that said Lyocellike PET multifunctional fiber contains 4 to 6 wt% of barium sulfate, 4 to 6 wt% of tourmaline and 0.03 to 0.5 wt% of BBOT.

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