A low chromatic aberration polyester different-shrinkage composite yarn and its preparation method

Abstract

A low chromatic aberration polyester different-shrinkage composite yarn is made of polyester POY yarn and polyester FDY composite yarn. The polyester POY yarn and polyester FDY yarn is obtained by spinning the polyester solution, the rupture strength of the low color polyester different-shrinkage composite yarn is 1.9 cN/dtex, the elongation at break is 30.05.0%, the crimp shrinkage is 2.503.0%, the network degree is 205/m, the color difference E is less than 0.200. In the invention, the magnesium ethylene glycol is relatively mild, the thermal degradation coefficient is small, the oligomers in the polymerization process is reduced, and the oligomers in the dissolution process are further reduced, so that the appearance of stains and streaks reduces during the dyeing and post-processing heat setting of the polyester fiber, which ensures the fiber's leveling and rubbing fastness.

Claims

1. A low chromatic aberration polyester different-shrinkage composite yarn comprising a composite of polyester POY yarn and polyester FDY yarn; wherein the polyester POY yarn and the polyester FDY yarn are obtained by spinning after dissolving the polyester; wherein a breaking strength of the low chromatic aberration polyester different-shrinkage composite yarn is greater than or equal to 1.9 cN/dtex, a breaking elongation is 30.05.0% and a curling shrinkage is 2.53.0%, a network degree is 205/m, a color difference E is less than 0.200, wherein the polyester is made after an esterification of terephthalic acid and ethylene glycol and a polycondensation under the catalysis of a mixture of magnesium ethylene glycol and antimony ethylene glycol, and finally granulation to obtain polyester chips; wherein in a slice of industrial polyester, a content of oligomer by mass is less than 0.5% and a content of diethylene glycol is less than 0.5%; wherein the molecular formula of magnesium ethylene glycol is Mg(OCH.sub.2CH.sub.2OH).sub.2; wherein the granulated slices are brewed and washed with water and a rinsing agent at 120-130 C. and 0.2-0.3 MPa.

2. The low chromatic aberration polyester different-shrinkage composite yarn according to claim 1, wherein the low chromatic aberration polyester different-shrinkage composite yarn has a linear density deviation of 2.5%, an elongation at break CV value is 10.0%, coefficient of variation CV value is 10.0%, an oil content of 1.00.2%, and a fineness of 100-150 dtex.

3. The low chromatic aberration polyester different-shrinkage composite yarn according to claim 1, wherein the mixture of magnesium ethylene glycol and antimony ethylene glycol has magnesium ethylene glycol and antimony ethylene glycol in a mass ratio of 2:1 to 3:1.

4. A method for preparing a low chromatic aberration polyester different-shrinkage composite yarn, the method comprising: spinning a polyester by a POY method and a FDY method, and then plying and wiring, composite, winding a final formation of the low chromatic aberration polyester different shrinkage composite yarn.

5. The method according to claim 4, further comprising: preparing magnesium ethylene glycol, adding ethylene glycol is in a single-compartment electrolytic cell, wherein magnesium chloride is a supporting electrolyte, an anode is comprised of magnesium, a cathode is graphite; operating the single-compartment electrolytic cell is at 50 to 60 for 10 to 12 h under DC, at an initial voltage of 6 to 10V, a cathodic current density of 150 to 200 mA; after the electrolysis, a white suspension liquid is obtained followed by removing the electrodes, decompression filtration and washing by anhydrous alcohol, the obtain the magnesium ethylene glycol after drying; performing the esterification and polycondensation to prepare polyester, using terephthalic acid and ethylene glycol as raw materials for the esterification reaction, adding a polyether-inhibitor to obtain esterification products after the esterification reaction; wherein the esterification reaction is performed at a pressure controlled in the scale of atmospheric pressure to 0.3 MPa, and a temperature controlled between 250 to 260; the esterification reaction is completed after an amount of distillate water in the esterification reaction reaches at least at 90% of a theoretical value; performing a condensation reaction, including a low vacuum stage and a high vacuum stage of the condensation reaction, wherein, in the low vacuum stage of the condensation reaction, adding a catalyst and a stabilizer into a product obtained from the esterification reaction; wherein the condensation reaction is performed under a negative pressure, where the pressure is decreased gradually from the atmospheric pressure to a pressure lower than the absolute pressure 500 Pa, and a temperature of the condensation reaction is controlled between 260 to 270; wherein the reaction is carried out for 30 to 50 mins, wherein the catalyst is the mixture of magnesium ethylene glycol and antimony ethylene glycol; in the high vacuum stage of the condensation reaction, continuously pumping vacuum after the low vacumm stage of the condensation reaction to an absolute pressure lower than 100 Pa, the low vacuum stage of the condensation reaction temperature is controlled between 275 to 280 C., and the low vacuum stage of the condensation reaction is carried out for 50 to 90 mins; then preparing the polyester section through granulation; scouring and washing the polyester section with water and a rinsing agent at 120 to 130 C. and 0.2 to 0.3 MPa for 3 to 5 h followed by washing with water; wherein spinning parameters include a spinning temperature of 280 to 300 C., an air temperature of 20 to 22 C., a joint stock network pressure of 3.5 to 4.5 bar, a GR1 speed of 800 to 1000 m/min, an SR1 speed of 3000 to 4200 m/min, a GR2 speed of 3000 to 4000 m/min, a HT1 temperature of 90 to 115 C., a HT2 temperature of 130 to 140 C. and a winding speed of 3000 to 4000 m/min.

6. The method according to claim 4 to 5, wherein a molar ratio of the ethylene glycol to terephthalic acid is 1.2:1 to 2.0:1.

7. The method according to claim 5, wherein, in the mixture of magnesium ethylene glycol and antimony ethylene glycol, a mass ratio of the magnesium ethylene glycol and the antimony ethylene glycol is from 2:1 to 3:1; an amount of the catalyst is 0.01% to 0.05% of the mass of the terephthalic acid; the stabilizer is selected from the group consisting of triphenyl phosphate, trimethyl phosphate and trimethyl phosphite, wherein the stabilizer is used in an amount of 0.01% to 0.05% of the weight of the terephthalic acid.

8. The method according to claim 5, wherein a mass ratio of water to the rinsing agent is 100:4 to 100:3, and a ratio of polyester section to water and the rinsing agent is 1:5-10, the rinsing agent is selected from the group consisting of 2-ethoxyethanol, 2-propoxyethanol and ethylene glycol monobutyl ether.

9. The method according to claim 5, wherein the cleaning is performed by washing the polyester sections with 70-80 C. water for 10-15 min after scouring the polyester sections, then washing with cold water, and drying and cooling down to make the sections.

10. The method according to claim 5, wherein the polyether inhibitor is selected from the group consisting of sodium acetate and calcium acetate, wherein the mass of the polyether inhibitor agent is 0.01-0.05% of terephthalic acid.

Description

DETAILED DESCRIPTION

[0054] Hereinafter, the present invention will be described in more detail by the following examples, but not limited thereto.

[0055] The process for preparing the low-chromatic aberration polyester shrink-wrapped composite yarn according to the invention is that the polyesters are respectively spun by applying the POY process and the FDY process, then plied and combined, and then subjected to network compaction and finally wound to form isocomplexed composite strands.

1. Dye:

[0056] Disperse Brilliant Blue 2BLN, 5% (o.w.f)

2. Dyeing Process:

[0057] The fibers are incubated at 70-80 C. for 10-15 min, and the heating rate is 1.0-2.0 C./min, the temperature is maintained at 120-130 C. for 40-60 min, the temperature is reduced, and the samples are reduced and washed at 70-80 C. for 20-30 min.

3. The Percentage of Dye Determination

[0058] According to the above process for dyeing, and were dyed dye solution, the residual solution of 2 ml in 10 ml volumetric flask, add acetone 4 ml, the dye fully dissolved. Diluted with distilled water to the mark, and then measured max spectrophotometer, when the dye absorbance A0, A1 is:

Dyeing percentage (%)=(1aA1/A0)100%

[0059] Where: A0 - - - dye solution before absorbance

[0060] A1 - - - Residue absorbance

4. Determination of Color Fastness

[0061] Press GB3920-83, GB251-64, GB3921-83 test

5. Color Yield and Color Measurement

[0062] Color measurement using colorimeter test.

6. The Determination of Apparent Color Depth (K/S)

[0063] The Kubelka-munk function is used in the formula: K/S=(1R) 2//2R where K is the absorption coefficient of the measured object, S is the scattering coefficient of the measured object, R is the measured object when the infinite thickness of the reflectivity. Apply the SF600X Datacolor colorimetric colorimeter test, each sample tested in different regions 5 times, whichever is the mathematical average.

Example 1

[0064] a low chromatic aberration polyester different-shrinkage composite yarn, wherein the main process is:

1. Preparation of Catalyst Magnesium Glycol:

[0065] Add ethylene glycol into the single-compartment electrolytic cell, magnesium chloride is electrolyte, the anode is magnesium, the cathode is graphite. Under DC, the initial voltage is 6V, the cathode current density is 150 mA, and electrolysis is carried out for 10 hours at 50 C. Remove the electrode after the electrolysis, we can get white suspension. Filter it under reduced pressure, wash the white solid with anhydrous ethanol, and we get magnesium ethylene glycol.

2. Preparation of Polyester, Including Esterification and Polycondensation:

[0066] Esterification Reaction:

[0067] Using terephthalic acid and ethylene glycol as raw materials, ethylene glycol and terephthalic acid molar ratio of 1.2:1, adding polyether-inhibitor sodium acetate, sodium acetate dosage of terephthalic acid in an amount of 0.01% by weight. Start esterification reaction under nitrogen atmosphere pressure, and control the pressure at atmospheric pressure, the temperature at 250 C. When esterified water distillate amount reaches 91% of the theoretical value of the esterification, reaction ends.

[0068] Polycondensation Reaction:

[0069] Including polycondensation reaction of low vacuum phase and polycondensation reaction high vacuum phase:

[0070] In the polycondensation reaction low-vacuum stage, add catalyst and the stabilizer acid triphenyl ester into the esterification product. The acid triphenyl ester dosage is 0.01% of terephthalic acid by weight, and the amount of catalyst is 0.01% of terephthalic acid by mass. The polycondensation reaction is started under the condition of negative pressure, the pressure is steadily pumped from the atmospheric pressure to the absolute pressure of 498 Pa, the temperature is controlled at 260 C., and the reaction time is 30 minutes. The catalyst is a mixture of magnesium ethylene glycol and antimony ethylene glycol, in which magnesium glycol and antimony ethylene glycol mass ratio is 2:1;

[0071] After the polycondensation reaction in the low-vacuum stage, the vacuum is continued to reduce the reaction pressure to 98 Pa, the reaction temperature is controlled at 275 C., and the reaction time is 50 minutes. The polyester sections are obtained by granulation.

3. Solvent Cleaning

[0072] Polyester sections are washed with water and rinsing agengt ethylene glycol monoethyl ether at 120 C. and 0.2 MPa for 3 hours. After washing, the polyester sections are washed with hot water at 70 C. for 10 minutes and then washed with cold water. After drying and cooling, the mass ratio of water to the rinsing agengt is 100:3, the ratio of the polyester slice to the water and the rinsing agengt, that is, the solid to liquid ratio is 1:5.

4. The Main Process Parameters of Spinning:

[0073] Spinning temperature: 280 C.,

[0074] Air temperature: 20 C.,

[0075] Joint stock network pressure: 3.5 bar,

[0076] GR1 speed: 800 m/min,

[0077] SR1 speed: 3000 m/min,

[0078] GR2 speed: 3000 m/min,

[0079] HT1 temperature: 90 C.,

[0080] HT2 temperature: 130 C.,

[0081] Winding speed: 3000 m/min.

[0082] The prepared low shrinkage polyester heterocomplex composite yarn has a breaking strength of 1.9 cN/dtex, and breaking extension is 35%, the crimp shrinkage is 5.5%, the network degree is 24/m, the linear density deviation rate is +2.5%, CV value of breaking extension is 9.8%, CV coefficient of variation is 9.8%, oil content is 1.2%, fineness: 100 dtex.

5. Dyeing

[0083]

TABLE-US-00001 chromatic Dyeing aberration Sample rate % K/S value E Common products 81.8 20.76 0.633 Low-chromatic 89.1 22.78 0.125 aberration products Soaping fastness Polyester Cotton Dry Wet Sample staining staining friction friction Common products 4 4 4 3 Low-chromatic 5 5 5 4 aberration products

Example 2

[0084] a low chromatic aberration polyester different-shrinkage composite yarn, wherein the main process is:

1. Preparation of Catalyst Magnesium Glycol:

[0085] Add ethylene glycol into the single-compartment electrolytic cell, magnesium chloride is electrolyte, the anode is magnesium, the cathode is graphite. Under DC, the initial voltage is 10V, the cathode current density is 200 mA, and electrolysis is carried out for 12 hours at 60 C. Remove the electrode after the electrolysis, we can get white suspension. Filter it under reduced pressure, wash the white solid with anhydrous ethanol, and we get magnesium ethylene glycol.

2. Preparation of Polyester, Including Esterification and Polycondensation:

[0086] Esterification Reaction:

[0087] Using terephthalic acid and ethylene glycol as raw materials, ethylene glycol and terephthalic acid molar ratio of 2.0:1, adding polyether-inhibitor calcium acetate, calcium acetate dosage of terephthalic acid in an amount of 0.05% by weight. Start esterification reaction under nitrogen atmosphere pressure, and control the pressure at 0.3 MPa, the temperature at 260 C. When esterified water distillate amount reaches 92% of the theoretical value of the esterification, reaction ends.

[0088] Polycondensation Reaction:

[0089] Including Polycondensation Reaction of Low Vacuum Phase and Polycondensation Reaction High Vacuum Phase:

[0090] In the polycondensation reaction low-vacuum stage, add catalyst and the stabilizer trimethyl phosphate into the esterification product. The trimethyl phosphate dosage is 0.05% of terephthalic acid by weight, and the amount of catalyst is 0.05% of terephthalic acid by mass. The polycondensation reaction is started under the condition of negative pressure, the pressure is steadily pumped from the atmospheric pressure to the absolute pressure of 496 Pa, the temperature is controlled at 270 C., and the reaction time is 40 minutes. The catalyst is a mixture of magnesium ethylene glycol and antimony ethylene glycol, in which magnesium glycol and antimony ethylene glycol mass ratio is 3:1:

[0091] After the polycondensation reaction in the low-vacuum stage, the vacuum is continued to reduce the reaction pressure to 95 Pa, the reaction temperature is controlled at 280 C., and the reaction time is 90 minutes. The polyester sections are obtained by granulation.

3. Solvent Cleaning

[0092] Polyester sections are washed with water and rinsing agengt ethylene glycol monopropyl ether at 130 C. and 0.3 MPa for 5 hours. After washing, the polyester sections are washed with hot water at 80 C. for 15 minutes and then washed with cold water. After drying and cooling, the mass ratio of water to the rinsing agengt is 100:4, the ratio of the polyester slice to the water and the rinsing agengt, that is, the solid to liquid ratio is 1:10;

4. The Main Process Parameters of Spinning:

[0093] Spinning temperature: 300 C.,

[0094] Air temperature: 22 C.

[0095] Joint stock network pressure: 4.5 bar,

[0096] GR1 speed: 1000 m/min,

[0097] SR1 speed: 4200 m/min,

[0098] GR2 speed: 4000 m/min,

[0099] HT1 temperature: 115 C.,

[0100] HT2 temperature: 140 C.,

[0101] Winding speed: 4000 m/min.

[0102] The prepared low shrinkage polyester heterocomplex composite yarn has a breaking strength of 1.9 cN/dtex, and breaking extension is 25.0%, the crimp shrinkage is 0.5%, the network degree is 15/m, the linear density deviation rate is 2.5%, CV value of breaking extension is 8.9%, CV coefficient of variation is 9.7%, oil content is 0.8%, fineness: 105 dtex.

5. Dyeing

[0103]

TABLE-US-00002 chromatic Dyeing aberration Sample rate % K/S value E Common products 81.8 20.76 0.633 Low-chromatic 93.1 25.75 0.143 aberration products Soaping fastness Polyester Cotton Dry Wet Sample staining staining friction friction Common products 4 4 4 3 Low-chromatic 5 5 5 5 aberration products

Example 3

[0104] a low chromatic aberration polyester different-shrinkage composite yarn, wherein the main process is:

1. Preparation of Catalyst Magnesium Glycol:

[0105] Add ethylene glycol into the single-compartment electrolytic cell, magnesium chloride is electrolyte, the anode is magnesium, the cathode is graphite. Under DC, the initial voltage is 7V, the cathode current density is 160 mA, and electrolysis is carried out for 11 hours at 55 C. Remove the electrode after the electrolysis, we can get white suspension. Filter it under reduced pressure, wash the white solid with anhydrous ethanol, and we get magnesium ethylene glycol.

2. Preparation of Polyester. Including Esterification and Polycondensation:

[0106] Esterification Reaction:

[0107] Using terephthalic acid and ethylene glycol as raw materials, ethylene glycol and terephthalic acid molar ratio of 1.5:1, adding polyether-inhibitor calcium acetate, calcium acetate dosage of terephthalic acid in an amount of 0.02% by weight. Start esterification reaction under nitrogen atmosphere pressure, and control the pressure at 0.2 MPa, the temperature at 255 C. When esterified water distillate amount reaches 92% of the theoretical value of the esterification, reaction ends.

[0108] Polycondensation Reaction:

[0109] Including Polycondensation Reaction of Low Vacuum Phase and Polycondensation Reaction High Vacuum Phase:

[0110] In the polycondensation reaction low-vacuum stage, add catalyst and the stabilizer trimethyl phosphate into the esterification product. The trimethyl phosphate dosage is 0.02% of terephthalic acid by weight, and the amount of catalyst is 0.02% of terephthalic acid by mass. The polycondensation reaction is started under the condition of negative pressure, the pressure is steadily pumped from the atmospheric pressure to the absolute pressure of 496 Pa, the temperature is controlled at 265 C., and the reaction time is 35 minutes. The catalyst is a mixture of magnesium ethylene glycol and antimony ethylene glycol, in which magnesium glycol and antimony ethylene glycol mass ratio is 3:1:

[0111] After the polycondensation reaction in the low-vacuum stage, the vacuum is continued to reduce the reaction pressure to 98 Pa, the reaction temperature is controlled at 277 C., and the reaction time is 60 minutes. The polyester sections are obtained by granulation.

3. Solvent Cleaning

[0112] Polyester sections are washed with water and rinsing agengt ethylene glycol monopropyl ether at 125 C. and 0.2 MPa for 3 hours. After washing, the polyester sections are washed with hot water at 70 C. for 15 minutes and then washed with cold water. After drying and cooling, the mass ratio of water to the rinsing agengt is 100:4, the ratio of the polyester slice to the water and the rinsing agengt, that is, the solid to liquid ratio is 1:10;

4. The Main Process Parameters of Spinning:

[0113] Spinning temperature: 290 C.,

[0114] Air temperature: 21 C.,

[0115] Joint stock network pressure: 3.8 bar,

[0116] GR1 speed: 900 m/min,

[0117] SR1 speed: 3500 m/min,

[0118] GR2 speed: 3500 m/min,

[0119] HT1 temperature: 100 C.,

[0120] HT2 temperature: 135 C.,

[0121] Winding speed: 3200 m/min.

[0122] The prepared low shrinkage polyester heterocomplex composite yarn has a breaking strength of 2.3 cN/dtex, and breaking extension is 26.0%, the crimp shrinkage is 4.5%, the network degree is 16/m, the linear density deviation rate is 2.5%, CV value of breaking extension is 9.1%, CV coefficient of variation is 9.9%, oil content is 0.9%, fineness: 132 dtex.

5. Dyeing

[0123]

TABLE-US-00003 chromatic Dyeing aberration Sample rate % K/S value E Common products 81.8 20.76 0.633 Low-chromatic 92.2 22.87 0.137 aberration products Soaping fastness Polyester Cotton Dry Wet Sample staining staining friction friction Common products 4 4 4 3 Low-chromatic 5 5 5 5 aberration products

Example 4

[0124] a low chromatic aberration polyester different-shrinkage composite yarn, wherein the main process is:

1. Preparation of Catalyst Magnesium Glycol:

[0125] Add ethylene glycol into the single-compartment electrolytic cell, magnesium chloride is electrolyte, the anode is magnesium, the cathode is graphite. Under DC, the initial voltage is 7V, the cathode current density is 170 mA, and electrolysis is carried out for 11 hours at 58 C. Remove the electrode after the electrolysis, we can get white suspension. Filter it under reduced pressure, wash the white solid with anhydrous ethanol, and we get magnesium ethylene glycol.

2. Preparation of Polyester, Including Esterification and Polycondensation:

[0126] Esterification Reaction:

[0127] Using terephthalic acid and ethylene glycol as raw materials, ethylene glycol and terephthalic acid molar ratio of 1.8:1, adding polyether-inhibitor calcium acetate, calcium acetate dosage of terephthalic acid in an amount of 0.02% by weight. Start esterification reaction under nitrogen atmosphere pressure, and control the pressure at 0.3 MPa, the temperature at 250 C. When esterified water distillate amount reaches 98% of the theoretical value of the esterification, reaction ends.

[0128] Polycondensation Reaction:

[0129] Including Polycondensation Reaction of Low Vacuum Phase and Polycondensation Reaction High Vacuum Phase:

[0130] In the polycondensation reaction low-vacuum stage, add catalyst and the stabilizer trimethyl phosphate into the esterification product. The trimethyl phosphate dosage is 0.02% of terephthalic acid by weight, and the amount of catalyst is 0.02% of terephthalic acid by mass. The polycondensation reaction is started under the condition of negative pressure, the pressure is steadily pumped from the atmospheric pressure to the absolute pressure of 496 Pa, the temperature is controlled at 264 C., and the reaction time is 38 minutes. The catalyst is a mixture of magnesium ethylene glycol and antimony ethylene glycol, in which magnesium glycol and antimony ethylene glycol mass ratio is 3:1;

[0131] After the polycondensation reaction in the low-vacuum stage, the vacuum is continued to reduce the reaction pressure to 99 Pa, the reaction temperature is controlled at 280 C., and the reaction time is 90 minutes. The polyester sections are obtained by granulation.

3. Solvent Cleaning

[0132] Polyester sections are washed with water and rinsing agengt ethylene glycol monopropyl ether at 120 C. and 0.3 MPa for 3 hours. After washing, the polyester sections are washed with hot water at 70 C. for 15 minutes and then washed with cold water. After drying and cooling, the mass ratio of water to the rinsing agengt is 100:4, the ratio of the polyester slice to the water and the rinsing agengt, that is, the solid to liquid ratio is 1:8.

4. The Main Process Parameters of Spinning:

[0133] Spinning temperature: 280 C.,

[0134] Air temperature: 20 C.,

[0135] Joint stock network pressure: 4.5 bar,

[0136] GR1 speed: 1000 m/min,

[0137] SR1 speed: 3000 m/mm,

[0138] GR2 speed: 3000 m/min,

[0139] HT1 temperature: 90 C.,

[0140] HT2 temperature: 140 C.,

[0141] Winding speed: 3000 m/min.

[0142] The prepared low shrinkage polyester heterocomplex composite yarn has a breaking strength of 2.3 cN/dtex, and breaking extension is 26.0%, the crimp shrinkage is 5.5%, the network degree is 15/m, the linear density deviation rate is 2.5%, CV value of breaking extension is 9.2%, CV coefficient of variation is 9.3%, oil content is 0.8%, fineness: 150 dtex.

5. Dyeing

[0143]

TABLE-US-00004 chromatic Dyeing aberration Sample rate % K/S value E Common products 81.8 20.76 0.633 Low-chromatic 92.8 25.85 0.156 aberration products Soaping fastness Polyester Cotton Dry Wet Sample staining staining friction friction Common products 4 4 4 3 Low-chromatic 5 5 5 5 aberration products