KR20220076117A - Water-soluble Polyester Split Short Fiber - Google Patents

Abstract

In the present invention, the synthetic resin constituting the microfiber and the eluted water-soluble polyester resin are formed into split short fibers, wherein the synthetic resin is any one or two or more of polypropylene, polyethylene, polyester, and polybutylene terephthalate, and the water-soluble poly The ester resin is a polymer of acids including terephthalic acid, isophthalic acid, and dimethyl 5-sodiosulfo isophthalate, and diols including ethylene glycol, diethylene glycol, neopentyl glycol, and polyethylene glycol, which are esterified during polymerization. It relates to a water-soluble polyester-based split short fiber additionally mixed with bis-β-hydroxyethyl terephthalate (BHET) for the reaction.

Description

Water-soluble Polyester Split Short Fiber

The present invention relates to a water-soluble polyester-based split staple fiber, and more particularly, a water-soluble polyester capable of producing a split fiber having a split cross-section by composite spinning two different polymers and splitting the fiber by an elution method It relates to a system split short fiber.

In general, water-soluble polyester is applied in various fields such as fibers, adhesives, and biodegradable materials. In particular, in the textile field, it is sometimes used as a raw material for manufacturing microfibers.

As a method for producing such water-soluble polyester, 5-sodium sulfoisophthalic acid and its derivatives are used to have sodium sulfonate salt in the polyester molecular chain to make it water-soluble, or after reacting dicarboxylic acid with a glycol component, A method is known in which a carboxyl group is introduced into the terminal and molecular chain by reacting again with melittic anhydride, and then a salt is formed with an alkali component such as ammonia and amines to make it water-soluble.

Specifically, in Korean Patent Laid-Open Publication No. 1994-14494, "In a water-soluble polyester resin composition obtained by reacting a glycol component with a dicarboxylic acid, dicarboxylic acid 1 is added to an ester oligomer prepared by reacting a glycol component with the dicarboxylic acid. It is prepared by adding butyltetracarboxylic acid alone or a mixture with trimellitic anhydride in a molar ratio of 3 to 10 per mole, and has a viscosity of 0.15 to 0.8 dl/g and an acid value of 40 to 100 mg/g. A water-soluble polyester resin composition" is proposed.

In addition, International Patent Publication WO2002/57334 discloses "a) preparing an aqueous or methanolic slurry comprising 1,4-cyclohexanedimethylol (CHDM) and dicarboxylic acid, and maintaining the slurry at a temperature below the melting point of CHDM. , b) feeding the slurry to the reactor, c) esterifying the slurry at a temperature and pressure sufficient to effect the esterification, optionally in the presence of a suitable catalyst, d) forming a prepolymer, and e) polycondensation of a prepolymer in the presence of a suitable catalyst at a temperature and pressure sufficient to carry out polycondensation to form a polyester." suggesting a way

In the disclosed technology, adding CHDM is to increase Tg, but it does not substantially affect Tg, and there is a problem in that the weight reduction rate is reduced when weight reduction processing is performed.

In addition, in the case of the existing dissolution type resin, since NaOH is used as a solvent, it undergoes processes such as elution, water washing, boiling water washing, and acid washing, resulting in an increase in process time and environmental problems due to wastewater treatment.

Therefore, it is possible to develop a polyester-based resin that can be eluted only with water, thereby reducing process time and improving environmental problems compared to conventional leaching-type resins using NaOH.

In order to solve the above problems, the present invention is a polyester-based split staple fiber using a water-soluble polyester that can express water solubility even after removing the components included to express water solubility in the prior art such as CHDM or amine groups is to provide

In the present invention, the synthetic resin constituting the microfiber and the eluted water-soluble polyester resin are formed into split short fibers, wherein the synthetic resin is any one or two or more of polypropylene, polyethylene, polyester, and polybutylene terephthalate, and the water-soluble poly The ester resin is a polymer of acids including terephthalic acid, isophthalic acid, and dimethyl 5-sodiosulfo isophthalate, and diols including ethylene glycol, diethylene glycol, neopentyl glycol, and polyethylene glycol, which are esterified during polymerization. Provided is a water-soluble polyester-based split staple fiber additionally mixed with bis-β-hydroxyethyl terephthalate (BHET) for the reaction.

In addition, the split staple fiber of the present invention is a water-soluble polyester-based split staple fiber, characterized in that it is composed of 20 to 80% by weight of synthetic resin and 80 to 20% by weight of water-soluble polyester resin. provides

In addition, the present invention provides a water-soluble polyester-based split staple fiber characterized in that the intrinsic viscosity (IV) of the polyester resin among the synthetic resins is 0.55 to 0.64 dl/g.

In addition, the acid of the present invention is a water-soluble polyester-based split short fiber characterized in that it is composed of a mixture of 80-10 mol% of terephthalic acid, 80-10 mol% of isophthalic acid, and 20-1 mol% of dimethyl 5-sodiosulfo-isophthalate provides

In addition, the present invention is a water-soluble polyester-based division characterized in that it is composed of a mixture of 80 to 10 mol% of ethylene glycol, 80 to 1 mol% of diethylene glycol, 80 to 1 mol% of neopentyl glycol, and 20 to 1 mol% of polyethylene glycol. Provides short fibers.

In addition, the present invention provides a water-soluble polyester-based split short fiber characterized in that at least one additive selected from the group consisting of a reaction catalyst, an antifoaming agent, an antioxidant, and a heat stabilizer during polymerization of the polymer is included.

In order to express the water solubility of the resin, the polyester-based split staple fiber of the present invention uses a water-soluble polyester that expresses water solubility without separate components such as CHDM or amine groups. .

1 is a view showing the fiber cross-section before the water-soluble polyester of the water-soluble polyester split short fibers according to the present invention is eluted.

Hereinafter, preferred embodiments of the present invention will be described in detail. First, in describing the present invention, detailed descriptions of related known functions or configurations are omitted so as not to obscure the gist of the present invention.

As used herein, the terms 'about', 'substantially' and the like are used in a sense at or close to the numerical value when the manufacturing and material tolerances inherent in the stated meaning are presented, and serve to enhance the understanding of the present invention. To help, precise or absolute figures are used to prevent unfair use by unconscionable infringers of the stated disclosure.

The present invention relates to a split short fiber, characterized in that it is composed of two components: a synthetic resin constituting the microfiber and a water-soluble polyester resin that is eluted.

The synthetic resin is any one or two or more of polypropylene, polyethylene, polyester, and polybutylene terephthalate, and it is preferable to use polyester having an intrinsic viscosity (IV) of 0.55 to 0.64 dl/g.

If the intrinsic viscosity (IV) is less than 0.55 dl/g, poor cross-sectional formability and deterioration of physical properties may occur due to the difference in viscosity with the water-soluble polyester resin. It can be difficult to form a divided cross section.

The water-soluble polyester resin is characterized in that it is composed of a polymer of acids including terephthalic acid, isophthalic acid, and dimethyl 5-sodiosulfo isophthalate, and diols containing ethylene glycol, diethylene glycol, neopentyl glycol, and polyethylene glycol. There is this.

As for the split short fiber, it is preferable that the synthetic resin constituting the microfiber is divided into four or more as shown in FIGS. 1 (a) and (b).

When the synthetic resin constituting the split short fibers is divided into less than four, the fineness of the microfibers may be high and the tactile feel may be reduced.

If the number of the synthetic resins constituting the split short fibers is more than 20, it is preferable to form less than 20 because it is difficult for the eluate to penetrate in the splitting process, so that the splitting process may not be performed smoothly.

The synthetic resin constituting the split short fibers may use any one of polypropylene, polyethylene, polyester, and polybutylene terephthalate, or the microfibers divided using two or more synthetic resins may form different types of synthetic resins. will be.

Next, the water-soluble polyester resin constituting the split short fibers is composed of polymers of acids and diols.

Examples of the acid include, but are not limited to, terephthalic acid (TPA), isophthalic acid (IPA), and dimethyl 5-sodiosulfo isophthalate (DMS, Dimethyl 5-sodiosulfo Isophthalate).

At this time , 80 to 10 mol% of terephthalic acid, 80 to 10 mol% of isophthalic acid, and 20 to 1 mol% of dimethyl 5-sodiosulfo isophthalate may constitute acids.

In addition, diols may include, but are not limited to, ethylene glycol (EG), diethylene glycol (DEG), neopentyl glycol, and polyethylene glycol (PEG).

As diols, it may be composed of a mixture of 80 to 10 mol% of ethylene glycol, 80 to 1 mol% of diethylene glycol, 80 to 1 mol% of neopentyl glycol, and 20 to 1 mol% of polyethylene glycol .

The content of neopentyl glycol is 1 to 80 mol% based on the glycol component of all diols. The amount of neopentyl glycol used is an amount corresponding to the desired mole % of neopentyl glycol in the final polymer. Here, when the content of neopentyl glycol is less than 1 mol%, it is difficult to prevent moldability defects due to crystallization of the polyester resin, and when it exceeds 80 mol%, there is a problem in that the polymerization reaction is slowed down.

As an example of preparing the polymer of the present invention, first, the dimethyl 5-sodiosulfo isophthalate and ethylene glycol are mixed in a ratio of 1:8 to 1:12 to initiate polymerization. When the reaction catalyst may be added in a ratio of about 0.1 to 0.5% by weight to the total polymer.

When the polymerization is initiated, bis-β-hydroxyethyl terephthalate (BHET) may be additionally mixed for the esterification reaction. In addition, the esterification reaction may be performed by reacting the polymer with terephthalic acid, isophthalic acid, and dimethyl glycol.

At this time, the mixing ratio of terephthalic acid and dimethyl glycol may be about 1:1 to 1:1.5, and the mixing ratio of isophthalic acid and dimethyl glycol may be 1:1 to 1:1.5.

Thereafter, polyethylene glycol may be added for condensation polymerization, and the polyethylene glycol preferably has a number average molecular weight of 300 to 2,000, and the amount may be included in an amount of 5 to 10% by weight of the polymer.

Thereafter, optionally, one or more additives selected from the group consisting of a reaction catalyst, an antifoaming agent, an antioxidant, and a heat stabilizer may be further included. At this time, the antifoaming agent may be included in 0.01 to 0.05 wt% of the polymer, the antioxidant may be included in 500 to 800 ppm in the polymer, and the heat stabilizer may be included in 100 to 500 ppm in the polymer.

The split short fibers of the present invention may be composed of 20 to 80% by weight of synthetic resin, 80 to 20% by weight of water-soluble polyester resin, preferably 70 to 80% by weight of synthetic resin, and 30 to 20% by weight of water-soluble polyester resin.

The water-soluble polyester-based split staple fiber according to the present invention as described above can be produced by a general split staple fiber manufacturing process, and the prepared split staple fiber can be formed into microfibers by dissolving polyester in a solution composed of water.

In general, the spinning speed is set at 500~1500 m/min for winding. If the spinning speed is higher than 1500 m/min, there is a high probability that one or more filaments will be momentarily broken irregularly, and only one component, not two, is spun due to poor cross-section. The paper may be manufactured in the form of single yarns.

The spinning temperature is preferably set within 275 °C to 295 °C. If it is less than 275 ℃, there is a problem with the flow of the polymer, so the icicle-shaped surface has a high efficiency at which irregular fibers are spun. On the other hand, if it exceeds 295 ℃, the polymer ejected from the nozzle adheres to the nozzle surface.

If a general emulsion is used, the water-soluble resin exposed on the surface of the yarn reacts with moisture, resulting in poor maritime properties, so an emulsion containing a Si component that can prevent moisture penetration can be selected as the spinning emulsion.

Hereinafter, examples of a method for producing a water-soluble polyester-based split staple fiber according to the present invention are shown, but the present invention is not limited to the examples.

<Examples and Comparative Examples>

Example One

(1) Synthesis of water-soluble polyester resin

Dimethyl 5-sodiosulfo isophthalate and ethylene glycol were added to initiate the reaction, and bis-β-hydroxyethyl terephthalate, terephthalic acid, isophthalic acid, and diethylene glycol were added to initiate the esterification reaction.

At this time, dimethyl 5-sodiosulfo isophthalate had a molecular weight of about 300 and was added at 10 mol% of the total acid, terephthalic acid had a molecular weight of about 150 and was added at 60 mol% of the total acid, and isophthalic acid had a molecular weight of about 150 As a result, the total amount of acid was added at 30 mol%.

In addition, ethylene glycol had a molecular weight of 60 and 40 mol% based on diols, and diethylene glycol had a molecular weight of 110 and 50 mol% was added with 5 mol% of neopentyl glycol and 5 mol% of polyethylene glycol.

After that, an antifoaming agent, an antioxidant, and a heat stabilizer were added while polyethylene glycol was added for condensation polymerization. The polyethylene glycol had a molecular weight of 300 and accounted for 7% by weight of the total polymer, and other antifoaming agents were added at 0.02% by weight, antioxidants at 500ppm, and heat stabilizers at 200ppm.

(2) Manufacture of split short fibers

9-split yarn was spun by applying 30w% of water-soluble polyester resin (component 1) and 70w% of polyester having an intrinsic viscosity (IV) of 0.55 dl/g among synthetic resins (component 2).

The spinning speed is set to 1,100 m/min, and the spinning temperature is set to 275°C, and a silicone emulsion is used and the coil is wound in the form of undrawn yarn.

Microfibers were prepared by eluting the wound undrawn yarn with hot water during the stretching process.

Comparative Example 1

In Example 1, a synthetic resin was used as nylon (RV 3.0), a non-silicone emulsion was used, and a general post-process elution process was applied.

Comparative Example 2

The same as in Example 1, except that a non-silicone oil was used as the oil agent.

<Elution conditions>

In the example, the water drawing method was applied during the drawing process of the undrawn yarn, and the hot water temperature was set to 80° C. and eluted during the drawing process.

Comparative Example 1 was subjected to alkali elution (NaoH 95 ℃ 40 min), water washing, hot water washing (70 ℃ 5 min), acid washing (60 ℃ 10 min), and water washing.

division Example 1 Comparative Example 1 Comparative Example 2 ingredient 1 Ingredients, wt% water soluble, 30 nylon, 30 water soluble, 30 ingredient 2 SD, 70 SD, 70 SD, 70 spinning emulsion Si emulsion Non-Si emulsion Non-Si emulsion Radiation Fairness Good Good error stretching temperature 80 30 30 section yarn

after dissolution

- dissolution Water (Ton) 0 19.38 - Steam (Ton) 0 1.29 - Electricity (kW) 0 59 - NaOH 0% 10 g/l - Saving effect (based on 200kg amount) \92,755/LOT standard -

Table 1 shows the cross-sections after dissolution of Examples and Comparative Examples. In Example, it can be confirmed that the water-soluble polyester resin is all eluted under the dissolution conditions in the table, and the remaining synthetic resin progresses to microfibers, but Comparative Example 1 is a nylon alkali eluted microfiber. It can be seen that water, steam, and electric capacity used for elution with the furnace are used more than in the example. In addition, Comparative Example 2 uses a non-silicone emulsion as a spinning emulsion, and has poor dismantling properties, resulting in a problem in spinning fairness.

The present invention described above is not limited by the above-described embodiments and the accompanying drawings, and it is common in the technical field to which the present invention pertains that various substitutions, modifications, and changes are possible without departing from the technical spirit of the present invention. It will be clear to those who have the knowledge of

100: synthetic resin 200: water-soluble polyester

Claims (6)

The synthetic resin constituting the microfiber and the eluted water-soluble polyester resin are formed into split short fibers,
The synthetic resin is any one or two or more of polypropylene, polyethylene, polyester, and polybutylene terephthalate,
The water-soluble polyester resin is a polymer of acids including terephthalic acid, isophthalic acid, and dimethyl 5-sodiosulfo isophthalate, and diols including ethylene glycol, diethylene glycol, neopentyl glycol, and polyethylene glycol,
Water-soluble polyester-based split short fibers additionally mixed with bis-β-hydroxyethyl terephthalate (BHET) for esterification during polymerization .
According to claim 1,
The split short fibers are water-soluble polyester-based split staple fibers, characterized in that it is composed of 20 to 80% by weight of synthetic resin and 80 to 20% by weight of water-soluble polyester resin.
According to claim 1,
Water-soluble polyester-based split short fibers, characterized in that the intrinsic viscosity (IV) of the polyester resin among the synthetic resins is 0.55 to 0.64 dl/g.
In claim 1,
The acid is 80 to 10 mol% of terephthalic acid, 80 to 10 mol% of isophthalic acid, and 20 to 1 mol% of dimethyl 5-sodiosulfo-isophthalate.
In claim 1,
Water-soluble polyester-based split short fibers, characterized in that the mixture is 80 to 10 mol% of ethylene glycol, 80 to 1 mol% of diethylene glycol, 80 to 1 mol% of neopentyl glycol, and 20 to 1 mol% of polyethylene glycol .
In claim 1,
A water-soluble polyester-based split staple fiber characterized in that at least one additive selected from the group consisting of a reaction catalyst, an antifoaming agent, an antioxidant, and a heat stabilizer is included during polymerization of the polymer.

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