KR20170131060A - Differential Shrinkage Flame Retardant Composite Yarn Using High Shrinkage Flame Retardant Polymer And Preparation Thereof - Google Patents

Abstract

The present invention relates to different shrinkage flame retardant composite yarn using a high shrinkage flame retardant polymer. The present invention is composite yarn manufactured by overfeed and heat treatment by using: core yarn which is produced by using a high shrinkage polyester to which 5-10 mol% of isophthalic acid compared to terephthalic acid and 1-5 mol% of diethylene glycol compared to ethylene glycol are added during polymerization; and effective yarn which is produced by using general polyester. In the core yarn, added isophthalic acid reduces the volume of the crystalline region of polyester; a contraction ratio is improved by 10-20% than the effect yarn since the diethylene glycol increases the volume of the amorphous region of the polyester and reduces the volume of the crystalline region; 5000-7000 ppm of phosphorus-based flame retardant is included respectively in the core yarn and the composite yarn; and a limit oxygen index is 30 or more.

Description

TECHNICAL FIELD The present invention relates to a shrinkable flame retardant composite yarn using a high shrinkage flame retardant polymer and a method for producing the same.

The present invention relates to a shrinkage-retardant composite yarn using the high shrinkage flame retardant polymer, and more particularly, to a shrinkage-retardant composite yarn using a core yarn of a high shrinkage flame retardant polymer and an effect yarn of a flame retardant polymer containing the flame retardant, This composite shrinkage-retarding composite yarn using a high shrinkage flame retardant polymer excellent in bulkiness.

In industrial textile and interior products, flame retardancy is recognized as one of the most basic performance requirements. The technique of expressing such flame retardancy to fiber is generally classified into a post-processing method in which a flame retardant is treated on the surface of a fabric through a post-processing in the state of a woven or knitted fabric and a method in which a fiber produced by adding or copolymerizing a large amount of a flame retardant compound to exhibit permanent flame retardancy It can be classified into a flame-retardant fiber production method by a mixing method. However, in the case of the post-processing method, the surface of the product is hardened and discolored and uneven flame retardancy is exhibited.

Japanese Patent Application Laid-Open No. 62-6912 discloses a method for producing a flame-retardant fiber by a bromine-based compound. However, these brominated flame retardants are restricted to use in many countries due to the problem of low heat resistance and the harmfulness of gas caused by combustion in many countries.

Instead of applying a bromine-based compound, Japanese Patent Laid-Open Nos. 52-47891 and 2001-0004814 disclose a method for producing a flame-retardant fiber by adding a phosphorus compound to a polyester resin polycondensation reaction step have. However, since the flame-retarded fiber produced by such a manufacturing method usually has a monofilament fineness of 2 to 3 denier levels, it has a problem that it is somewhat stiff and emotional in softness.

Korean Patent Registration No. 10-1276098 discloses a method for producing a split type composite spinning fiber comprising a polyester copolymer resin copolymerized with a flame retardant compound and an alkali-soluble polyester resin. However, such a manufacturing method can secure fibers having less than one denier per unit fiber, but has a problem of poor bulkiness and washing fastness.

Therefore, in order to solve the above problems, a high shrinkage flame retardant polymer is manufactured by core yarn, a flame retardant polymer containing a flame retardant is produced as an effect yarn, The heat shrinkage ratio of the core yarn was maximized to develop the shrinkage flame retardant composite yarn excellent in flame retardancy and bulkiness.

In order to solve the above-mentioned problems, the present invention relates to a method of producing a core yarn by subjecting a high shrinkage flame retardant polymer to an effect yarn by preparing a flame retardant polymer containing a flame retardant, Which is superior in flame retardancy, dyed yarn and bulkiness by maximizing a difference in shrinkage ratio between core yarn and core yarn through overfeed heat treatment.

In order to solve the above problems, the present invention provides a shrinkable flame-retardant composite yarn using a high shrinkage flame retardant polymer, which comprises 5 to 10 mol% of isophthalic acid and 1 to 5 mol% of diethylene glycol relative to terephthalic acid The present invention relates to a method for producing a polyester resin composition, which comprises the steps of: preparing a polyester resin composition by using a high shrinkage polyester resin; And the diethylene glycol further increases the volume of the amorphous region of the polyester and the volume of the crystalline region so that the shrinkage ratio is improved by 10 to 20% than that of the effect yarn, and 5000 to 7000 ppm of the phosphorus flame retardant And a limiting oxygen index of not less than 30. The shrinkage retardant composite yarn is obtained by using a high shrinkage flame retardant polymer.

The present invention also provides a shrinkage retardant composite yarn using the high shrinkage flame retardant polymer, wherein the number of interlocking yarns of the shrinkage retardant composite yarn is 70 / m or more.

The present invention also relates to a method for producing a shrinkage retardant conjugated yarn using a high shrinkage flame retardant polymer, which comprises adding 5 to 10 mol% of isophthalic acid to terephthalic acid and 1 to 5 mol% of diethylene glycol to ethylene glycol, The present invention provides a method for producing a polyester yarn, comprising the steps of: supplying a polyester containing 5000 to 7000 ppm of a phosphorus flame retardant to an effect yarn as a raw material, using a high shrinkage polyester containing phosphorus flame retardant; A contact heat treatment step of performing relaxation heat treatment by an overfeed method through a heat roller; A non-contact heat treatment step of heat-treating the effect yarn heat-treated in the contact heat treatment step in a heat plate; Wherein the isophthalic acid reduces the volume of the crystal region of the polyester, and the diethylene glycol has a melting point higher than the melting point of the polyester, The present invention provides a method for manufacturing the shrinkage-resistant flame-retardant composite yarn using the high shrinkage flame retardant polymer, characterized in that the volume of the amorphous region of the polyester is increased and the volume of the crystalline region is reduced.

Further, the present invention provides a method for manufacturing the shrinkage-resistant flame-retardant composite yarn, wherein the shrinkage ratio of the shrinkage-proofing is improved by 10 to 20% and the marginal oxygen index is 30 or more.

In addition, the present invention provides a method for manufacturing the shrinkage-resistant flame-retardant composite yarn, wherein the overfeeding ratio is 5 to 15% and the shrinkage ratio after the relaxation heat treatment is 1 to 10%.

The present invention also provides a process for producing the shrinkage retardant conjugated yarn, wherein the number of interlocking yarns of the shrinkage retardant conjugated yarn is not less than 70 / m.

The present invention relates to a method for producing a core yarn by subjecting a high shrinkage flame retardant polymer to an effect yarn by making a flame retardant polymer containing a flame retardant and then subjecting the resultant to an over feed heat treatment The difference in shrinkage ratio between the core yarn and the core yarn is maximized, and the flame retardancy and bulkiness are excellent.

In addition, in the present invention, when the shrinkable composite yarn is manufactured, the difference in shrinkage ratio between the examination and the effect yarn is expressed by 10 to 20%, and the bulkiness provides excellent effects.

In addition, the present invention is characterized in that the interlace of the shrinkage composite yarn is imparted with the number of entangled bands of 70 / m or more, so that the yarn after dyeing is good.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a process diagram of a method for producing a polyester composite yarn excellent in flame retardancy and bulkiness according to the present invention.
Fig. 2 is a schematic view of a polyester composite yarn process having excellent flame retardancy and bulkiness according to the present invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, 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 "substantially", "substantially", and the like are used herein to refer to a value in or near the numerical value when presenting manufacturing and material tolerances inherent in the meanings mentioned, Absolute numbers are used to prevent unauthorized exploitation by unauthorized intruders of the mentioned disclosure.

The present invention relates to a shrinkage retardant composite yarn using the high shrinkage flame retardant polymer, wherein a high shrinkage polyester obtained by adding 5 to 10 mol% of isophthalic acid and 1 to 5 mol% of diethylene glycol relative to terephthalic acid A core yarn 100 and a polyester yarn 200 using the general polyester yarn are subjected to an overfeed heat treatment,

The isophthalic acid can reduce the volume of the crystalline region of the polyester and the diethylene glycol can expand the volume of the amorphous region of the polyester and reduce the volume of the crystalline region. The present invention relates to a shrinkage-retardant composite yarn using the high shrinkage flame retardant polymer, wherein the difference is 10 to 20%, the yarn 100 and the composite yarn each contain 6000 ppm of a phosphorus flame retardant, .

The isophthalic acid serves to reduce the volume of the crystalline region of the polyester. Diethylene glycol is added to increase the volume of the amorphous region and shrinkage due to the reduction of the crystalline region.

In general, it can be divided into a two-phase structure, which is divided into a crystalline region and an amorphous region in a fiber formation condition. The crystalline region is characterized by the orderly arrangement of the polymer chains regularly and is functionally involved in the strength, elasticity and heat resistance of the fibers.

On the other hand, the amorphous region is characterized by a disordered state in which polymer chains are loose and low in regularity, and is related to flexibility, which is an easily deformed, fiber curved or stretched characteristic.

Therefore, when the above isophthalic acid and diethylene glycol are added to a general polyester as a modifier, the bulk of the amorphous region becomes large and the volume of the crystalline region becomes small, so that the strength of the fiber is reduced. Polyester fibers.

However, addition of 5 mol% or less of isophthalic acid causes the effect of inhibiting the crystallization in the polyester fiber to be lowered, and even if the preparation conditions are optimized, the shrinkage rate is hardly expressed by 20% or more. When 10 mol% or more of isophthalic acid is added, So that heat resistance is deteriorated.

Each of the test yarn 100 and the effect yarn 200 contains about 5,000 to 7,000 ppm of a phosphorus flame retardant in the respective spinning stages.

The phosphorus flame retardant is a phosphorus compound such as RDXP (resorcinol bis (di 2,6-xylenylphosphate)), ADPP (anilinodiphenylphosphate), RDPP (resorcinol bis (diphenylphosphate) (Triphenylphosphine oxide) may be used.

In the examination 100 and the effect yarn 200, 6,000 ppm or more is added, and then the limiting oxygen index is 30 or more after fiber production. However, when the content of the flame retardant is less than 5,000 ppm, there is a problem that the flame retardancy is low due to the limit oxygen index of 30 or less after the production of the fiber. When the content of the flame retardant is 7,000 ppm or more,

The limit oxygen index (LOI) value obtained by quantifying the degree of flame retardancy has a value of 30 to 40 in view of the content of the flame retardant.

When the number of entangled bonds of the composite yarn is greater than 70 / m and the entangled number is less than 70 / m in the intermingling step of the two judges 100 and the effect yarn 200, ) May occur.

In order to obtain the bulkiness effect of the shrinkage effect of the screen 100 and the effector 200, the shrinkage ratio of the screen 100 is greater than that of the effector 200, and the difference is about 10 to 20%. When the content is less than 10%, the shrinkage ratio is small and the winding property is insufficient. Thus, the bulkiness effect due to shrinkage of the fibers may be insufficient. If the blending ratio exceeds 20%, the winding property is too strong.

Basically, the contraction ratio of the effect yarn 200 has a value of 5 to 10%, and the evaluation value 100 of the polyester fiber modified to a high shrinkage has a value of 20 to 25%. Therefore, the contraction ratio, which is the difference in shrinkage ratio between the screen 100 and the effect yarn 200, has a value of 10-20% and has a proper bulkiness effect.

FIG. 1 is a process diagram of a method for producing a polyester composite yarn excellent in flame retardancy and bulkiness according to the present invention, and FIG. 2 is a schematic diagram of a polyester composite yarn process having excellent flame retardancy and bulkiness according to the present invention.

The process of FIG. 1 is a process in which 5 to 10 mol% of isophthalic acid is added to terephthalic acid in polymerization, 1 to 5 mol% of diethylene glycol is added to ethylene glycol, and a high shrinkage polyester containing 6000 ppm of phosphorus- ) Supplying polyester yarns containing 6000 ppm of a phosphorus flame retardant to the effect yarn 200 as a raw material; A contact heat treatment step of relaxing the effect yarn 200 by an over feed method through a heat roller; A non-contact heat treatment step of heat-treating the effect yarn 200 heat-treated in the contact heat treatment step in a heat plate; An entanglement step of entangling the heat-treated effect yarn 200 and the test yarn 100 through air entanglement, and a coiling step of winding the entangled composite yarn, wherein the isophthalic acid is used to reduce the volume of the crystalline region of the polyester And the diethylene glycol is capable of expanding the amorphous region volume of the polyester and reducing the volume of the crystalline region. BACKGROUND OF THE INVENTION [0002] The present invention relates to a method for producing a shrinkable flame retarded composite yarn using a high shrinkage flame retardant polymer.

As shown in FIG. 2, when the impact yarn 200 is manufactured by applying the flame retardant polymer for the effect yarn 200, the heat plate 30 (heat (heat)) is applied between the heat roller 10 and the drawing roller 70 Plate, it is possible to secure a partially oriented yarn (POY) having excellent shrinkage ratio of less than 10% and excellent flame retardancy by applying an over feed.

If the overfeed rate is less than 5%, the contraction ratio of the yarn yarns 200 is expressed by 10% or more, and the difference in contraction ratio with the core yarn 100 is not large enough to cause poor balancing property and softness, Is more than 15%, there is a problem that when the relaxed heat treatment is performed, the yarn is shaken so much that a dyed yarn is produced and then a dyed yarn is generated when the yarn is observed.

In addition, the effect yarn 200 imparts an overfeed to the relaxation heat treatment, and the judging yarn 100 is subjected to an entanglement step in an interlace device, such as the effect yarn 200, after passing through the stretching roller. When the shrinkage composite yarn is produced, it is necessary to provide sufficient entanglement and the number of entangled bands should be 70 / m or more to obtain a shrinkage retardant composite yarn having a good afterglow dyeing. When the number of entangled bands is less than 70 pieces / m, there is a problem that a dyed yarn occurs when the dyed yarn is observed. This is because the difference in dyeability between the judging yarn 100 and the effect yarn 200 results in a difference in dyeability between the judging yarn 100 and the effect yarn 200 when the yarn is not sufficiently mixed and the yarn is insufficient, Resulting in a dyed yarn.

Hereinafter, the present invention will be described in more detail with reference to examples. It is to be understood, however, that these examples are provided so as to understand the scope of the present invention, and are not to be construed as limiting the scope of the present invention.

Example  One

(100), 6,300 ppm of phosphorus flame retardant was added, 6.0 mol% of isophthalic acid was added to terephthalic acid, and 3 mol% of diethylene glycol was added to ethylene glycol to prepare a high shrinkage flame retardant polymer After that, a spinning speed of 1,200 m / min and a stretching ratio of 3.33 were applied to produce a core yarn of 50 denier / 24 fila.

The flame retardant polymer was prepared by adding 6,300 ppm of a phosphorus flame retardant agent to the flame retardant polymer prepared by the effect yarn 200, and then the flame retardant polymer was prepared at a spinning speed of 2,850 m / min to prepare 120 denier / 72 filament of partially oriented yarn (POY).

In the production of this composite shrinkage composite yarn, the examination yarn 100 is subjected to external and internal yarns, and the effect yarn 200 is subjected to a relaxation heat treatment at a heat treatment temperature of 200 ° C and an overfeed of 9%, passed through a drawing roller 70 And the entanglement was carried out at an entanglement pressure of 3,5 kgf / cm < 2 >

Example  2

The shrinkage retardant composite yarn was prepared in the same manner as in Example 1, except that the overfeed ratio was set to 5% in the relaxation heat treatment of the effect yarn.

Comparative Example  One

This shrinkage retardant composite yarn was prepared in the same manner as in Example 1, except that 5,000 ppm of a flame retardant was added in the production of the high shrinkage flame retardant polymer and the flame retardant polymer.

Comparative Example  2

This shrinkage retardant composite yarn was prepared in the same manner as in Example 1, except that the overfeed ratio was set to 0% in the relaxation heat treatment of the effect yarn.

Comparative Example  3

This shrinkage retardant composite yarn was prepared in the same manner as in Example 1, except that 3.0 mol% of isophthalic acid was added to terephthalic acid in the production of the high shrinkage flame retardant polymer.

Comparative Example  4

The shrinkage retardant composite yarn was prepared in the same manner as in Example 1, except that the overfeed ratio was set to 15% in the relaxation heat treatment of the effect yarn.

Comparative Example  5

The shrinkage retardant composite yarn was produced in the same manner as in Example 1, except that the entanglement pressure of the shrinkage retardant composite yarn was 2.0 kgf / cm 2.

◎ Shrinkage

  - Boiling water shrinkage (BWS): The ratio of the length reduced to the original length when measured after immersing the test and effect yarn at 100 ° C for 30 minutes under no-

    L0: Initial length of sample yarn

    L1: Length reduced after immersion of the sample yarn at 100 DEG C for 30 minutes

    Shrinkage ratio (BWS) = (L0-L1) / L0 * 100

◎ The shrinkage ratio (ΔBWS)

   - Contraction rate: Core Yarn BWS Effect Yarn BWS

◎ Interchange

   - Visually check the number of this shrinkage flame retardant composite yarn manufactured per 1m with handrail lock.

◎ Flammability

   - This shrinkage flame retardant composite yarn was prepared and evaluated by limiting oxygen index (LOI) analysis according to KS M ISO 4589 evaluation method.

◎ Dye

   - Observation of the naked eye dyed yarn after dyeing this shrinkage flame retardant composite yarn manufactured

◎ Bulkiness

   - Measure the thickness of knitted fabric after dyeing this shrinkage retardant composite yarn

     Thickness of 100μm or more: Good bulging property

     Thickness less than 100μm: Badness defectiveness

The results of Table 1 show that the flame retardant content of the Example is 6,300 ppm and the limit oxygen index (LOI) of the knitted fabric made of the flame retardant composite made of the flame retardant polymer is good at 34 and the flame retardant content is less than 6,000 ppm In Comparative Example 1, the flame retardancy was found to be inferior.

In Comparative Example 2, when the heat shrinkable flame retardant polymer was produced, the overfeed rate was 0, which is less than 5%, and the contraction ratio of the effect yarn was 18%. Thus, the core yarn and shrinkage difference were as large as 4% It can be seen that the bulkiness becomes poor.

In Comparative Example 3, when the addition amount of isophthalic acid was less than 6 mol% in the preparation of the high shrinkage flame retardant polymer, the contraction ratio of the core yarn made of the polymer was formed to be 3%, which is less than 20% It can be seen that the bulkiness becomes poor.

Comparative Example 4 shows that when the overfeeding rate is more than 15% when the shrinkage-retarding polymer is produced, the shrinking composite yarn is unstable during the relaxation heat treatment, resulting in a dyed yarn (dyeing unevenness) Able to know.

Also, in Comparative Example 5, when the shrinkage composite yarn is produced at a mixing ratio of less than 70 / m, it can be seen that the shrinkage composite yarn is subjected to a dyeing operation after the yarn is dyed.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the inventions. It will be clear to those who have knowledge of.

DESCRIPTION OF THE RELATED ART [0002]
100: Screening 200: Effectiveness
10: Heat roller 30: Heat plate
50: interlocking device 70: stretching roller

Claims (6)

In this shrinkage retardant composite yarn using a high shrinkage flame retardant polymer,
In the polymerization, overfeeding was carried out using a high shrinkage polyester obtained by adding 5 to 10 mol% of isophthalic acid to terephthalic acid and 1 to 5 mol% of diethylene glycol to ethylene glycol, And a composite made by heat treatment,
The above examination shows that the added isophthalic acid reduces the volume of the crystalline region of the polyester and the diethylene glycol increases the volume of the amorphous region of the polyester and the volume of the crystalline region to thereby improve the shrinkage by 10 to 20% And,
The shrinkage retardant composite yarn using the high shrinkage flame retardant polymer according to any one of claims 1 to 5, wherein the flame retardant comprises 5000 to 7000 ppm of a phosphorus flame retardant.
The method according to claim 1,
Characterized in that the number of entanglement of the shrinkage retardant composite yarn is 70 / m or more.
A method for manufacturing a shrinkage-resistant flame-retarded composite yarn using a high-shrinkage flame retardant polymer,
In the examination, 5 to 10 mol% of isophthalic acid and 5 to 10 mol% of diethylene glycol were added to terephthalic acid and 5 to 7000 ppm of ethylene glycol, respectively, and the high shrinkage polyester containing phosphorus- To an effect yarn as a raw material;
A contact heat treatment step of relaxing the effect yarn by an overfeed method through a heat roller;
A non-contact heat treatment step of heat-treating the effect yarn heat-treated in the contact heat treatment step in a heat plate;
An engraving step of juxtaposing the heat-treated effect yarn with the judging through air entanglement, and
And a winding step of winding the entangled composite yarn,
Wherein the isophthalic acid reduces the volume of the crystalline region of the polyester and the diethylene glycol increases the volume of the amorphous region of the polyester and reduces the volume of the crystalline region. The shrinkable flame retardant composite Lt; / RTI >
The method of claim 3,
Wherein the shrinkage ratio of the shrinkage-proof yarn is 10 to 20% higher and the marginal oxygen index is 30 or more.
The method of claim 3,
Wherein the overfeed rate is 5 to 15% and the shrinkage ratio after the relaxation heat treatment is 1 to 10% in the relaxation heat treatment of the effect yarn.
The method of claim 3,
Wherein the number of entanglement of the shrinkage retardant composite yarn is 70 / m or more.

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