CN1439751A - Soluble thermokalite polyester fibre preparation - Google Patents
Soluble thermokalite polyester fibre preparation Download PDFInfo
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- CN1439751A CN1439751A CN 03112012 CN03112012A CN1439751A CN 1439751 A CN1439751 A CN 1439751A CN 03112012 CN03112012 CN 03112012 CN 03112012 A CN03112012 A CN 03112012A CN 1439751 A CN1439751 A CN 1439751A
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- 239000000835 fiber Substances 0.000 title claims abstract description 59
- 229920000728 polyester Polymers 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims description 25
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 title claims description 10
- 238000009987 spinning Methods 0.000 claims abstract description 24
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 8
- 239000011734 sodium Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 18
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 14
- 239000002202 Polyethylene glycol Substances 0.000 claims description 13
- 229920001223 polyethylene glycol Polymers 0.000 claims description 13
- 238000010009 beating Methods 0.000 claims description 9
- 239000012760 heat stabilizer Substances 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 229940011182 cobalt acetate Drugs 0.000 claims description 6
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 6
- 230000032050 esterification Effects 0.000 claims description 6
- 238000005886 esterification reaction Methods 0.000 claims description 6
- 238000005904 alkaline hydrolysis reaction Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 4
- 230000003078 antioxidant effect Effects 0.000 claims description 4
- 238000009998 heat setting Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- FYIBGDKNYYMMAG-UHFFFAOYSA-N ethane-1,2-diol;terephthalic acid Chemical compound OCCO.OC(=O)C1=CC=C(C(O)=O)C=C1 FYIBGDKNYYMMAG-UHFFFAOYSA-N 0.000 claims description 3
- 238000002074 melt spinning Methods 0.000 claims description 3
- 230000003252 repetitive effect Effects 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000003513 alkali Substances 0.000 abstract description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 4
- 235000019260 propionic acid Nutrition 0.000 description 4
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical compound CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 description 2
- MQWCQFCZUNBTCM-UHFFFAOYSA-N 2-tert-butyl-6-(3-tert-butyl-2-hydroxy-5-methylphenyl)sulfanyl-4-methylphenol Chemical compound CC(C)(C)C1=CC(C)=CC(SC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O MQWCQFCZUNBTCM-UHFFFAOYSA-N 0.000 description 2
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 2
- -1 pentaerythritol ester Chemical class 0.000 description 2
- LZFNKJKBRGFWDU-UHFFFAOYSA-N 3,6-dioxabicyclo[6.3.1]dodeca-1(12),8,10-triene-2,7-dione Chemical compound O=C1OCCOC(=O)C2=CC=CC1=C2 LZFNKJKBRGFWDU-UHFFFAOYSA-N 0.000 description 1
- 229920001634 Copolyester Polymers 0.000 description 1
- 206010042008 Stereotypy Diseases 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Artificial Filaments (AREA)
Abstract
A hot alkali-soluble polyester fibre is prepared through adding 5-sodium sulfonate-ethanediol metaphenyl diformate (SIPE), metaphenyl diformic acid (IPA) and polyethanediol, drying, fusing, spinning, and stretching or thermal deforming to obtain preoriented yarn (POY), drafted yarn (DY), or low-elasticity yarn. Its advantages are high solubility in alkali solution and spinnability and low viscosity.
Description
(1) technical field
The present invention relates to a kind of manufacture method of modified polyester fiber, particularly a kind of very easily dissolving in hot alkaline solution, the preparation method with conventional polymerization and the easy polyester fiber for preparing of spinning equipment belongs to chemical fiber field.
(2) background technology
Water-soluble fibre and conventional fibre are formed compound silk and are used to weave, and by solvent processing water-soluble fibre are removed again, increase interfibrous space, are used to make the fabric of mannerism.The water-soluble poly ester fiber had been carried out research, and the modified poly ester of opening the aliphatic dibasic acid preparation of the M-phthalic acid of 5-sulfonate-isophthalic acid component of having proposed to add 8-6 mole % in the clear 63-165516 communique, 5-20 mole % and 5-20 mole % as the spy is done one-component and is prepared the water-soluble poly ester fiber.The modified poly ester of the aliphatic ring binary acid preparation of 5-sulfonate-M-phthalic acid of Te Kaiping 4-327209 communique proposition interpolation 5-15 mole %, the M-phthalic acid of 30-70 mole % and 5-30 mole % is done one-component and is prepared the water-soluble poly ester fiber.The modified component of these copolyesters is more, causes the softening point of polyester lower, discharging difficulty when producing with present conventional polymerization unit, and the section bonding seriously can not high speed spinning during simultaneously with present conventional spinning equipment spinning.
(3) summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of preparation method of thermokalite soluble poly ester fiber is provided, prepared polyester fiber is very easily dissolving in hot alkaline solution, can easily carry out high speed spinning with conventional spinning equipment.
The preparation method of thermokalite soluble poly ester fiber comprises the preparation of modified poly ester and the preparation of fiber:
(1) preparation of polyester, constitute main repetitive ethylene glycol terephthalate by p-phthalic acid, ethylene glycol, the M-phthalic acid that in sour composition, contains 4-8 mole %, 5-sodium sulfonate-ethylene isophthalate with the 5-10% of p-phthalic acid and M-phthalic acid integral molar quantity, the mean molecule quantity that contains 6-12 weight % in polymer is the polyethylene glycol of 1000-8000 and contains heat stabilizer that polyester process makes the easy alkaline hydrolysis polyester of modification routinely;
(2) melt spinning after the above-mentioned polyester drying stretches or thermal deformation makes pre-oriented yarn (POY), drafted fibre (DT), low-stretch yarn various fibers such as (DTY).
The preparation of above-mentioned fiber is: this modified poly ester is carried out spinning with conventional spinning equipment, is 275～290 ℃ of extruder temperatures at spinning condition, spins 2000～3500 meters/minute of speed, makes preorientation POY fiber under the condition of wind speed 0.4～0.6 meter per second;
60～100 ℃ of drawing temperatures, spin 400～800 meters/minute of speed, 1.0～2.5 times of drafting multiples, the drafted fibre (DT) that makes under 150～190 ℃ of conditions of heat setting temperature with above-mentioned POY fiber.
Perhaps spin 400～800 meters/minute of speed with above-mentioned POY fiber, 1.0～2.0 times of drafting multiples make low-stretch yarn (DTY) under 150～190 ℃, 140～170 ℃ conditions of first, second heater temperature.
Above-mentioned heat stabilizer is made of following component:
A) have the antioxidant of sterically hindered phenol, addition is the 0.02-0.04% of weight polyester.
B) cobalt acetate, addition are the 0.01-0.03% of weight polyester.
C) phosphoric acid, phosphorous acid or its ester class, addition is the 0.01-0.03% of weight polyester.
Above-mentioned antioxidant is: four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), 2,2-thiobis (4-methyl-6-tert butyl phenol) (antioxidant 2246) or [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] octadecanol (antioxidant 1076).
Above-mentioned easy alkaline hydrolysis preparation process of polyester detailed process is as follows:
With ethylene glycol, p-phthalic acid, M-phthalic acid in accordance with regulations mol ratio join making beating still making beating, can add conventional catalyst etc. in the making beating still.Isophthalic acid comprises 4-8 mole % in acid constituents wherein, the mol ratio of ethylene glycol and acid is controlled between the 1.2-1.5.
Send into esterifying kettle and carry out esterification after above-mentioned slurry is even, add 5-sodium sulfonate-ethylene isophthalate (SIPE) after esterification is finished, its amount is the 5-10% of PTA, IPA integral molar quantity.
Stir and added the mean molecule quantity contain in 25 ~ 35 minutes and be the polyethylene glycol (PEG) of 1000-8000 and add heat stabilizer that the addition of polyethylene glycol is the 6-12% of weight polyester.
Heat stabilizer is made of following component:
A) have the antioxidant of sterically hindered phenol, addition is the 0.02-0.04% of weight polyester.
B) cobalt acetate, addition are the 0.01-0.03% of weight polyester.
C) phosphoric acid, phosphorous acid or its ester class, addition is the 0.01-0.03% of weight polyester.
Above-mentioned material stirred 25～35 minutes, method for making polyester production routinely.
Problems such as bigger fall in viscosity when the invention solves in the polymer that prior art exists bubble, poor heat resistance, melt spinning, and thermokalite soluble poly ester fiber of the present invention has sufficient buck dissolubility, melt when spinning viscosity and fall for a short time, and spinning operation is good.Concrete experimental data will provide in the following embodiments.
(4) specific embodiment
Embodiment 1:
The easily preparation of alkaline hydrolysis polyester: with 1000kg p-phthalic acid (PTA), 60kg (5.67% mole) M-phthalic acid (IPA), 500kg ethylene glycol (EG), polymerization catalyst antimonous oxide 0.32kg drops into the making beating of making beating still, enter esterifying kettle continuously after the making beating evenly, normal pressure esterification under 250--260 ℃ of temperature, esterification water outlet 220kg finishes, move into polymeric kettle, 5-sodium sulfonate-the ethylene isophthalate (SIPE) that adds 140kg (6.0% mole), stirred 30 minutes, the mean molecule quantity that adds 120kg (9.0%) is 4000 polyethylene glycol (PEG) and adds four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010): 0.4kg (0.03%), cobalt acetate 0.2kg (0.015%), trimethyl phosphate 0.2kg (0.015%), stirred 30 minutes, in low vacuum, temperature 240--270 ℃ of following precondensation, at high vacuum (less than 100Pa), 276～280 ℃ of polymerizations of temperature get easy alkaline hydrolysis polyester.
The preparation of POY fiber: this modified poly ester is carried out spinning with conventional spinning equipment, is 284 ℃ of extruder temperatures at spinning condition, spins 3200 meters/minute of speed, makes the POY fiber of 175dtex/36f under the condition of wind speed 0.5 meter per second.
The making of DT fiber: above-mentioned POY fiber is spinning 600 meters/minute of speed, 80 ℃ of drawing temperatures, 1.5 times of drafting multiples, the drafted fibre DT of the 101dtex/36f that makes under 185 ℃ of conditions of heat setting temperature.
The making of DTY fiber: above-mentioned POY fiber is spinning 500 meters/minute of speed, 1.4 times of drafting multiples, 180 ℃ of first heater temperatures, the low-stretch yarn DTY of the 110dtex/36F that makes under the condition that second heater temperature is 160 ℃.
This DT, DTY fiber carry out the alkali dissolution experiment with 1.5% sodium hydrate aqueous solution (bath raio 50,100 ℃ of temperature), and solubilized is complete in 10 minutes.
The leading indicator of fiber sees the following form.
| Project | ??POY | ??DT | ??DTY |
| Fiber number, dtex/36f | ??175.6 | ??101 | ??110 |
| Intensity, CN/dtex | ??1.29 | ??1.90 | ??1.83 |
| Elongation, % | ??120.3 | ??24.9 | ??26 |
Embodiment 2: as described in embodiment 1, different is,
The preparation of fiber is: at spinning condition is 286 ℃ of extruder temperatures, spins 2800 meters/minute of speed, makes fiber number 210dtex/36f, powerful 1.19CN/dtex under the condition of wind speed 0.5 meter per second, the POY fiber of elongation 145%.
Above-mentioned POY fiber is spinning 600 meters/minute of speed, 80 ℃ of drawing temperatures, 1.75 times of drafting multiples, the fiber number 105dtex/36f, the powerful 2.1CN/dtex that make under 186 ℃ of conditions of heat setting temperature, the DT fiber of elongation 20%.
This DT fiber carries out the alkali dissolution experiment with 1.5% sodium hydrate aqueous solution (bath raio 50,100 ℃ of temperature), and solubilized is complete in 8 minutes.
Embodiment 3: as described in embodiment 1, different is that the preparation of fiber is: at spinning condition is 286 ℃ of extruder temperatures, spins 2800 meters/minute of speed, make fiber number 210dtex/36f, powerful 1.19CN/dtex under the condition of wind speed 0.5 meter per second, the POY fiber of elongation 145%.
Above-mentioned POY fiber is spinning 490 meters/minute of speed, 1.7 times of drafting multiples, 180 ℃ of first heater temperatures, the fiber number 110dtex/36f that makes under the condition that second heater temperature is 165 ℃, powerful 1.80CN/dtex, the DTY fiber of elongation 24%.This DTY fiber carries out the alkali dissolution experiment with 1.5% sodium hydrate aqueous solution (bath raio 50,100 ℃ of temperature), and solubilized is complete in 10 minutes.
Embodiment 4: as described in embodiment 1, different is, the raw material of polyester manufacture is: the M-phthalic acid (IPA) that contains 5 moles of % in sour composition, 5-sodium sulfonate-ethylene isophthalate (SIPE) of 4% with p-phthalic acid and M-phthalic acid integral molar quantity, the mean molecule quantity that contains 9 weight % in polymer is 5000 polyethylene glycol (PEG), and contains following heat stabilizer:
A) 2,2-thiobis (4-methyl-6-tert butyl phenol) (antioxidant 2246), addition is 0.04% of a weight polyester,
B) cobalt acetate, addition are 0.02% of weight polyester,
C) phosphoric acid, addition are 0.015% of weight polyester.
Embodiment 5: as described in embodiment 1, different is
Constitute main repetitive ethylene glycol terephthalate by p-phthalic acid (PTA), ethylene glycol (EG), the M-phthalic acid (IPA) that in sour composition, contains 5 moles of %, 5-sodium sulfonate-ethylene isophthalate (SIPE) of 6% with p-phthalic acid and M-phthalic acid integral molar quantity, the mean molecule quantity that contains 7 weight % in polymer is 5000 polyethylene glycol (PEG), and contains following heat stabilizer:
A) [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] octadecanol (antioxidant 1076), addition is 0.025% of a weight polyester,
B) cobalt acetate, addition are 0.03% of weight polyester,
C) phosphorous acid, addition are 0.025% of weight polyester.
Claims (4)
1. the preparation method of thermokalite soluble poly ester fiber comprises the preparation of polyester and the preparation of fiber, it is characterized in that,
(1) preparation of polyester, constitute main repetitive ethylene glycol terephthalate by p-phthalic acid, ethylene glycol, the M-phthalic acid that in sour composition, contains 4-8 mole %, 5-sodium sulfonate-ethylene isophthalate with the 5-10% of p-phthalic acid and M-phthalic acid integral molar quantity, the mean molecule quantity that contains 6-12 weight % in polymer is the polyethylene glycol of 1000-8000 and contains heat stabilizer that polyester process makes the easy alkaline hydrolysis polyester of modification routinely;
(2) melt spinning after the above-mentioned polyester drying stretches or thermal deformation makes pre-oriented yarn, drafted fibre, low-stretch yarn thermokalite soluble poly ester fiber.
2. the preparation method of thermokalite soluble poly ester fiber as claimed in claim 1, it is characterized in that, the preparation of described fiber is: carry out spinning with conventional spinning equipment, spinning condition is 275～290 ℃ of extruder temperatures, spin 2000～3500 meters/minute of speed, wind speed 0.4～0.6 meter per second makes the preorientation fiber;
60～100 ℃ of drawing temperatures, spin 400～800 meters/minute of speed, 1.0～2.5 times of drafting multiples, the drafted fibre that makes under 150 ~ 190 ℃ of conditions of heat setting temperature with above-mentioned POY fiber;
Perhaps spin 400～800 meters/minute of speed with above-mentioned POY fiber, 1.0～2.0 times of drafting multiples make low-stretch yarn under 150～190 ℃, 140～170 ℃ conditions of first, second heater temperature.
3. the preparation method of thermokalite soluble poly ester fiber as claimed in claim 1 is characterized in that, described heat stabilizer is made of following component:
A) have the antioxidant of sterically hindered phenol, addition is the 0.02-0.04% of weight polyester,
B) cobalt acetate, addition are the 0.01-0.03% of weight polyester,
C) phosphoric acid, phosphorous acid or its ester class, addition is the 0.01-0.03% of weight polyester.
4. the preparation method of thermokalite soluble poly ester fiber as claimed in claim 1, it is characterized in that, the preparation of described polyester be with ethylene glycol, p-phthalic acid, M-phthalic acid in accordance with regulations mol ratio join making beating still making beating, can add conventional catalyst in the making beating still, isophthalic acid comprises 4-8 mole % in acid constituents wherein, the mol ratio of ethylene glycol and acid is controlled between the 1.2-1.5; Send into esterifying kettle and carry out esterification after above-mentioned slurry is even, add 5-sodium sulfonate-ethylene isophthalate after esterification is finished, its amount is the 5-10% of p-phthalic acid, M-phthalic acid integral molar quantity; Stir and added the mean molecule quantity contain in 25～35 minutes and be the polyethylene glycol of 1000-8000 and add heat stabilizer that the addition of polyethylene glycol is the 6-12% of weight polyester.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 03112012 CN1219116C (en) | 2003-03-20 | 2003-03-20 | Soluble thermokalite polyester fibre preparation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03112012 CN1219116C (en) | 2003-03-20 | 2003-03-20 | Soluble thermokalite polyester fibre preparation |
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| CN1439751A true CN1439751A (en) | 2003-09-03 |
| CN1219116C CN1219116C (en) | 2005-09-14 |
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| CN 03112012 Expired - Fee Related CN1219116C (en) | 2003-03-20 | 2003-03-20 | Soluble thermokalite polyester fibre preparation |
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| CN1317315C (en) * | 2004-07-08 | 2007-05-23 | 厦门翔鹭化纤股份有限公司 | Modified poly ester and its preparing method |
| CN100348641C (en) * | 2004-11-12 | 2007-11-14 | 中国石油天然气集团公司 | Alkali soluble polyester chip and its prepn |
| US7910207B2 (en) | 2004-03-30 | 2011-03-22 | Teijin Fibers Limited | Islands-in-sea type composite fiber and process for producing same |
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- 2003-03-20 CN CN 03112012 patent/CN1219116C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
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