POLYESTER STAPLE YARN FOR WET NON-WOVEN FABRIC, WET NON-WOVEN FABRIC COMPRISING SAME, AND PREPARATION METHOD THEREFOR
20230416957 ยท 2023-12-28
Assignee
Inventors
Cpc classification
C08G63/85
CHEMISTRY; METALLURGY
D04H1/52
TEXTILES; PAPER
International classification
D04H1/52
TEXTILES; PAPER
C08G63/85
CHEMISTRY; METALLURGY
Abstract
The present invention relates to a polyester staple yarn for a wet non-woven fabric, and a wet non-woven fabric including the same, wherein the polyester staple yarn is manufactured by using a polymerization catalyst including a titanium-based compound. The polyester staple yarn is superb in terms of dispersibility due to the remarkably low defect formation thereof, and thus, the present invention can provide a wet non-woven fabric having excellent mechanical strength, and a manufacturing method therefor.
Claims
1. A polyester staple yarn for a wet non-woven fabric, which has a fineness of 0.3 to 3.0 de and a dispersibility of 10 ppm or less as measured by Relationship Formula 1 below:
2. The polyester staple yarn of claim 1, wherein the polyester staple yarn comprises a spinning material in which a polymerization product is spun, and wherein the polymerization product is a reaction product obtained by polymerization of an ester reaction product, and the ester reaction product is a reaction product obtained by reacting a mixture including an ester reaction product, a thermal stabilizer and a titanium-based compound represented by Chemical Formula 1 below: ##STR00005## wherein in Chemical Formula 1 above, R.sup.1 and R.sup.2 are each independently a straight-chain alkylene group having 1 to 5 carbon atoms or a branched alkylene group having 3 to 5 carbon atoms.
3. The polyester staple yarn of claim 1, wherein the polyester staple yarn has an average fiber length of 3 to 12 mm.
4. A wet non-woven fabric, comprising: the polyester staple yarn for a non-woven fabric according to claim 1; and a binder staple yarn, wherein the binder staple yarn and the polyester staple yarn are comprised at a weight ratio of 1:1.20 to 1:1.90.
5. The wet non-woven fabric of claim 4, wherein the wet non-woven fabric has an MD (machine direction) tensile strength of 150 to 300 N/15 mm.
6. The wet non-woven fabric of claim 4, wherein the standard deviation of the MD (machine direction) tensile strengths of the wet non-woven fabric satisfies Relationship Formula 2 below:
7. The wet non-woven fabric of claim 4, wherein the binder staple yarn has a fineness of 0.3 to 3.0 de and an average fiber length of 3 to 12 mm.
8. A method for manufacturing a wet non-woven fabric, comprising: Step 1 of manufacturing a handsheet by mixing a polyester staple yarn for a wet non-woven fabric and a binder staple yarn; Step 2 of manufacturing a paper sheet by drying the handsheet; and Step 3 of manufacturing a wet non-woven fabric by performing calendaring by applying at least one selected from heat and pressure to the paper sheet, wherein the polyester staple yarn is manufactured by comprising: Step 1-1 of obtaining an ester reaction product by reacting an acid component and a diol component; Step 1-2 of preparing a polyester resin by mixing and reacting polymerization reactants including the ester reaction product, a heat stabilizer and a titanium-based compound; Step 1-3 of preparing a spinning material by spinning the polyester resin; and Step 1-4 of manufacturing a polyester staple yarn by stretching the spinning material.
9. The method of claim 8, wherein the temperature is increased to a final temperature of 275 to 285 during the polymerization.
10. The method of claim 8, wherein the titanium-based compound includes 10 to 20 ppm of titanium element based on the total weight of the polymerization reactants.
11. A wet non-woven fabric, comprising: the polyester staple yarn for a non-woven fabric according to claim 2; and a binder staple yarn, wherein the binder staple yarn and the polyester staple yarn are comprised at a weight ratio of 1:1.20 to 1:1.90.
12. A wet non-woven fabric, comprising: the polyester staple yarn for a non-woven fabric according to claim 3; and a binder staple yarn, wherein the binder staple yarn and the polyester staple yarn are comprised at a weight ratio of 1:1.20 to 1:1.90.
Description
EXAMPLE
Example 1-1: Manufacture of Polyester Staple Yarn for Wet Non-Woven Fabric
[0088] (1) Preparation of Polyester Resin
[0089] 100 mol % of terephthalic acid (TPA) as an acid component and 100 mol % of ethylene glycol (EG) as a diol component were added to an ester reactor, and then reacted under 250 C. at a pressure of 1,140 torr to obtain an ester reaction product. In this case, the acid component and the diol component were introduced at a molar ratio of 1:1.2.
[0090] Then, the ester reaction product was transferred to a polycondensation reactor.
[0091] Then, a polyester resin was prepared by mixing and polymerizing the polymerization reaction product including the ester reaction product, a heat stabilizer and a titanium-based compound.
[0092] The polymerization reaction was carried out by increasing the temperature to a final temperature of 280 C. while gradually reducing the pressure to a final pressure of 0.5 torr.
[0093] In this case, the heat stabilizer was prepared by including triethyl phosphoric acid in an amount of 25 ppm based on phosphorus element in the total weight of the polymerization product.
[0094] In addition, as the titanium-based compound, a compound represented by the Chemical Formula 1-1 below was used, and it was added so as to be 15 ppm based on titanium element in the total weight of the polymerization product, and it was included at 300 ppm in the total weight of the polymerization product.
##STR00004##
[0095] In Chemical Formula 1-1, R.sup.1 and R.sup.2 are each independently an alkyl group having 1 carbon atom.
[0096] (2) Manufacture of Polyester Staple Yarn
[0097] The polyester resin was spun at a spinning rate of 1,500 ppm under 285 C. through an o-shaped spinneret to manufacture a spinning material.
[0098] Then, a polyester staple yarn was manufactured by stretching the spinning material at a stretching ratio of 3.0.
[0099] In this case, the polyester staple yarn had an average fiber length of 5 mm and a fineness of 1.2 de.
Example 1-2 to Example 1-9 and Comparative Example 1-1 to Comparative Example 1-8: Manufacture of Polyester Staple Yarns for Wet Non-Woven Fabric
[0100] Polyester staple yarns were manufactured in the same manner as in Example 1-1, except that the polymerization temperature (final elevated temperature), the amount of a titanium-based compound added (based on Ti element), the fineness of the staple yarn or the average fiber length of the staple yarn was set as shown in Tables 1 to 3 below to perform Examples 1-2 to 1-9 and Comparative Example 1-1 to Comparative Manufacture Example 1-8.
Comparative Examples 1-9 to Comparative Examples 1-12: Manufacture of Polyester Staple Yarns for Wet Non-Woven Fabric
[0101] Polyester staple yarns were manufactured in the same manner as in Example 1-1, except that the polymerization temperature (final elevated temperature), the type of polymerization catalyst or the amount of catalyst added (based on Ti element) was set as shown in Table 4 below to perform Comparative Example 1-9 to Comparative Examples 1-12.
Example 2-1: Manufacture of Binder Staple Yarn
[0102] 100 mol % of terephthalic acid (TPA) as an acid component and 100 mol % of ethylene glycol (EG) as a diol component were introduced into an ester reactor, and then reacted under 250 C. at a pressure of 1,140 torr to obtain an ester reaction product. In this case, the acid component and the diol component were introduced at a molar ratio of 1:1.2.
[0103] Then, the ester reaction product was transferred to a polycondensation reactor.
[0104] Then, a polyester binder resin was prepared through a polycondensation reaction in which the temperature of the ester reaction product was increased to 280 C. while gradually reducing the pressure to a final pressure of 0.5 torr.
[0105] Then, the polyester binder resin was spun through an o-shaped spinneret at a spinning rate of 1,900 ppm under 285 C. to manufacture a binder staple yarn.
[0106] In this case, the polyester binder staple yarn had an average fiber length of 5 mm and a fineness of 1.2 de.
Experimental Example 1: Evaluation of Physical Properties of Polyester Resins and Polyester Staple Yarns
[0107] The physical properties of the polyester resins (intermediate product) and polyester staple yarns for a wet non-woven fabric manufactured in Example 1-1 to Example 1-9 and Comparative Preparation Example 1-1 to Comparative Preparation Example 1-12 were evaluated in the following manner, and the results are shown in Tables 1 to 4 below.
[0108] (1) Intrinsic Viscosity (IV)
[0109] Polyester resin was melted at a concentration of 2.0 g/25 mL in the Ortho-Chloro Phenol solvent under 110 C. for 30 minutes, and then kept at 25 C. for 30 minutes to measure the intrinsic viscosity by using an automatic viscosity measurement device which was connected to a CANON viscometer.
[0110] (2) Quantification of Carboxyl Group Terminal Groups
[0111] The number of carboxyl groups of the polyester resin was measured according to the method of PHOL. Specifically, 0.1250 g of the polymerization product powder which was pulverized to a size of 20 mesh was precisely weighed and placed into a test tube, 5 mL of benzyl alcohol was added thereto, and it was stirred with a micro stirrer while heating and dissolving under 210 C. for about 135 seconds. Immediately after dissolution, the test tube was immersed in water at 25 C. for 6 seconds to rapidly cool, and the contents were poured into a 50 mL beaker containing 10 mL of chloroform. Afterwards, 5 mL of benzyl alcohol was added to the test tube, stirred for 60 seconds, and the remaining resin solution was completely rinsed and immediately added to a beaker, which was used as the titration solution. The carboxyl group content was neutralized and titrated with phenol red (0.1% benzyl alcohol solution) as an indicator and 0.1 N sodium hydroxide benzyl alcohol solution by using a microsyringe (mycrosyringe, 100 L capacity), and the titration determination value was corrected according to the blank test result for the titration reagent and calculated according to Relationship Formula 3 below.
[0112] In this case, f is the concentration coefficient of a 0.1N sodium hydroxide benzyl alcohol solution.
[0113] (3) Evaluation of Spinning Workability
[0114] For spinning workability, the number of drips (meaning a lump formed by partially fusion of the fiber strands passing through the spinneret or irregular fusion of the strands after trimming) during the spinning processing of polyester staple yarns was counted through a drip detector, and based on the number of drip occurrences in Example 1-1 as 100, the number of drips generated in the other examples and comparative examples was expressed as a relative percentage.
[0115] (4) Measurement of Wiping Cycle (Number of Times)
[0116] In the manufacturing process of polyester staple yarns, it was calculated how many times a spinneret was wiped per day. As the value of the wiping cycle increased, it was determined that the spinneret was contaminated with foreign matter.
[0117] (5) Measurement of b Value (b*)
[0118] The color of the polyester staple yarns was analyzed through a colorimeter to measure the b value. The measurement method was based on spectroscopy, and the method of calculating chromaticity coordinates by using the CIE standard light source and standard observer was used.
[0119] (6) Measurement of Dispersibility
[0120] Dispersibility was calculated according to Relationship Formula 1 below.
[0121] The number of undispersed fibers is determined by adding 3 g of a polyester staple yarn for a wet non-woven fabric having a moisture content of 25 wt. % to 1 L of water at a temperature of 25 C., stirring for 10 minutes under the condition of 600 rpm, leaving for 1 minute and then measuring the number of undispersed fibers.
[0122] In this case, it was determined that as the dispersibility was higher, the number of undispersed fibers was greater, and it was determined to be poor.
TABLE-US-00001 TABLE 1 Example Example Example Example Example Example Classification 1-1 1-2 1-3 1-4 1-5 1-6 Manu- Catalyst Type Chemical Chemical Chemical Chemical Chemical Chemical facturing Formula Formula Formula Formula Formula Formula process 1-1 1-1 1-1 1-1 1-1 1-1 Content based on 15 15 15 10 20 15 Ti element (ppm) Polymerization 280 275 285 280 280 280 temperature ( C.) Resin IV (dL/g) 0.64 0.62 0.64 0.60 0.64 0.64 Carboxyl group (ea) 33 35 37 33 39 33 Staple Fineness (de) 1.2 1.2 1.2 1.2 1.2 0.3 yarn Average fiber length (mm) 5 5 5 5 5 5 Spinning workability (%) 100 100 100 100 100 110 Wiping cycle (times/day) 1 1 2 1 2 3 b* 4.2 4.3 5.1 4.3 4.0 4.2 Dispersibility (ppm) 5.4 6.8 8.6 9.2 9.8 4.9
TABLE-US-00002 TABLE 2 Compar- Compar- Compar- ative ative ative Example Example Example Example Example Example Classification 1-7 1-8 1-9 1-1 1-2 1-3 Manu- Catalyst Type Chemical Chemical Chemical Chemical Chemical Chemical facturing Formula Formula Formula Formula Formula Formula process 1-1 1-1 1-1 1-1 1-1 1-1 Content based on 15 15 15 15 15 5 Ti element (ppm) Polymerization 280 280 280 270 290 280 temperature ( C.) Resin IV (dL/g) 0.64 0.64 0.64 0.61 0.64 0.54 Carboxyl group (ea) 33 33 33 40 49 31 Staple Fineness (de) 3.0 1.2 1.2 1.2 1.2 1.2 yarn Average fiber length (mm) 5 3 12 5 5 5 Spinning workability (%) 85 100 100 100 100 100 Wiping cycle (times/day) 1 1 1 2 6 1 b* 4.2 4.2 4.2 4.5 6.2 5.9 Dispersibility (ppm) 6.9 5.1 7.5 10.5 37.9 11.3
TABLE-US-00003 TABLE 3 Compar- Compar- Compar- Compar- Compar- ative ative ative ative ative Example Example Example Example Example Classification 1-4 1-5 1-6 1-7 1-8 Manu- Catalyst Type Chemical Chemical Chemical Chemical Chemical facturing Formula Formula Formula Formula Formula process 1-1 1-1 1-1 1-1 1-1 Content based on 25 15 15 15 15 Ti element (ppm) Polymerization 280 280 280 280 280 temperature ( C.) Resin IV (dL/g) 0.66 0.64 0.64 0.64 0.64 Carboxyl group (ea) 45 33 33 33 33 Staple Fineness (de) 1.2 0.1 3.2 1.2 1.2 yarn Average fiber length (mm) 5 5 5 2 13 Spinning workability (%) 80 215 80 100 100 Wiping cycle (times/day) 5 9 1 1 1 b* 3.9 4.2 4.2 4.2 4.2 Dispersibility (ppm) 16.9 4.5 7.6 4.9 8.1
TABLE-US-00004 TABLE 4 Comparative Comparative Comparative Comparative Classification Example 1-9 Example 1-10 Example 1-11 Example 1-12 Manufac- Catalyst Type Antimony Antimony Antimony Antimony turing Trioxide Trioxide Trioxide Trioxide process Content based on Ti 15 20 20 25 element (ppm) Polymerization temperature 290 290 300 290 ( C.) Resin IV (dL/g) 0.59 0.64 0.68 0.67 Carboxyl group (ea) 65 63 80 67 Staple Fineness (de) 1.2 1.2 1.2 1.2 yarn Average fiber length (mm) 5 5 5 5 Spinning workability (%) 100 100 100 100 Wiping cycle (times/day) 6 5 7 6 b* 5.8 5.5 9.1 6.1 Dispersibility (ppm) 35.3 19.6 45.8 40.5
[0123] Looking at Tables 1 to 4 above, it was found that Examples 1-1 to 1-9 had excellent physical properties. On the other hand, in Comparative Example 1-1 having a final elevated temperature (polymerization temperature) of less than 275 C., there was a problem in that the dispersibility exceeded 10 ppm when compared with Example 1-2 in which the final elevated temperature (polymerization temperature) was 275 C.
[0124] In addition, when Comparative Example 1-2 in which the final elevated temperature (polymerization temperature) was more than 285 C. is compared with Example 1-3 in which the final elevated temperature (polymerization temperature) was 285 C., 40 or more carboxyl groups were measured in the resin, which indicated that the contamination was high, and the dispersibility of the fibers was significantly increased, and there was a problem in that the wiping cycle was shortened due to the easy contamination of the spinneret. In addition, it was found that the b value (b*) was high, and the yarn was yellowish.
[0125] In addition, when Comparative Examples 1-3 in which the titanium (Ti) element reference content of the titanium-based compound was less than 10 ppm is compared with Examples 1-4 in which the titanium (Ti) element reference content of the titanium-based compound was 10 ppm, it was found that the b value was excessively high, and the commercial use of the non-woven fabric was impossible, and the dispersibility also exceeded 10 ppm.
[0126] In addition, when Comparative Examples 1-4 in which the titanium (Ti) element reference content of the titanium-based compound was more than 20 ppm is compared with Examples 1-5 in which the titanium (Ti) element reference content of the titanium-based compound was 20 ppm, it was found that the carboxyl groups of the resin were measured excessively, the number of wiping due to contamination increased remarkably, and the dispersibility was excessively high.
[0127] In addition, when Comparative Examples 1-5 in which the fineness of the polyester staple yarn was less than 0.3 de is compared with Example 1-6 in which the fineness thereof was 0.3 de, the wiping cycle was found to be the most frequent, which was predicted to be a problem caused by excessive fineness.
[0128] Further, in Comparative Examples 1-9 to Comparative Examples 1-12 in which an antimony-based catalyst was used instead of a titanium-based compound, an excessive amount of carboxyl groups was detected, and also, it was confirmed that as the dispersibility was excessively high, it could not be used as a wet non-woven fabric.
Manufacture Example 1: Manufacture of Wet Non-Woven Fabric
[0129] The polyester staple yarn for a wet non-woven fabric manufactured in Example 1-1 and the binder staple yarn manufactured in Example 2-1 were prepared.
[0130] Then, after dispersing the binder staple yarn and polyester staple yarn in water at a weight ratio of 1:1.50, draining the water, drying under 100 C. and calendering under 240 C., a wet non-woven fabric having a basis weight of 75 g/m.sup.2 and an average thickness of 0.08 mm was manufactured.
Manufacture Example 2 to Manufacture Example 11 and Comparative Manufacture Example 1 to Comparative Manufacture Example 14: Manufacture of Wet Non-Woven Fabrics
[0131] Wet non-woven fabrics were manufactured in the same manner as in Manufacture Example 1, except that the polyester staple yarns for a wet non-woven fabric manufactured in Examples 1-2 to 1-9 or Comparative Examples 1-1 to 1-12 were used, or the weight ratio of the binder staple yarn and the polyester staple yarn was set as shown in Tables 5 to 9 below to perform Manufacture Examples 2 to 11 and Comparative Manufacture Example 1 to Comparative Manufacture Example 14.
Experimental Example 2: Evaluation of Physical Properties of Wet Non-Woven Fabrics
[0132] Specimens were prepared by cutting the wet non-woven fabrics manufactured in Manufacture Examples 1 to 11 and Comparative Manufacture Examples 1 to 14 to 150 mm100 mm. In addition, the test was performed on the specimens in the following way, and the results are shown in Tables 5 to 9 below.
[0133] (1) Measurement of Average of MD (Machine Direction) Tensile Strengths
[0134] For MD tensile strength, the specimen was tested 10 times at a temperature of 25 C. and at a speed of 20 mm/min through a tensile strength tester (HZ-1007E, MMS), and the average value was taken as the average tensile strength.
[0135] (2) Measurement of Standard Deviation of MD (Machine Direction) Tensile Strength
[0136] The standard deviation of MD tensile strengths was calculated by Relationship Formula 2-1 below.
[0137] In Relational Formula 2-1 above, means the standard deviation, N is the number of regions obtained by dividing a specimen obtained by cutting the wet non-woven fabric by 150 mm100 mm into N equal parts, N=10, l.sub.i is the MD tensile strength of the central part of the i.sup.th region, and is the average value of MD tensile strengths of the region divided into N equal parts, and
[0138] (3) Surface Touch (Tactile) Evaluation
[0139] The sensory evaluation was performed by 8 panelists by hand feeling, and relative evaluation was performed as follows. (1: very soft, 2: medium, 3: stiff or rough)
TABLE-US-00005 TABLE 5 Manufacture Manufacture Manufacture Manufacture Manufacture Classification Example 1 Example 2 Example 3 Example 4 Example 5 Polyester staple yarn Example 1-1 Example 1-2 Example 1-3 Example 1-4 Example 1-5 Binder staple yarn Example 2-1 Example 2-1 Example 2-1 Example 2-1 Example 2-1 Weight ratio 1:1.50 1:1.50 1:1.50 1:1.50 1:1.50 (Binder staple yarn:Staple yarn) Non- MD Average 156 153 150 154 150 woven tensile Standard 0.08 0.52 0.73 0.86 0.94 fabric strength deviation (N/15 mm) Touch feeling 1 1 1 2 2
TABLE-US-00006 TABLE 6 Manufacture Manufacture Manufacture Manufacture Manufacture Classification Example 6 Example 7 Example 8 Example 9 Example 10 Polyester staple yarn Example 1-6 Example 1-7 Example 1-8 Example 1-9 Example 1-1 Binder staple yarn Example 2-1 Example 2-1 Example 2-1 Example 2-1 Example 2-1 Weight ratio 1:1.50 1:1.50 1:1.50 1:1.50 1:1.20 (Binder staple yarn:Staple yarn) Non- MD Average 161 150 151 160 159 woven tensile Standard 0.15 0.11 0.11 0.14 0.12 fabric strength deviation (N/15 mm) Touch feeling 1 1 1 2 2
TABLE-US-00007 TABLE 7 Comparative Comparative Comparative Comparative Manufacture Manufacture Manufacture Manufacture Manufacture Classification Example 11 Example 1 Example 2 Example 3 Example 4 Polyester staple yarn Example 1-1 Comparative Comparative Comparative Comparative Example 1-1 Example 1-2 Example 1-3 Example 1-4 Binder staple yarn Example 2-1 Example 2-1 Example 2-1 Example 2-1 Example 2-1 Weight ratio 1:1.90 1:1.50 1:1.50 1:1.50 1:1.50 (Binder staple yarn:Staple yarn) Non- MD Average 152 148 132 143 139 woven tensile Standard 0.13 1.01 1.75 1.06 1.23 fabric strength deviation (N/15 mm) Touch feeling 1 3 3 3 3
TABLE-US-00008 TABLE 8 Comparative Comparative Comparative Comparative Comparative Manufacture Manufacture Manufacture Manufacture Manufacture Classification Example 5 Example 6 Example 7 Example 8 Example 9 Polyester staple yarn Comparative Comparative Comparative Comparative Comparative Example 1-5 Example 1-6 Example 1-7 Example 1-8 Example 1-9 Binder staple yarn Example 2-1 Example 2-1 Example 2-1 Example 2-1 Example 2-1 Weight ratio 1:1.50 1:1.50 1:1.50 1:1.50 1:1.50 (Binder staple yarn:Staple yarn) Non- MD Average 166 139 136 165 140 woven tensile Standard 0.16 0.09 0.13 0.13 0.32 fabric strength deviation (N/15 mm) Touch feeling 1 2 1 2 3
TABLE-US-00009 TABLE 9 Comparative Comparative Comparative Comparative Comparative Manufacture Manufacture Manufacture Manufacture Manufacture Classification Example 10 Example 11 Example 12 Example 13 Example 14 Polyester staple yarn Comparative Comparative Comparative Example 1-1 Example 1-1 Example 1-10 Example 1-11 Example 1-12 Binder staple yarn Example 2-1 Example 2-1 Example 2-1 Example 2-1 Example 2-1 Weight ratio 1:1.50 1:1.50 1:1.50 1:1.10 1:2.00 (Binder staple yarn:Staple yarn) Non- MD Average 140 132 142 164 144 woven tensile Standard 0.32 0.29 0.46 0.11 0.13 fabric strength deviation (N/15 mm) Touch feeling 3 3 3 3 1
[0140] Looking at Tables 5 to 9, it was found that Manufacture Examples 1 to 11 were non-woven fabrics having excellent physical properties. On the other hand, it was found that in Comparative Manufacture Examples 1 to 14, the tensile strength of the non-woven fabric was less than 150N/15 mm, the standard deviation of the tensile strengths was more than 1.0 N/15 mm, or the touch feeling on the surface of the nonwoven fabric was poor.
[0141] Although an exemplary embodiment of the present invention has been described above, the spirit of the present invention is not limited to the exemplary embodiments presented herein, and a person skilled in the art who understands the spirit of the present invention may easily suggest other exemplary embodiments by modifying, changing, deleting or adding components within the scope of the same spirit, but this will also fall within the spirit of the present invention.