CN106592003A - Direct spinning preparation method of hydrolysis-resistant and anti-ageing polyester staple fiber - Google Patents
Direct spinning preparation method of hydrolysis-resistant and anti-ageing polyester staple fiber Download PDFInfo
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- CN106592003A CN106592003A CN201510665369.9A CN201510665369A CN106592003A CN 106592003 A CN106592003 A CN 106592003A CN 201510665369 A CN201510665369 A CN 201510665369A CN 106592003 A CN106592003 A CN 106592003A
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Abstract
The invention discloses a direct spinning preparation method of hydrolysis-resistant and anti-ageing polyester staple fiber. The hydrolysis-resistant and anti-ageing polyester staple fiber is prepared from a hydrolysis-resistant polyester melt with the intrinsic viscosity of 0.680-0.720 dl/g through procedures including heat exchange of the melt, melt spinning, circular blowing cooling, coiling, bundling, stretching, tension heat setting, relaxation heat setting, cutting, packaging of a finished product and the like. In the preparation process, the spinning temperature is 280-295 DEG C, the spinning speed is 1,200-1,600 m/min, the total drafting rate is 3.0-5.0, the drafting speed is 150-250 m/min, and the prepared product has the characteristics of ageing resistance, hydrolysis resistance and the like.
Description
Technical field
The present invention relates to the preparation method of polyester staple fiber, more particularly to a kind of Direct Spinning of hydrolysis aging resistance polyester staple fiber
Preparation method.
Background technology
Polyester staple fiber generates polyester staple fiber by polyester fondant spinning and post processing.Conventional polyester chopped fiber polyester fondant
Viscosity generally in 0.670～0.675dl/g or so, because polyester end base is to water vapor sensitive, particularly under hot humid environment
Hydrolytic resistance it is poor, easily hydrolyzed by its remaining terminal carboxylate group catalysis, cause the deterioration of mechanical property and other performances, very
Its application industrially is limited in big degree.Generally, polyester content of carboxyl end group is higher, the hydrolysis type of polyester
Poorer, this is because containing ester bond in polyester backbone, terminal groups are carboxyl and hydroxyl, cause the anti-hydrolytic performance of polyester poor,
Especially because polyester is hydrolyzed to self-accelerating reaction, acid content increase can accelerate hydrolysis.The anti-degraded polyester of hydrolysis, viscosity is
0.680～0.720dl/g or so, significantly larger than normal polyester.The polyester slice of conventional viscosity, no matter conventional speeds or at a high speed
Spinning, all have accumulated abundant knowhow, but then few for the spinning practice of high viscosity polyester.Therefore it is more right
Spinning equipment, spinning technique have higher requirements.Melt can produce expanded phenomenon, existing polyesters intrinsic through spinneret spinning
Viscosity ratio normal polyester is high, and under relatively low intrinsic viscosity, expanded phenomenon is weaker, right with the raising of melt characteristic viscosity
Expanded phenomena impair is larger, therefore can increase orifice diameter, while from corresponding spinning temperature, ring blowing temp, suitable
Draft ratio etc..
The content of the invention
In order to solve the problems, such as that high viscosity polyester fondant spinning obtains hydrolysis aging resistance polyester staple fiber, the purpose of the present invention exists
In a kind of direct electrospinning method for preparing of hydrolysis aging resistance polyester staple fiber of offer.The technical solution adopted in the present invention is as follows.
The present invention provides a kind of direct electrospinning method for preparing of hydrolysis aging resistance polyester staple fiber, and concrete steps include：
It is 0.680-0.720dl/g by intrinsic viscosity, content of carboxyl end group is 28-34mmol/t, and DEG content is less than 0.8%, melts
Point is more than 260 DEG C, and hydrolysis-resistant polyester melt of the moisture content less than 0.1wt% through static mixer, melt heat exchange, melts
Melt spinning, ring and blow cooling, winding, boundling, stretching, nervous thermal finalization, relaxation heat setting, cut-out and finished product packing operation
Prepare hydrolysis aging resistance polyester staple fiber；Wherein：Melt heat exchange temperature is 260～275 DEG C；Spinning temperature is
280～295 DEG C, ring blowing temperature is 20～28 DEG C, and winding speed is 1200～1600m/min, and the total multiplying power of drawing-off is 3.0～5.0,
75～80 DEG C of drawing temperature, draft speed is 150～250m/min.
In the present invention, shearing length is 4～51mm, and fiber number is 1.0～1.50dtex, and intensity is more than 6.5cN/dtex, and fracture is stretched
Long rate is 18～24%, 180 DEG C of dry shrinkage 3.5～6.0%.
In the present invention, the water-fast polyester fondant that paraphrases is obtained by following preparation methoies：PTA and EG low temperature are esterified,
Using Ti-Sb composite catalysts, add hydrolysis monomer, aid in the inorganic additive of high speed super drawing, add uvioresistant
Line agent is obtained after precondensation and whole polycondensation reaction.
In the present invention, the hydrolysis monomer be trimethyl phosphate, triethyl phosphate,PhosphorusAcyl acetic acid triethyl or double (3,5-
Di-tert-butyl-4-hydroxyl benzyl phosphonic acids mono ethyl ester) calcium salt, its addition is 20-100ppm, in terms of polyester theoretical weight.
In the present invention, the inorganic nano level additive is barium sulfate, titanium dioxide or silicon dioxide；The ultraviolet (UV) resistant agent
Selected from 2- (2H- benzotriazole -2- bases) -4,6- two (1- methyl isophthalic acids-phenylethyl) phenol (UV-234), 2- (4,6- diphenyl -1,3,5-
The base of triazine -2) at least one in -5- [(hexyl) epoxide]-phenol (UV-1577) or double benzoxazoles stilbene.
Compared with prior art, it is an advantage of the current invention that：
1) increase static mixer, be sufficiently mixed the various ingredients in polyester fondant；Simultaneously by adding hydrolysis monomer
Polyester fondant, polyester staple fiber hydrolysis, ageing resistace can be significantly improved.
2) using high viscosity polyester fondant, spinning speed and stretching ratio can be improved, increases fibre strength.
3) inherent quality of fiber is adjusted by melt heat exchange, spinning, the change of ring blowing equitemperature.
Specific embodiment
Technical scheme is described further below according to specific embodiment.Protection scope of the present invention be not limited to
Lower embodiment, enumerates these examples and limits the present invention never in any form merely for exemplary purpose.
Performance test methods
According to GB GB/T 14190-2008 chopped fiber measurement of test method.
Test without silk noil hydrolytic resistance index %BB：The hydrolysis system for handling that a certain amount of copolyester pellets are placed in sealing is taken,
6h is processed under 155 DEG C, the water vapor conditions of 0.46MPa, then its intrinsic viscosity will be determined after the sample drying after process,
The change of copolyester section viscosity relatively after before processing, i.e. the change of copolyester section %BB,
%BB=0.27 × ([IV1]-4/3-[IV0]-4/3)
In equation, IV0Represent the intrinsic viscosity of polyester before hydrolysis process, IV1Represent the intrinsic viscosity of polyester after hydrolysis process.
First, the preparation of hydrolysis-resistant polyester melt
By a certain proportion of p-phthalic acid, ethylene glycol, Titanium series catalyst slurry, send into reaction kettle of the esterification and reacted, instead
Should after through Oligomer pipeline send into prepolymerization reaction kettle.
Oligomer pipeline is sent into after hydrolysis agent, ultraviolet (UV) resistant agent, inorganic additive, ethylene glycol are allocated according to a certain percentage
Prepolymerization reaction kettle is together entered with polyester oligomer.Prepolymerization reaction is carried out at a certain temperature, obtains precondensation product.
Prepolymer is delivered to into the whole batch condensation polymerization reactor of Horizontal band squirrel-cage stirring by pressure reduction, under uniform temperature, pressure constantly
Stirring, carries out whole polycondensation reaction, obtains hydrolysis-resistant polyester melt, and final polyester fondant gear pump is continuously discharged, Jing
Spinning is sent after fondant filter.
2nd, aging resistance polyester staple fiber prepares example
Embodiment 1
Intrinsic viscosity is the hydrolysis-resistant polyester melt of 0.680dl/g, after static mixer mixing, the conveying of Jing melt pipes, and the time
For 40min；
Into melt heat exchanger, temperature is 260 DEG C, direct melt spinning, and spinning temperature is 280 DEG C, ring blowing temperature
For 28 DEG C；
Tow after cooling is wound, and winding speed is 1200m/min, and precursor tow enters to contain silk cylinder；
Front spinning precursor boundling, drawing-off, the total multiplying power of drawing-off is 3.0,78 DEG C of drawing temperature, and drafting rate is 150m/min；
Tow after drawing-off carries out finished product packing after nervous thermal finalization, lax, cut-out；
The course of processing is smooth when fiber is manufactured, stable physical property.
By analysis data are that shearing length is 38mm to finished product, and fiber number is 1.50dtex, and intensity 6.80cN/dtex, fracture is stretched
Long rate is 19.0%, 180 DEG C of dry shrinkage 4.0%.
Its intrinsic viscosity after processing that is hydrolyzed to finished product is 0.678dl/g.
Embodiment 2
Intrinsic viscosity is the hydrolysis-resistant polyester melt of 0.690dl/g, after static mixer mixing, conveys through melt pipe, when
Between be 40min；
Into melt heat exchanger, temperature is 263 DEG C, direct melt spinning, and spinning temperature is 285 DEG C, ring blowing temperature
For 27 DEG C；
Tow after cooling is wound, and winding speed is 1280m/min, and precursor tow enters to contain silk cylinder；
Front spinning precursor boundling, drawing-off, the total multiplying power of drawing-off is 3.5,78 DEG C of drawing temperature, and drafting rate is 200m/min；
Tow after drawing-off carries out finished product packing after nervous thermal finalization, lax, cut-out；
The course of processing is smooth when fiber is manufactured, stable physical property.
By analysis data are that shearing length is 38mm to finished product, and fiber number is 1.38dtex, and intensity 6.83cN/dtex, fracture is stretched
Long rate is 20.0%, 180 DEG C of dry shrinkage 4.0%.
Its intrinsic viscosity after processing that is hydrolyzed to finished product is 0.688dl/g.
Embodiment 3
Intrinsic viscosity is the hydrolysis-resistant polyester melt of 0.700dl/g, after static mixer mixing, conveys through melt pipe, when
Between be 40min；
Into melt heat exchanger, temperature is 265 DEG C, direct melt spinning, and spinning temperature is 290 DEG C, ring blowing temperature
For 26 DEG C；
Tow after cooling is wound, and winding speed is 1320m/min, and precursor tow enters to contain silk cylinder；
Front spinning precursor boundling, drawing-off, the total multiplying power of drawing-off is 3.8,78 DEG C of drawing temperature, and drafting rate is 250m/min；
Tow after drawing-off carries out finished product packing after nervous thermal finalization, lax, cut-out；
The course of processing is smooth when fiber is manufactured, stable physical property.
By analysis data are that shearing length is 38mm to finished product, and fiber number is 1.33dtex, and intensity 6.85cN/dtex, fracture is stretched
Long rate is 21.5%, 180 DEG C of dry shrinkage 4.0%.
Its intrinsic viscosity after processing that is hydrolyzed to finished product is 0.698dl/g.
Embodiment 4
Intrinsic viscosity is the hydrolysis-resistant polyester melt of 0.720dl/g, after static mixer mixing, conveys through melt pipe, when
Between be 40min；
Into melt heat exchanger, temperature is 270 DEG C, direct melt spinning, and spinning temperature is 295 DEG C, ring blowing temperature
For 25 DEG C；
Tow after cooling is wound, and winding speed is 1600m/min, and precursor tow enters to contain silk cylinder；
Front spinning precursor boundling, drawing-off, the total multiplying power of drawing-off is 5.0,78 DEG C of drawing temperature, and drafting rate is 250m/min；
Tow after drawing-off carries out finished product packing after nervous thermal finalization, lax, cut-out；
The course of processing is smooth when fiber is manufactured, stable physical property.
By analysis data are that shearing length is 38mm to finished product, and fiber number is 1.00dtex, and intensity 7.00cN/dtex, fracture is stretched
Long rate is 23.5%, 180 DEG C of dry shrinkage 4.0%.
Its intrinsic viscosity after processing that is hydrolyzed to finished product is 0.728dl/g.
Claims (5)
1. a kind of direct electrospinning method for preparing of hydrolysis aging resistance polyester staple fiber, it is characterised in that concrete steps include：
It is 0.680-0.720dl/g by intrinsic viscosity, content of carboxyl end group is 28-34mmol/t, and DEG content is less than 0.8%, melts
Point is more than 260 DEG C, and hydrolysis-resistant polyester melt of the moisture content less than 0.1wt% through static mixer, melt heat exchange, melts
Melt spinning, ring and blow cooling, winding, boundling, stretching, nervous thermal finalization, relaxation heat setting, cut-out and finished product packing operation
Prepare hydrolysis aging resistance polyester staple fiber；Wherein：Melt heat exchange temperature is 260～275 DEG C；Spinning temperature is
280～295 DEG C, ring blowing temperature is 20～28 DEG C, and winding speed is 1200～1600m/min, and the total multiplying power of drawing-off is 3.0～5.0,
75～80 DEG C of drawing temperature, draft speed is 150～250m/min.
2. direct electrospinning method for preparing according to claim 1, it is characterised in that shearing length is 4～51mm, fiber number is
1.0～1.50dtex, intensity is more than 6.5cN/dtex, and elongation at break is 18～24%, 180 DEG C of dry shrinkage 3.5～6.0%.
3. direct electrospinning method for preparing according to claim 1, it is characterised in that the water-fast polyester fondant that paraphrases is by following
Preparation method is obtained：PTA and EG low temperature are esterified, using Ti-Sb composite catalysts, add hydrolysis monomer, auxiliary
The inorganic additive of high speed super drawing, addition ultraviolet (UV) resistant agent is obtained after precondensation and whole polycondensation reaction.
4. direct electrospinning method for preparing according to claim 3, it is characterised in that the hydrolysis monomer is trimethyl phosphate,
Triethyl phosphate, phosphonoacetate or double (3,5- di-tert-butyl-4-hydroxyl benzyl phosphonic acids mono ethyl ester) calcium salts, its addition
For 20-100ppm, in terms of polyester theoretical weight.
5. direct electrospinning method for preparing according to claim 3, it is characterised in that the inorganic nano level additive be barium sulfate,
Titanium dioxide or silicon dioxide；The ultraviolet (UV) resistant agent is selected from 2- (2H- benzotriazole -2- bases) (the 1- methyl isophthalic acids-phenyl second of -4,6- two
Base) phenol (UV-234), 2- (base of 4,6- diphenyl -1,3,5- triazines -2) -5- [(hexyl) epoxide]-phenol (UV-1577) or double benzos
At least one in oxazole stilbene.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109252243A (en) * | 2018-08-14 | 2019-01-22 | 安徽和邦纺织科技有限公司 | A kind of copolymerization preparation method of porous polyester fiber |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102952260A (en) * | 2011-08-24 | 2013-03-06 | 东丽纤维研究所（中国）有限公司 | Polyester and production method thereof |
| CN103833992A (en) * | 2012-11-20 | 2014-06-04 | 东丽纤维研究所（中国）有限公司 | Polyester composition, and preparation method and use thereof |
| CN104963024A (en) * | 2015-06-18 | 2015-10-07 | 江苏江南高纤股份有限公司 | Polyester directly-spun short fiber for hydrolysis-resistant and photoaging-resistant industry and preparation method thereof |
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2015
- 2015-10-14 CN CN201510665369.9A patent/CN106592003A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102952260A (en) * | 2011-08-24 | 2013-03-06 | 东丽纤维研究所（中国）有限公司 | Polyester and production method thereof |
| CN103833992A (en) * | 2012-11-20 | 2014-06-04 | 东丽纤维研究所（中国）有限公司 | Polyester composition, and preparation method and use thereof |
| CN104963024A (en) * | 2015-06-18 | 2015-10-07 | 江苏江南高纤股份有限公司 | Polyester directly-spun short fiber for hydrolysis-resistant and photoaging-resistant industry and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109252243A (en) * | 2018-08-14 | 2019-01-22 | 安徽和邦纺织科技有限公司 | A kind of copolymerization preparation method of porous polyester fiber |
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Application publication date: 20170426 |