KR100687047B1 - Process for preparing polyethyleneterephthalate bulky continuous filament for carpet - Google Patents

Abstract

A manufacturing method of a PET(PolyEthyleneTerephthalate) BCF(Bulked Continuous Filament) for a carpet is provided to produce the uniform and high level crimp. A polyethylene terephthalate polymer having the inherent viscosity of 0.4-1.0 and containing the phosphorus retardant of 0.05-5 wt % is melted and spun at 245-335 degrees in centigrade and then passed through a spinneret(1). Thereafter, the polyethylene terephthalate polymer is cooled at a cooling region(3) by the air at the speed of 0.2-1.0m/sec. Thereafter, the spin finish process is performed by neat type solvent or aqueous solvent at a finish applicator(4). Thereafter, the filament is supplied to a drawing roller(7) at the speed of 400 to 800 m/min.

Description

Process for preparing polyethylene terephthalate bulky continuous filament for carpet

1 is a schematic view showing an apparatus for producing polyethylene terephthalate bulky continuous filaments according to the present invention

<Description of the symbols for the main parts of the drawings>

① Radiation detention ② Filament ③ Cooling zone ④ Finish

⑤ Supply roller ⑥ First drawing roller ⑦ Second drawing roller ⑧ Texturing unit

⑨Cooling section ⑩Interlocking machine ⑪ Relaxing roller ⑫End winding machine

The present invention relates to a method for preparing polyethylene (terephthalate) bulky continuous filament (hereinafter referred to as BCF), and more particularly to the phosphorus-based flame retardant in the production of polyethylene terephthalate BCF yarns. A polymer containing 0.05 to 5% by weight of phosphorus atoms is used, and the bulking property of the yarn is improved by using a texturing process using a steam jet or an air jet. The present invention relates to a method for producing a BCF yarn having a uniform physical property by stabilizing a crimp value.

As a synthetic material of BCF used in general carpet production, nylon, polypropylene, polyethylene terephthalate, and the like are typically used. In particular, in recent years, a process for producing BCF and carpet using a polyethylene terephthalate material is in the spotlight, because the polyethylene terephthalate material has superior properties compared to other materials in terms of economical efficiency.

There are two methods for imparting flame retardancy to fibers, and a method of imparting flame retardancy by providing a flame retardant process and a method of imparting permanent flame retardancy by flame retarding a polymer used in textile materials. BACKGROUND ART A method of imparting flame retardancy by using flame retardant processing has been conventionally made for natural fibers such as cotton and the like, and has recently been applied to synthetic fibers. However, imparting flame retardancy by post-processing not only has a problem of durability, but also causes environmental problems due to wastewater generated during processing, and thus its use is in decline.

Meanwhile, as a method of imparting permanent flame retardancy by flame retarding the polyethylene terephthalate fiber material itself, a method of imparting flame retardancy by copolymerization is mainly used, and a flame retardant having reactivity is industrialized in various ways.

Bromine-based and phosphorus-based flame retardants are mainly used in the production of flame-retardant polyethylene terephthalate by copolymerization. Bromine-based flame retardant inventions include Japanese Patent Laid-Open No. 62-6912, Japanese Patent Laid-Open No. 53-46398, Japanese Patent Laid-Open No. 51-28894, and bromine compounds are easily thermally decomposed at high temperatures, and therefore, a large amount must be added to obtain effective flame retardancy. As a result, the color of the polymer water is lowered and the light resistance is lowered. Also, recently, the possibility of generating carcinogenic substances such as dioxin and benzofuran is raised. .

The present invention was devised to improve the flame retardancy and bulkiness problems of the existing polyethylene terephthalate yarn for BCF as described above, flame retardant polyethylene terephthalate polymer containing 0.05 to 5% by weight phosphorus based flame retardant When stretching, stretching in one or two stages, and by using a steam jet or air jet texturing process to express a high bulky, create a uniform and high level crimp To provide a polyethylene terephthalate bulky continuous filament and a method for producing the same.

A method for producing a flame retardant polyethylene terephthalate bulky continuous filament according to the present invention for achieving the above object, A) a polyethylene terephthalate polymer containing 0.4 to 1.0 intrinsic viscosity, 0.05 to 5% by weight of phosphorus-based flame retardant based on phosphorus atoms Melt spinning at 245 to 335 ° C., B) cooling to 10 to 35 ° C. with air at a rate of 0.2 to 1.0 m / s in the cooling zone, C) knit type or water soluble oil at spin finish. Step of imparting an emulsion using D, feeding the filament to the stretching roller at a speed of 100 ~ 1,000m / min from the feed roller, the stretching roller is a hot roller (temperature hot roller) and the temperature is 100 ~ 230 Stretching at a speed of 2.5 to 6.0 times greater than the feed roller speed, E) passing through a texturing unit with a texturing nozzle to give bulkiness to the filament passing through the drawing roller. When the heating fluid is sprayed inside the texturing unit to give 3-50% crimp to crimp the filament in an irregular three-dimensional manner, F) After cooling the filament passing through the texturing unit, it passes through an entanglement 0-40 times / m. And G) passing through the relaxation roller at a speed of 0.65-0.95 times the stretching roller speed, giving a relaxation of 5 to 35%, and winding the winder.

In addition, the phosphorus-based flame retardant is characterized in that represented by the formula (1).

[Formula 1]

Wherein R ¹ and R ² have a hydrogen atom or a w-hydroxy group having 2 to 4 carbon atoms or another radical group, and n is an integer of 1 to 5;

In addition, the heating fluid injected in the texturing unit is preferably a steam jet or air jet.

In addition, the temperature of the heating fluid injected in the unit in step E) is 150 ~ 280 ℃, the pressure is preferably ³ ~ 10kg / cm ² .

In addition, the colorant may be included in the polyethylene terephthalate polymer in the step A) 1 to 5% by weight based on the total weight.

In addition, the present invention provides a polyethylene terephthalate bulky continuous filament having a crimp standard deviation of 5% or less.

The present invention also provides a carpet having excellent volume feeling including the polyethylene terephthalate bulky continuous filament of the present invention.

Hereinafter, the polyethylene terephthalate bulky continuous filament for carpet according to the present invention and a manufacturing method thereof will be described in detail with reference to the accompanying drawings.

In the description of the present invention, the terms defined are defined in consideration of the functions of the present invention, which may vary according to the intention or custom of those skilled in the art, and thus, limit the technical components of the present invention. It should not be understood.

1 is a view schematically showing an apparatus for producing polyethylene terephthalate BCF according to the present invention.

First, a polyethylene terephthalate polymer containing 0.4 to 1.0 intrinsic viscosity and 0.05 to 5% by weight of phosphorus-based flame retardant is melt-spun at 245 to 335 ° C to pass through the spinneret (1).

The polyethylene terephthalate resin underlying in the present invention contains 90 mol% or more of repeating units of ethylene terephthalate.

The phosphorus-based flame retardant is characterized in that represented by the formula (1).

Wherein R ¹ and R ² have a hydrogen atom or a w-hydroxy group having 2 to 4 carbon atoms or another radical group, and n is an integer of 1 to 5;

The content of the phosphorus-based flame retardant represented by the formula (1) is 0.05 to 5% by weight, preferably 0.1 to 2% by weight, based on the number of people. If the phosphorus atom content is less than 0.05% by weight, the flame retardant effect is inferior, and when the phosphorus atom content is more than 5% by weight, the polyester polymerization degree is lowered and the physical properties of the BCF company are lowered.

Thereafter, the cooling zone 3 is cooled with air having a speed of 0.2 to 1.0 m / sec. At this time, the cooling temperature is adjusted to 10 ~ 35 ℃. At this time, if the speed of the cooling air is less than 0.2m / sec, the cooling effect is insufficient, and if it exceeds 1.0m / sec, the shaking of the yarn is excessive and there is a problem in the spinning workability. In addition, if the cooling temperature is less than 10 ℃ economically disadvantageous, if it exceeds 35 ℃ cooling effect is inferior.

After cooling, go through the spin finish step of oiling. In the first and second stages of the finish applicator (4), oiling with neat type oil or water-soluble oil is performed to oil the yarn's focusing power and lubricity. , Improves smoothness.

Thereafter, the feed rollers 5 and 6 feed the filament to the stretching roller 7 at a speed of 100 to 1,000 m / min, preferably 400 to 800 m / min, wherein the stretching roller is 100 to 230 ° C. The drawing is performed at a speed of 2.5 to 6.0 times the speed of the feed rollers 5 and 6, and preferably at 3.5 to 5.0 times. When the stretching speed is less than 2.5 times, it is not stretched sufficiently, and when the stretching speed is greater than 6.0 times, the polyethylene terephthalate material is not able to withstand the stretching and is trimmed.

The filament passed through the stretching roller passes through the texturing unit 8 with the texturing nozzle to impart bulking properties. At this time, the heating fluid is sprayed at a pressure of ³ to 10 kg / cm ² at 150 to 270 ° C. inside the texturing unit. The filament is crimped in irregular three dimensions, and the crimp rate is 3-50%.

At this time, the temperature of the heating fluid is preferably 150 ~ 270 ℃, which is less than 150 ℃ texturing effect and exceeds 270 ℃ causes damage to the filament. In addition, the pressure of the heating fluid and the 3~10kg / cm ² Preferably, this results in damage to the filament when the falling texturing effect exceeding 10kg / cm ² is less than 3kg / cm ^2.

The filament passing through the texturing unit is cooled while passing through the cooling section 9 and passes through the entanglement device 10. In this part, in order to improve the focusing force of the yarn, a slight twist and a knot are applied at a pressure of 2.0 to 8.0 kg / m ^2. The range is 0 to 40 times / m, preferably 10 to 25 times. When the entanglement is given more than 40 times, the entanglement remains unchanged even after dyeing and post-processing, thereby damaging the appearance of the carpet.

Thereafter, the relaxation roller 11 is passed through at a speed of 0.65 to 0.95 times the stretching roller speed to give a relaxation rate of 5 to 35%, and then wound up at the final winding machine 12. The speed of the winder is usually adjusted so that the tension of the thread is in the range of 50 to 350 g. At this time, if the tension of the winder is less than 50g, the winding is impossible. If it exceeds 350g, the bulkiness decreases, the yarn shrinks greatly, and high tension causes the work. In addition, if the speed of the relaxation roller is less than 0.65 times of the stretching roller speed, it is not wound, and if it exceeds 0.95 times, the bulkiness is decreased, the yarn shrinks greatly, and high tension causes the work.

The method relates to a BCF made of polyethylene terephthalate resin only, the step-by-step process when manufacturing the raw yarn according to the use of the carpet is the same as above, but in the raw material supply by inserting a predetermined amount of colorant to the base chip input spinning yarn It is also possible to prepare.

The polyethylene terephthalate bulky continuous filaments produced by the present invention exhibit the following physical properties.

   1) Crimp rate: 5-50%, 2) Strength: 1.5g / denier or more, 3) Elongation: 5-50%

In addition, the bulky continuous filament produced according to the present invention as described above is manufactured into a carpet through a post-process. Carpets made with the BCF company of the present invention may be prepared in any manner known to those skilled in the art. Preferably a plurality of BCF yarns are cable twisted and heat set together and then weave to the primary back side. The latex adhesive and secondary backing are then applied. Cut pile style carpets or loop pile style carpets having pile heights of approximately 2-20 mm can be produced. At this time, the weight of the carpet is 400 to 4000g / m ² .

The invention can be better understood by the following examples, which are intended for the purpose of illustration of the invention and are not intended to limit the scope of protection defined by the appended claims.

<How to evaluate bulky continuous filament properties>

1) Intrinsic viscosity (I.V.)

 After dissolving 0.1 g of the sample in a reagent (90 ° C.) mixed with phenol and 1,1,2,3-tetrachloroethanol at a weight ratio of 6: 4 for 90 minutes to give a concentration of 0.4g / 100ml, Ubbelohde Transfer to a viscometer was carried out for 30 minutes in a 30 degreeC thermostat, and the drop number of seconds of the solution was calculated | required using a viscometer and an aspirator. The number of falling seconds of the solvent was also determined in the same manner, and then the R.V.value and the I.V.value were calculated by the following equation.

Where C represents the concentration of the sample in solution (g / 100ml).

2) strength, elongation

  The test was conducted according to KS, K 0412 (Filament's test method for strength and elongation). The test conditions before measurement were 20cm in sample length, 200mm / min tensile speed, 20g super load, and 8 times / 10cm twist.

3) Crimp rate and standard deviation

  Measured by TYT-EW (Textured Yarn Tester) measuring device, measuring length is 20m, measuring 5 times at intervals of 2m. Heating zone temperature is 130 ℃ and measuring speed is 20m / min.

4) denier

  Weight of yarn 9,000 m (g)

5) Compression Modulus

The pile height of the carpet is measured 5 minutes after the load of 1 kg is added to the carpet. At this time, the ratio of the compression height to the pile height before the load part is called the compression ratio. After removing the load on the same sample, measure the pile height after 5 minutes. At this time, the ratio of the height after the removal of the load to the pile height of the load addition gun is referred to as the modulus of elasticity.

6) Flame retardant

  The fabrics were tested according to the KS M 3032 standard in Korea to evaluate the LOI (Limited Oxygen Index).

7) Combustibility

  The prepared carpets were evaluated by testing to the ASTM E 648-99 standard.

Example 1

The slurry prepared with 8650 g of terephthalic acid (TPA) and 2700 g of ethylene glycol (EG) was subjected to an esterification reaction by a semi-batch method. At this time, the temperature of the esterification tank was kept at 250-260 degreeC. The prepared oligomer was transferred to a polycondensation reactor. As the flame retardant, in the formula (1), a substance having n = 1 R ¹ = R ² = CH ₂ CH ₂ OH dissolved in 65% by weight of EG was used. After adding 1580 g of flame retardant solution, 50 ppm to 45 ppm of manganese acetate and phosphoric acid were added as UV stabilizers, respectively, and 200 g of antimony trioxide solution dissolved in EG as a catalyst was added by 200 g to carry out a polycondensation reaction. The polymer of intrinsic viscosity (IV) 0.65 dl / g was obtained.

The polyethylene terephthalate polymer having a intrinsic viscosity (IV) of 0.65 and a moisture content of 120 ppm was melt-spun at 275 ° C. through a spinneret having a 68-hole (Hole) and Y-shaped cross section. The polymer exiting the spinneret is cooled by 0.5 m / s at 20 ° C. cooling air at the bottom of the nozzle and then passed through the emulsion feeder. The emulsified yarn is fed through a feed roller at a speed of 598 m / min and then drawn at a speed of 170 ° C. and 2,840 m / min in the drawing roller. The yarn passed through the stretching roller passes through the texturing nozzle and is crimped. At this time, the steam temperature is 183 ℃, the pressure is 4.8kg / cm ² and the back pressure is 2.5kg / cm ² . Thereafter, after cooling by cooling water, the concentrator is applied 20 times / m at a pressure of 4.0 kg / m ² . It passes through the relax roller at 2250m / min and is relaxed by 21% and then wound up on a winding machine. Denier, strength, and crimp values of polyethylene terephthalate BCF yarns prepared in this process were measured.

Example 2

Spinning to the same polymer as in Example 1, but by varying the speed of the feed roller, stretching roller, relax roller to produce flame-retardant PET BCF with different denier, strength, elongation.

After the spin finish step, the polymer is stretched by the stretching roller at a speed of 2532 m / min past the feed roller at a speed of 532 m / min, where the temperature of the stretching roller is 160 ° C. The yarn passed through the stretching roller passes through the texturing nozzle and is crimped. At this time, the steam temperature is 208 ℃, the pressure is 4.8kg / cm ² and the back pressure is 2.5kg / cm ² . Thereafter, after cooling by the cooling water, the concentrator is applied 16 times / m at a pressure of 4.0 kg / m ² . It passes through the relaxation roller at 2275m / min and is relaxed by 24% and then wound up on a winding machine. Denier, strength, and crimp values of polyethylene terephthalate BCF yarns prepared in this process were measured.

Example 3

Spinning was carried out under the same conditions as in Example 1 except that the raw yarn was prepared by blending spinning 3% by weight of color masterbatch (Color masterbatch) compared to the base chip input amount.

Comparative Example 1

It was spun under the same conditions as in Example 1 using a pure polyethylene terephthalate polymer containing no phosphorus-based flame retardant. The denier, strength and crimp, and LOI values of the yarn thus prepared were measured.

division Denier Strength (g / d) Crimp (%) Crimp Standard Deviation (%) Phosphorus content (% by weight) Flame Retardant (LOI) Example 1 1252 3.32 17 3.5 0.6 30.3 Example 2 1440 3.76 19 4.1 0.6 30.5 Example 3 1245 3.11 16 3.8 0.6 30.5 Comparative Example 1 1242 3.16 16 5.2 0 23.8

As shown in Table 1, Examples 1 and 3 and Comparative Example 1 were manufactured by BCF company under the same spinning conditions, so that physical properties such as strength and crimp ratio were not significantly different, and Example 2 having different draw ratios and relaxations had high strength. Relatively high.

However, Examples 1, 2 and 3 used a polyester polymer including a flame retardant, and Comparative Example 1 showed a large difference in LOI value using pure polyester. In addition, in the same spinning conditions, it can be seen that in the case of Examples 1 and 3, the crimp standard deviation value is lower than that of Comparative Example 1.

Example 4

The compressive modulus was measured by producing a carpet of the BCF yarn prepared through the above process under the following conditions.

Yarn Crimp Rate: 17%

Pile Height: 11mm

Stitch Length: 12.8 pcs / in

Gauge Length: 1/10 Gauge

Comparative Example 2

BCF yarn prepared by the same process as the pure polyester polymer was prepared in the carpet under the same conditions as in Example 4 and the compression modulus and flame retardance thereof were measured.

TABLE 2

Compression ratio Modulus Flame retardant Example 4 38.4% 90.7% 30.7 Comparative Example 2 38.3% 90.9% 23.6

As described above, the method for producing a polyethylene terephthalate bulky continuous filament according to the present invention shows high flame retardancy.

Claims (8)

A) melt spinning a polyethylene terephthalate polymer containing 0.4 to 1.0 intrinsic viscosity and 0.05 to 5% by weight of phosphorus based flame retardant at 245 to 335 ° C, B) cooling to 10-35 ° C. with air at a rate of 0.2-1.0 m / s in the cooling zone, C) emulsifying the emulsion at spin finish using a knit type or water soluble oil, D) Feed the filament to the stretching roller at the speed of 100 ~ 1,000m / min from the feed roller, the stretching roller is a hot roller, the temperature is between 100 ~ 230 ℃ and the speed is higher than the feed roller speed Stretching at a speed of 2.5 to 6.0 times, E) When passing through a texturing unit with a texturing nozzle to give bulkyness to the filament passing through the stretching roller, the heating fluid is sprayed inside the texturing unit to give 3-50% crimp to crimp the filament in an irregular three-dimensional manner. step, F) after cooling the filament passed through the texturing unit, passing through an entanglement device to impart entanglement of 0-40 times / m, and G) A method for producing a polyethylene terephthalate bulky continuous filament, comprising the steps of winding a winder at a rate of 0.65 to 0.95 times the stretching roller speed in a relax roller to give 5 to 35% relaxation. A) melt spinning a polyethylene terephthalate polymer containing 0.4 to 1.0 intrinsic viscosity and 0.05 to 5% by weight of phosphorus based flame retardant at 245 to 335 ° C, B) cooling to 10-35 ° C. with air at a rate of 0.2-1.0 m / s in the cooling zone, C) emulsifying the emulsion at spin finish using a knit type or water soluble oil, D) Feed the filament to the stretching roller at the speed of 400 ~ 800m / min from the feeding roller, where the stretching roller is a hot roller, the temperature is between 100 ~ 230 ℃ and the speed is 3.5 higher than the feeding roller speed. Stretching at a rate of ˜5.0 times, E) When passing through a texturing unit with a texturing nozzle to give bulkyness to the filament passed through the stretching roller, the heating fluid is sprayed inside the texturing unit to give 7-23% crimp to crimp the filament in an irregular three-dimensional manner. step, F) after cooling the filament passed through the texturing unit, passing through an entanglement machine to impart entanglement of 10-25 times / m, and G) A method for producing a polyethylene terephthalate bulky continuous filament, comprising the steps of winding a winder at a rate of 0.65 to 0.95 times the stretching roller speed in a relax roller to give 5 to 35% relaxation. The method according to claim 1 or 2, The phosphorus flame retardant is represented by the following formula (1) characterized in that the polyethylene terephthalate bulky continuous filament manufacturing method.

[Formula 1] Wherein R ¹ and R ² have a hydrogen atom or a w-hydroxy group having 2 to 4 carbon atoms or another radical group, and n is an integer of 1 to 5; The method according to claim 1 or 2, Method for producing a polyethylene terephthalate bulky continuous filament, characterized in that the heating fluid is injected in the texturing unit is steam jet or air jet. The method according to claim 1 or 2, The heating fluid is sprayed in the texturing unit is steam, the temperature of the steam is 150 ~ 270 ℃, the pressure is 3 ~ 10kg / cm ^{2 The} method of producing a polyethylene terephthalate bulky continuous filament. The method according to claim 1 or 2, Method for producing a polyethylene terephthalate bulky continuous filament, characterized in that 1 to 5% by weight based on the total weight of the polyethylene terephthalate polymer in the step A). A polyethylene terephthalate bulky continuous filament having a crimp standard deviation of 5% or less produced by the method of claim 1. A carpet comprising polyethylene terephthalate bulky continuous filaments prepared by the method of claim 1.

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