KR20030040587A - Method for producing functional polyester fiber - Google Patents

Abstract

PURPOSE: A manufacturing method of functional polyester fiber which is characterized by radiating far infrared rays and having excellent storage effect, antibiosis and deodorizing effect is provided. The functional polyester fiber is useful for underclothes, outer garments, socks, stockings and bedclothes. CONSTITUTION: Functional polyester fiber is obtained by the steps of: mixing 0.3-10% of mica such as sericite particles, illite particles or a mixture thereof based on the total weight of a polyester and 5-30% of silver type inorganic antibacterial agent particles based on the mica; grinding the mixture by a water system and an ethylene glycol system sequentially to manufacture an ethylene glycol slurry; and adding the ethylene glycol slurry while polymerizing a polyester.

Description

Method for producing functional polyester fiber {Method for producing functional polyester fiber}

The present invention relates to a polyester fiber, and more particularly, to a method for producing a functional polyester fiber containing a mica mineral, Sriteite, Illite, or a mixture thereof and a silver-based inorganic antibacterial agent.

Polyester fiber is one of the representative synthetic fibers that are used in various fields such as clothing, industrial materials and medical care because it has a variety of excellent properties and advantages.

Moreover, in recent years, as part of efforts to eliminate the disadvantages of polyesters and highlight new advantages, many studies have been carried out, such as changing and modifying existing components of polyester composites with other special ingredients or adding special additives. have.

Among them, in recent years, attempts have been made to add polyester special natural minerals to polyester fibers.

Especially in textile products for clothing, bacteria and microorganisms are propagated by sweat and other organic substances such as fats and proteins, and these microorganisms can decompose organic substances and cause odor or skin diseases by physical contact. do.

Accordingly, Japanese Patent Application Laid-Open No. 59-134418, Japanese Patent Application Laid-Open No. 61-17567, Korean Patent Publication No. 95-018915, etc., prepare a liquid composition by mixing a ceramic antimicrobial agent with a polyurethane resin and a surfactant, and then The technique of spraying on the surface of the ester fiber and the inorganic ceramic particles to adhere to the surface has been introduced, but the polyester fiber product produced in this way has the disadvantage that the functionality is not permanent due to the problem of washing resistance.

In addition, in order to alleviate such disadvantages, a method of dispersing an inorganic zeolite substituted with antimicrobial metal in a fiber by using a master batch method or using a ceramic is disclosed in Japanese Patent Application Laid-Open No. 61-234390. , Japanese Patent Application Laid-Open No. 62-101643, but this technique can improve the washing resistance of functional textile products, but due to the hygroscopic zeolite, there is a problem of frequent trimming and discoloration of the textile products during melt spinning. In the dyeing process leads to poor dyeing, there are many problems in the actual fiberization.

In addition, Korean Patent Publication No. 98-033453 discloses a method for adding microparticles and antimicrobial powders before vacuum operation of a polyester polymerization reaction to produce polyester fibers having antibacterial and deodorizing functions. In the case of the normal polyester polymerization process, the inorganic materials are aggregated to cause pack pressure increase and trimming of the spinning process, and thus, there is a disadvantage in that the production processability is bad.

On the other hand, in order to make up for the shortcomings, Korean Patent Publication No. 98-033438 discloses a masterbatch containing low-melting polyester particles having a particle size of 0.2-1 μm and particles having a particle size of 0.5 μm or less, which are 60% or more of all of the elvan particles. The method of mixing and spinning chips and general polyester chips is also introduced. This method improves the spinning workability of functional polyester fibers, but due to the high hardness of elvan mineral particles, there is a problem in processing during spinning or spinning, resulting in work production efficiency. There is a disadvantage of falling or falling of physical properties due to the uneven strength of the elongation.

In general, ores added to the polyester to improve the functionality of the polyester include mica, hornblende, alum, loess and the like. Among them, mica ore, called sericite or illite, is known to have the best performance.

The mica has a three-layered laminar structure, and when absorbed, the side-to-side spacing extends to about 1.8Å, and because of the charge of (-) 2, it causes coagulation precipitation by floating neutralization of cations in water and electrical neutralization. It improves turbidity and has a high moisturizing effect due to its own water function, prevents direct sunlight, and has high activity.It emits more than 80% of far infrared rays with a wavelength of 5 to 25 microns at room temperature and generates dissolved acidity to generate double adsorption and far infrared radiation. It has the advantage of excellent deodorizing ability.

Sericite or illite is very excellent in far-infrared emission, antibacterial, heat storage, deodorizing and the like. However, in addition to these advantages, there is also a disadvantage that it is difficult to grind to less than 1㎛ suitable for use in fibers. In other words, the mica mineral has a three-layered scaly structure of mineralogy, but has a disadvantage in that crushing between layers is easy, but crushing of mica on a hexagonal plate is not easy.

Mica ore has a hardness of 1 ~ 2, which is softer than other ores, so it is not easy to crush into fine particles, and it is easy to reaggregate after crushing. Although a method of pulverizing and then pulverizing using a jet mill is known, there is a fatal disadvantage that re-agglomeration occurs during the polymerization process when the mica prepared in this way is directly added to the polymerization process. In addition, when directly dispersed and dispersed in ethylene glycol so as to be added in the slurry state during the polymerization process, the viscosity of ethylene glycol is high, so that high heat occurs in the milling machine during the milling process, so that mica minerals cannot be crushed to 1 μm or less.

Accordingly, the present invention can produce functions such as far-infrared emission, heat storage, antimicrobial activity, deodorization, etc. in producing functional fiber products, without problems in production processability such as washing resistance, spinning processability and processing processability. It is an object of the present invention to provide a process for producing functional polyester fibers.

In the present invention, the mica mineral Sericite particles, illite particles or mixture particles thereof are 0.3-10% of the total weight of the polyester, and the silver-based inorganic antimicrobial particles are 5-30% of the total weight of the mica mineral. Method of producing a functional polyester fiber, characterized in that to prepare a glycol slurry by pulverizing in the first water-based grinding step and the second ethylene glycol-based grinding step, and to add the prepared slurry during the polyester polymerization process. To provide.

In addition, the present invention provides a method for producing a functional polyester fiber, characterized in that the average particle size of the mica mineral and the silver-based inorganic antibacterial agent in the ethylene glycol slurry prepared above.

The present invention also provides a functional fiber product containing the functional polyester fiber produced by the above method.

Hereinafter, the present invention will be described in more detail.

The present invention is a polyester polymerization process in the form of a glycol slurry of mica minerals sericite, illite or mixtures thereof and silver inorganic antibacterial agents in order to impart permanent far-infrared emission and antibacterial and deodorant functionality to conventional polyester fibers. It is characterized by adding in the.

The mica minerals include illite, sericite, gold mica, dolomite, biotite, and double sericite is known to have the highest purity. It is a fine mica-like natural mineral that expresses a function such as sex and belongs to a monoclinic system, and its chemical composition is (K, H ₃ O) (Al, Mg, Fe) ₂ (Si, Al) ₄ O ₁₀ [(OH) ₂ , (H ₂ O)], which is very complicated. Main components include silica (SiO ₂ ) 45 ~ 80%, alumina (Al ₂ O ₃ ) 20-40%, potassium oxide (K ₂ O) 5-15%, ferric oxide (Fe ₂ O ₃ ) 0.7-4% Hardness is 1-2 and specific gravity is 2.6-2.9.

In addition, the present invention is characterized by adding a small amount of silver-based inorganic antimicrobial agent to mica minerals in order to maximize the function of antimicrobial properties,

The silver inorganic antimicrobial agent is an inorganic antimicrobial agent that combines silver (Ag), zinc (Zn), etc., which are metal ions having antibacterial activity, with zeolite, which is an inorganic ceramic material, as a carrier. 5-30% is suitable for the functional expression of this invention.

In addition, in the present invention, in order to apply the mica mineral and the silver-based inorganic antimicrobial agent to the polyester fiber, the particle size is preferably 1 μm or less,

The average particle size of the raw mica mineral powder used for synthetic fibers is about 9.4 μm, and the maximum particle size is about 76.4 μm, which is not suitable as an additive for producing synthetic fibers.

Therefore, the present invention is characterized in that it comprises a first water-based grinding process and a second ethylene glycol-based grinding process in order to produce mica minerals and silver-based inorganic antimicrobial agent having a particle size of 1 ㎛ or less suitable as an additive for the production of synthetic fibers, detailed process Is as below.

First, the mica mineral powder is first pulverized in a water-based state with a steel ball mill having a diameter of 0.1 to 1 μm and dried. Particles having a particle size of 1 µm or more among the pulverized and dried inorganic minerals are separated and regrind using a 1 µm mesh filter to maintain 99.9% and 1 µm or less of a ground powder slurry.

After the first grinding process, the ground powder slurry is dried and subjected to the second grinding process.

In the secondary process, it is preferable to disperse the pulverized powder slurry in ethylene glycol in order to directly add the pulverized powder slurry in the polyester polymerization process, and further, by pulverizing the powder which has reaggregated during the drying process with a forced ball mill to prepare a mica mineral ethylene glycol slurry. do.

The prepared mica mineral ethylene glycol slurry has an average particle diameter of about 0.29 μm and particles having a size of 1 μm or more are suitable for adding to about 1 to 2% of polyester fiber.

In addition, the present invention comprises the step of preparing a silver inorganic inorganic antimicrobial ethylene glycol slurry having a particle size of 1㎛ or less together with the mica mineral ethylene glycol slurry of 1㎛ or less in the step of polymerization in the polymerization step of a conventional polyester. The sericite or illite and the silver-based inorganic antimicrobial agent are characterized in that they do not have mutual cohesion, so they may be separately prepared and added, or may be simultaneously prepared in a mixed state.

In the present invention, the step of injecting the additive slurry in the polymerization step of the polyester may be added immediately before the mixing step of terephthalic acid and ethylene glycol, or just before the polycondensation process in which the ester reaction is completed. It is preferable to add just before starting the decompression step of the summation step.

In the present invention, the polyester polymer is prepared by a conventional polyester polymerization process, antimony trioxide and phosphoric acid can be used as a polymerization catalyst and a heat stabilizer, respectively, the reaction temperature and melt viscosity of 285 ℃ at 3000 ~ 3500poise at 100rad / s It can superpose | polymerize with phosphorus polymerization degree.

The polyester resin polymerized by the above method is fiberized by a conventional spinning process.

In the present invention, the amount of mica minerals should not exceed 10% of the total weight of the polyester. If this content is exceeded, the fairness during spinning becomes very poor and only a few hours of production is difficult. On the other hand, when the content of mica minerals is less than 0.3%, the content of mica minerals is so small that it is difficult to substantially see the effect of functional improvement. Therefore, the content of the mica mineral to be added should be 0.3 to 10% based on the total weight of the polyester, preferably 0.5 to 4.0%.

In addition, in the present invention, the amount of the silver-based inorganic antimicrobial agent is preferably 5 to 50% of the total weight of the mica mineral. When the amount is less than 5%, the antimicrobial activity of the polyester fiber is not sufficiently exhibited, and when the amount exceeds 50%, the cost is increased. This is because the addition of excessive inorganic particles decreases yarn workability such as poor yarn dyeing and increase in pack pressure during spinning. More preferably, 10 to 30% of the total weight of the mica mineral is added.

Features and other advantages of the present invention as described above will become more apparent from the following examples. However, the present invention is not limited to the following examples.

Physical properties of the following examples are measured by the following method.

* Particle size distribution: measured using Coulter's LS particle size analyzer (Coulter, LS Particle Size Analyzer).

* Far infrared ray emission: Requested by Korea Institute of Construction Materials.

* Pack pressure change: The pressure of the powder filter applied during the spinning process is measured as a change rate over time. (Unit: pressure change per day, Kg / ㎠ / day)

* Initial tensile strength: The filament made of 75 denia is measured by a conventional method using an elongation measuring instrument.

* Antimicrobiality: Measured by the Keske 0693 (KS K 0693) method.

* Regenerative property: Fabrics were prepared in plain weave using the fibers prepared in Examples and Comparative Examples and dyed to white using disperse dyes to prepare comparative fabrics and measured by comparing polyesters (measurement fabrics). . The measuring method was as follows. Two thermostats set at 50 ° C. in a 10 ° C. thermostat were placed and covered with measuring fabric and comparative fabric, respectively, and held for 60 minutes. Then, 10 minutes after removing the heating element, the inside of each fabric was measured. And by comparing each measured temperature, the value of subtracting the temperature of the comparison fabric from the temperature of the measurement fabric was expressed as a representative value of the heat storage property.

Example 1

Serisite raw powder (Nextex, Gyeongju, Korea) with an average particle size of about 9.4 µm and a maximum particle diameter of about 76.4 µm and inorganic antibacterial agent, which is 15% of silver zeolite based on the weight of raw powder of Serisite, Inc. The inorganic additive prepared by mixing the raw material and the unikiller was subjected to the first aqueous grinding process and the second ethylene glycol based grinding process, and the average particle size of the inorganic additive in the slurry was 0.29 μm. The particles having a size of at least μm were prepared to be less than 1%.

The prepared ethylene glycol slurry was added immediately before the depressurization process of the polyester polycondensation reaction. The content of the added inorganic additive was 2% of the total polyester resin weight. In the polyester polymerization process in which the inorganic additive is added, the polymer is polymerized to a melt viscosity of 3,200 poise at a temperature of 285 ° C., chipped, and dried at 140 ° C. for 8 hours. The dried polyester was fibrous at 290 ° C. at a rate of 3,500 m / min so that the fibers had a fineness of 75 denier and the number of constituent filaments being 24 strands.

Example 2

It was the same as in Example 1 except that the content of the inorganic additives was polymerized to 4% of the total polyester resin weight.

Example 3

It was the same as in Example 1 except that the content of the inorganic additive was polymerized to 0.5% of the total polyester resin weight.

Comparative Example 1

Polyester fibers were made using normal polyester semi-dull chips without the addition of inorganic additives.

Comparative Example 2

It was the same as in Example 1 except that the content of the inorganic additives was polymerized to 0.3% of the total polyester resin weight.

Comparative Example 3

The content of the inorganic additive was the same as in Example 1 except that the polymerization was carried out to 10% of the total polyester resin weight.

[Comparative Example 4]

The content of the inorganic additive was adjusted to 2% of the total polyester resin weight, except that the raw powder was directly added to the polymerization process without using the pulverized and dispersed ethylene glycol slurry.

The content and other physical properties of the inorganic additives obtained in the above Examples and Comparative Examples are shown in Table 1. In the case of Comparative Example 4, the yarn manufacturing processability was so poor that yarn production could not be made and the functional evaluation could not be performed.

division Example Comparative example One 2 3 One 2 3 4 Inorganic additives (wt% per polyester) 2.0 4.0 0.5 0.0 0.3 10.0 2.0 Average particle size (㎛) 0.29 0.29 0.29 - 0.29 0.29 9.40 Melt viscosity 3,000 2,700 3,200 3,400 3,300 2,400 3,100 Strength (g / d) 4.1 4.0 4.2 4.2 4.1 3.5 - Elongation (%) 40.0 36.8 37.2 39.0 38.6 37.8 - Pack pressure (kg / ㎠ / day) 2.4 2.8 1.8 1.0 1.4 18.2 - % Reduction 99.9 99.9 99.6 0.0 89.2 99.9 - Heat storage (℃) 4.0 4.5 3.0 0.0 1.5 4.5 - Far infrared ray radioactivity (%) 88.9 88.9 88.7 88.3 88.5 88.9 - Deodorization rate (%) 45.1 45.2 40.2 0.0 29.3 45.1 -

The polyester fiber produced by the present invention has excellent far-infrared emission, heat storage, antibacterial and deodorizing properties, and also has excellent fiber manufacturing processability, and its use and application field have been significantly expanded. Products made using the fibers of the present invention are not only excellent in heat retention and fit, but are also beneficial to health. Its main uses include underwear, outerwear, socks, stockings and cotton for duvets.

Claims (3)

Serisite particles, illite particles, or mixtures thereof, which are mica minerals, are 0.3-10% of the total weight of the polyester, and the silver-based inorganic antimicrobial particles are 5-30% of the total weight of the mica minerals. And secondly, milling in an ethylene glycol-based grinding step to produce an ethylene glycol slurry, and adding the prepared slurry during a polyester polymerization step to produce the functional polyester fiber. The method for producing a functional polyester fiber according to claim 1, wherein the average particle size of the mica mineral and the silver inorganic antibacterial agent in the prepared ethylene glycol slurry is 1 µm or less. A functional fiber product containing the functional polyester fiber produced by the method of claim 1.