CN1896346A - Preparation of multi-stage shrinkage polyester fibre by one-step method - Google Patents
Preparation of multi-stage shrinkage polyester fibre by one-step method Download PDFInfo
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- CN1896346A CN1896346A CN 200510040967 CN200510040967A CN1896346A CN 1896346 A CN1896346 A CN 1896346A CN 200510040967 CN200510040967 CN 200510040967 CN 200510040967 A CN200510040967 A CN 200510040967A CN 1896346 A CN1896346 A CN 1896346A
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Abstract
The present invention provides a one-step preparation process of multiple segment shrinkage polyester fibre. It uses terephthalic acid, isophthalic acid, glycol and ethoxybisphenol A as main materials to produce copolyester with intrinsic viscosity of 0.67-0.695 and melting point of 220DEG C-235DEG C. Via the crystallization, drying and screw extrusion of the copolyester, multiple segment shrinkage polyester fibre is prepared with low speed spinning and. The boiling water shrinkage is above 35% and the initial shrinkage temperature is above 75DEG C, and the fibre has high resistance to alkali. Furthermore, the fibre after shrinkage in boiling water will shrink 3.5% again when relaxing heat treating at 160DEG C. This fibre can act as twine to produce fabric with high adding value and special style.
Description
Technical field
The present invention relates to the production of modified polyester fiber, relate in particular to the production method of multi-stage shrinkage polyester fibre, be in particular a kind of preparation method of preparation of multi-stage shrinkage polyester fibre by one-step, belong to the synthetic fiber technical field.
Background technology
The thermal contraction of chemical fibre is a kind of very general phenomenon, and the boiling water shrinkage of conventional polyester fiber and dry-hot shrinkage are all lower, is 7～8% as the boiling water shrinkage of conventional polyester filament.Yet, it is diversified that the thermal contraction of fiber requires, shrink as secondary, high shrinkage stress or the like, in order to reach certain style requirement of fabric, often adopt the fiber Split Down of several different thermal contractions, wherein high-shrinkage fibre is main stress carrier, certain powerful requirement is arranged, taken on important role.
Prior art generally adopts the method for copolymerization chemical modification or physical modification (spinning technique adjusting) to make high-shrinkage fiber.The prior art of high-shrinkage fiber is only pursued the high boiling water shrinkage of fiber, and other performance relates to seldom.
First kind method is as the synthetic comonomer of polyester with M-phthalic acid, adipic acid, M-phthalic acid sodium, neopentyl glycol, adopt 4.5%～8% M-phthalic acid and adipic acid combined polymerization as patent JP3152213, the preparation inherent viscosity is 0.6～0.69 copolyesters, obtains the high-shrinkage fiber of boiling water shrinkage 〉=30%, 170 ℃ following dry-hot shrinkage 〉=20%, shrinkage stress 〉=0.15g/d through spinning.The application producer of these class methods has Yangzhou to synthesize chemical plant, Shandong chemical fibre group, Dong Li company etc., but because of adipic acid, sodiosulfoisophthalic acid not alkaline-resisting, the not alkaline-resisting processing of the high-contraction copolyester fiber that this method is made can not be used for preparing joint stock wire with islands-in-sea type fibre.
Another kind of method is to adopt the normal polyester section to be raw material, adopts cryogenic tensile, cryogenic shaping process, and preparation boiling water is punctured into 15%～60% polyester fiber.Though the polyester fiber that this method makes has very high apparent boiling water shrinkage, true shrinkage factor is not high, initial shrinkage temperature low (about 50 ℃), shrinkage factor instability.
In addition, the patent KR9311338 of Kolon company, the ethoxylation bisphenol-A that adopts the M-phthalic acid account for total dicarboxylic acid 0～10% molar fraction and total dicarboxylic acid 5～15% molar fractions be as comonomer, composite character viscosity [η]＞0.7 copolyester section.Section is through melt spinning, 120 ℃ of nervous HEAT SETTING 2 minutes down, obtains the polyester fiber that 170 ℃ of xeothermic contraction 〉=35%, secondary dry-hot shrinkage 〉=10%, shrinkage stress reach 1.0g/d.Though this patented method has than high shrinkage and shrinkage stress, but owing to added a large amount of ethoxylation bisphenol-As, the color of fiber is yellow, and the increase of high viscosity section ([η]＞0.7) production cost, and its 120 ℃ of nervous HEAT SETTING practical applications of 2 minutes are difficulty relatively.
On the whole, the high-shrinkage fibre that prior art for preparing obtains, its contraction behavior is more single, and fiber no longer shrinks even extends when xeothermic typing after shrinking through boiling water treating.For occasions such as the different contraction combined yarns of production, single contraction behavior can not meet the demands.
Summary of the invention
On the whole, the high-shrinkage fibre that prior art for preparing obtains, its contraction behavior is more single, and fiber no longer shrinks even extends when xeothermic typing after shrinking through boiling water treating.For occasions such as the different contraction combined yarns of production, single contraction behavior can not meet the demands.
The objective of the invention is to overcome the deficiency that prior art exists, provide a kind of one-step method preparation to have the method for the multi-stage shrinkage polyester fibre of superperformances such as stable high boiling water shrinkage, higher initial shrinkage temperature, excellent alkali resistance and multistage contraction behavior concurrently.
Purpose of the present invention is achieved through the following technical solutions:
The method of preparation of multi-stage shrinkage polyester fibre by one-step may further comprise the steps:
1. the preparation of copolyesters modification section---
With terephthalic acid (TPA) and M-phthalic acid is binary acid, the mole dosage of M-phthalic acid accounts for 10～15% of the total consumption of binary acid mole, with ethylene glycol and ethoxylation bisphenol-A is dihydroxylic alcohols, ethylene glycol is 1.15: 1～1.8: 1 with the ratio of the mole total amount of binary acid, and the consumption of ethoxylation bisphenol-A accounts for 3～5% of the total consumption of binary acid mole; Above-mentioned binary acid, dihydroxylic alcohols and catalyst preparation form slurry, under normal pressure～0.25MPa gauge pressure, 230 ℃～280 ℃ conditions, carry out esterification, when esterification yield reaches after 95%, reactant of esterification is 0.0 in vacuum～-carry out polycondensation reaction under the 0.99MPa, 285 ℃～290 ℃ conditions of temperature, prepare inherent viscosity and be 0.62～0.68 copolyesters modification section;
2. the spinning of copolyesters modification section---
Above-mentioned copolyesters modification section pre-crystallization 30～40 minutes under 100 ℃～130 ℃ temperature earlier, be lower than in-70 ℃ the dry air packed tower dry 16～20 hours at 100 ℃～130 ℃, dew point again, obtain the dried section of moisture content 40～60ppm, then under 200 ℃～290 ℃ temperature through the screw extruder melt extruded, melt is at 260 ℃～285 ℃ melt spinnings, through the coiling drafting process, make multi-stage shrinkage polyester fibre.
Further, in the method for above-mentioned preparation of multi-stage shrinkage polyester fibre by one-step, the 1. middle esterification of step divides two stages to carry out, and the phase I reaction condition is 0.15～0.25MPa gauge pressure, 230 ℃～260 ℃ temperature, and the second stage reaction condition is normal pressure, 260 ℃～280 ℃ temperature; Altered contents in the dihydroxylic alcohols---ethoxyquin bisphenol-A both can also can add reaction system before the esterification after esterification.
Again further, in the method for above-mentioned preparation of multi-stage shrinkage polyester fibre by one-step, step 2. described in the coiling drafting process can adopt the UDY-DT process route: fibre bundle earlier forms undrafting wire (UDY) under 600～800m/min spinning speed, and then is drawn into drawn yarn (DT) under the condition of 60 ℃～100 ℃ of draft temperatures, draw ratio 3.0～3.9; Also can adopt FDY technology: fibre bundle is directly processed and coiling and molding through first drawing roller and second drawing roller, two rollers, obtain fully oriented filament (FDY), wherein the process velocity of first drawing roller is that 600～800m/min, temperature are 60 ℃～100 ℃, and the process velocity 3200～4000m/min of second drawing roller, temperature are 90 ℃～120 ℃.
And, in the method for above-mentioned preparation of multi-stage shrinkage polyester fibre by one-step, step 1. described in catalyst be antimony triacetate or antimonous oxide, its consumption is 0.02～0.05% of a binary acid gross weight; Step 1. described in slurry in process for preparation, can also add heat stabilizers such as triphenyl phosphate, its consumption is 0.03～0.04% of a binary acid gross weight.
Substantive distinguishing features and obvious improvement that the present invention gives prominence to are mainly reflected in: the method that (1) its employing chemical modification combines with physical modification, be different from the high-shrinkage fiber that adopts normal polyester section cryogenic tensile prepared, its initial shrinkage temperature is greater than 75 ℃, and the Split Down silk can be applicable to the warping processed of warp thread; (2) high-shrinkage fiber for preparing of the present invention not only has alkali resistance preferably, and has the multistage heat-shrinkable, and fiber is through boiling water shrink process after-contraction 35%, and 160 ℃ of following heat treatments, fiber shrinks 3.5% once more again.This high shrinkage can be used as the Split Down silk, is used to prepare added value height, the special fabric of style.
The specific embodiment
The present invention adopts the chemical copolymerization modification to prepare the high-contraction copolyester fiber with the method that low speed spinning, low temperature, high magnification drawing process combine, and its key step is:
1. the preparation of high-contraction copolyester section: with terephthalic acid (TPA) (PTA) and M-phthalic acid (IPA) is dicarboxylic acid constituent, and wherein the mol ratio of IPA and PTA is 10/90～15/85; With ethylene glycol (EG) is main dihydroxylic alcohols, the ethoxylation bisphenol-A is a dihydroxylic alcohols modification composition, consumption is a benchmark with the integral molar quantity of binary acid all, the mole dosage of ethylene glycol is 1.15～1.8 times of mole total amount of binary acid, the consumption of ethoxylation bisphenol-A account for binary acid the mole total amount 3%～5%; Catalysts can be selected antimony triacetate or antimonous oxide for use, and its consumption is 0.02～0.05% of a binary acid gross weight; In addition, add the antioxidant of 1222 trades mark such as grade, its consumption is 0.03～0.04% of a binary acid gross weight.Above-mentioned material is mixed with slurry, under 0.15～0.25MPa gauge pressure, 230 ℃～260 ℃ temperature conditions, carries out the phase I esterification, under normal pressure and 260 ℃～280 ℃ temperature, carry out the second stage esterification; When esterification yield reaches after 95%, change reaction condition, with the product after the esterification vacuum 0.0～-carry out polycondensation reaction under the 0.99MPa, 285 ℃～290 ℃ conditions of temperature, obtain inherent viscosity [η] and be 0.62～0.68 copolyesters modification section.
2. the spinning of high-contraction copolyester section: the copolyesters modification that will above-mentionedly prepare is cut into slices under 100 ℃～130 ℃ temperature through ebullated bed or the pre-crystallization of rotary drum drier 30～40 minutes, be lower than in-70 ℃ the dry air packed tower dry 16～20 hours at 100 ℃～130 ℃ temperature, dew points again, obtaining moisture content is the dried section of 40～60ppm.With screw extruder melt extruded under 200 ℃～290 ℃ conditions, melt temperature is to carry out melt spinning under 260 ℃～285 ℃ conditions, through operations such as coiling drawing-offs, can make multi-stage shrinkage polyester fibre.
Wherein, the coiling draft process can adopt UDY-DT or two kinds of process routes of FDY:
One, UDY-DT process route: under 600～800m/min spinning speed, form undrafting wire (UDY), be drawn into drawn yarn (DT) then under the condition of 60 ℃～100 ℃ of draft temperatures, draw ratio 3.0～3.9, stretching device can adopt ring ingot device or the flat device that leads;
They are two years old, FDY process route: 60～80 ℃ of the first drawing roller speed, 600～800m/min, temperature, 90～100 ℃ of the second drawing roller speed, 3200～4000m/min, temperature through coiling and molding after this two rollers drawing-off, make high-shrinkage fibre fully oriented filament (FDY).
Two kinds of routes of above-mentioned UDY-DT and FDY all can spin the high-shrinkage polyester filaments of 30dtex/12f～50dtex/12f specification.
Enumerating exemplary embodiments below elaborates to technical solution of the present invention.
Terephthalic acid (TPA) (PTA): 450 parts (by weight, down together), M-phthalic acid (IPA): 50 parts, 230 parts of ethylene glycol (EG), The catalytic antimony trioxide (Sb
2O
3): 0.25 part, titanium dioxide (TiO
2) delustering agent: 1.8 parts.Above-mentioned material drops into reaction kettle of the esterification together, under 230 ℃～265 ℃ of temperature, gauge pressure 0.15MPa～0.25MPa, carry out esterification, reaction system is constantly emitted moisture, reach 110 parts to water yield, finish esterification, change material over to batch condensation polymerization reactor then, drop into 20 parts of ethoxylation bisphenol-As again, 260 ℃～280 ℃, vacuum 0.0～-carry out polycondensation reaction under the 0.99MPa condition.Judge the viscosity of material in reactor according to the power of agitator of batch condensation polymerization reactor, when material characteristic viscosity [η] when reaching 0.67, finish reaction, discharging, blank make the high modified poly ester section of shrinking.
Above-mentioned section through the pre-crystallization of ebullated bed 30 minutes, enters the paddle dryer tower then under 120 ℃ of temperature, in the dry air of 130 ℃, dew-point temperature-70 ℃ dry 18 hours, dry back section moisture content was about 50ppm.Set 220 ℃ of screw extruder one district's temperature, 280 ℃ of melt temperatures, section after the above-mentioned processing is melt extruded, under the condition of 280 ℃ of spinning body temperatures, lateral blowing 0.35m/min, 23 ℃ of lateral blowing temperature, humidity 65%, the first drawing roller speed 750m/min, 80 ℃ of the first drawing roller temperature, the second drawing roller speed 3200m/min, 100 ℃ of the second drawing roller temperature, winding speed 3150m/min, spinning makes fully oriented filament FDY then.
After testing, the polyester fiber that makes of said method has stable high boiling water shrinkage (〉=35%), higher initial shrinkage temperature (〉=75 ℃), excellent alkali resistance and multistage and shrinks behavior.Behind the fiber nature airing that boiling water shrank, again in 160 ℃ of heat treatments 3 minutes, fiber shrinks about 3.5% once more under relaxed state.
Claims (7)
1. the method for preparation of multi-stage shrinkage polyester fibre by one-step may further comprise the steps:
1. the preparation of copolyesters modification section---
With terephthalic acid (TPA) and M-phthalic acid is binary acid, the mole dosage of M-phthalic acid accounts for 10～15% of the total consumption of binary acid mole, with ethylene glycol and ethoxylation bisphenol-A is dihydroxylic alcohols, ethylene glycol is 1.15: 1～1.8: 1 with the ratio of the mole total amount of binary acid, and the consumption of ethoxylation bisphenol-A accounts for 3～5% of the total consumption of binary acid mole; Above-mentioned binary acid, dihydroxylic alcohols and catalyst preparation form slurry, under normal pressure～0.25MPa gauge pressure, 230 ℃～280 ℃ conditions, carry out esterification, when esterification yield reaches after 95%, reactant of esterification is 0.0 in vacuum～-carry out polycondensation reaction under the 0.99MPa, 285 ℃～290 ℃ conditions of temperature, prepare inherent viscosity and be 0.62～0.68 copolyesters modification section;
2. the spinning of copolyesters modification section---
Above-mentioned copolyesters modification section pre-crystallization 30～40 minutes under 100 ℃～130 ℃ temperature earlier, be lower than in-70 ℃ the dry air packed tower dry 16～20 hours at 100 ℃～130 ℃, dew point again, obtain the dried section of moisture content 40～60ppm, then under 200 ℃～290 ℃ temperature through the screw extruder melt extruded, melt is at 260 ℃～285 ℃ melt spinnings, through the coiling drafting process, make multi-stage shrinkage polyester fibre.
2. the method for preparation of multi-stage shrinkage polyester fibre by one-step according to claim 1, it is characterized in that: the 1. middle esterification of step divides two stages to carry out, the phase I reaction condition is 0.15～0.25MPa gauge pressure, 230 ℃～260 ℃ temperature, and the second stage reaction condition is normal pressure, 260 ℃～280 ℃ temperature.
3. the method for preparation of multi-stage shrinkage polyester fibre by one-step according to claim 1 and 2, it is characterized in that: the ethoxyquin bisphenol-A in the dihydroxylic alcohols adds reaction system before esterification or after the esterification.
4. the method for preparation of multi-stage shrinkage polyester fibre by one-step according to claim 1, it is characterized in that: step 2. described in the coiling drafting process be, fibre bundle forms undrafting wire earlier under 600～800m/min spinning speed, and then is drawn into drawn yarn under the condition of 60 ℃～100 ℃ of draft temperatures, draw ratio 3.0～3.9.
5. the method for preparation of multi-stage shrinkage polyester fibre by one-step according to claim 1, it is characterized in that: step 2. described in the coiling drafting process be, fibre bundle is directly processed and coiling and molding through first drawing roller and second drawing roller, two rollers, wherein the process velocity of first drawing roller is that 600～800m/min, temperature are 60 ℃～80 ℃, and the process velocity 3200～4000m/min of second drawing roller, temperature are 90 ℃～100 ℃.
6. the method for preparation of multi-stage shrinkage polyester fibre by one-step according to claim 1 is characterized in that: step 1. described in catalyst be antimony triacetate or antimonous oxide, its consumption is 0.02～0.05% of a binary acid gross weight.
7. the method for preparation of multi-stage shrinkage polyester fibre by one-step according to claim 1 is characterized in that: step 1. described in slurry in process for preparation, also add antioxidant, its consumption is 0.03～0.04% of a binary acid gross weight.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787583A (en) * | 2010-03-13 | 2010-07-28 | 浙江理工大学 | Method for preparing continuous polymerization directly-spun high-shrinkage polyester filaments |
| CN102154728A (en) * | 2011-03-09 | 2011-08-17 | 宁波大发化纤有限公司 | Preparation method of deoiled hard short fibers |
| CN101736417B (en) * | 2009-11-25 | 2012-01-25 | 彭书成 | Preparation method of modified polyester fiber and modified polyester fiber prepared by same |
| CN101525423B (en) * | 2008-03-04 | 2012-07-04 | 东丽纤维研究所（中国）有限公司 | High-contraction polyester and method for preparing same |
| CN108998850A (en) * | 2018-08-31 | 2018-12-14 | 江苏江南高纤股份有限公司 | High-shrinkage fiber, preparation method and preparation system |
| CN109137180A (en) * | 2018-10-22 | 2019-01-04 | 浙江四通新材料科技股份有限公司 | A kind of imitative wool carpet yarn preparation method of terylene twisting sizing |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2605298B2 (en) * | 1987-09-08 | 1997-04-30 | 東レ株式会社 | Polyester composition and method for producing the same |
| IT1226148B (en) * | 1988-07-04 | 1990-12-19 | Ausimont Spa | SEGMENTED THERMOPLASTIC COPOLYESTERS WITH ELASTOMERIC PROPERTIES. |
| JP2000265325A (en) * | 1999-03-15 | 2000-09-26 | Toray Ind Inc | Combined filament polyester yarn having shrinkage difference and its production |
| JP2002302836A (en) * | 2001-04-04 | 2002-10-18 | Nippon Ester Co Ltd | Spun yarn including latently crimpable fiber |
| CN1272359C (en) * | 2003-07-09 | 2006-08-30 | 中国石化上海石油化工股份有限公司 | Process for preparing modified polyester for the preparation of polyester fibre with high elasticity |
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2005
- 2005-07-11 CN CNB2005100409673A patent/CN100396829C/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525423B (en) * | 2008-03-04 | 2012-07-04 | 东丽纤维研究所（中国）有限公司 | High-contraction polyester and method for preparing same |
| CN101736417B (en) * | 2009-11-25 | 2012-01-25 | 彭书成 | Preparation method of modified polyester fiber and modified polyester fiber prepared by same |
| CN101787583A (en) * | 2010-03-13 | 2010-07-28 | 浙江理工大学 | Method for preparing continuous polymerization directly-spun high-shrinkage polyester filaments |
| CN102154728A (en) * | 2011-03-09 | 2011-08-17 | 宁波大发化纤有限公司 | Preparation method of deoiled hard short fibers |
| CN108998850A (en) * | 2018-08-31 | 2018-12-14 | 江苏江南高纤股份有限公司 | High-shrinkage fiber, preparation method and preparation system |
| CN109137180A (en) * | 2018-10-22 | 2019-01-04 | 浙江四通新材料科技股份有限公司 | A kind of imitative wool carpet yarn preparation method of terylene twisting sizing |
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Effective date of registration: 20160206 Address after: 211900 Yizheng Changjiang Road, Jiangsu, China, No. 1, No. Patentee after: CHINA SINOPEC YIZHENG CHEMICAL FIBER CO., LTD. Address before: 211900 No. 1 West Changjiang Road, Xu Town, Jiangsu City, Yizheng Province Patentee before: Yizheng Chemical Fiber Co., Ltd., China Petrochemical Group Corp. |