CN108642580A - A kind of method that structure induction drawing-off prepares high intensity biology base fatty acid polyglycol ester fiber - Google Patents
A kind of method that structure induction drawing-off prepares high intensity biology base fatty acid polyglycol ester fiber Download PDFInfo
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- CN108642580A CN108642580A CN201810387685.8A CN201810387685A CN108642580A CN 108642580 A CN108642580 A CN 108642580A CN 201810387685 A CN201810387685 A CN 201810387685A CN 108642580 A CN108642580 A CN 108642580A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/098—Melt spinning methods with simultaneous stretching
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
- D01F6/625—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters derived from hydroxy-carboxylic acids, e.g. lactones
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- Manufacturing & Machinery (AREA)
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- Thermal Sciences (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention relates to the methods that a kind of induction drawing-off of structure prepares high intensity biology base fatty acid polyglycol ester fiber, including：Nano material tungsten oxide or iron sulfide are blended with biology base fatty acid polyester, then melt spinning, obtain modification biological base polyester fiber, secondary drawing-off or multistage drafting, fiber between the first draw roll and the second draw roll carries out continuous near infrared light, the temperature that first draw roll and the second draw roll are set simultaneously be room temperature to get.The present invention is simple to operation, by the accurate temperature control of fiber unformed area, achievees the effect that fiber height is orientated, and obtained biology base aliphatic polyester fiber mechanics intensity is high, and fracture strength is 2.5~5.5cN/dtex, and elongation at break is 15.0~25.0%.
Description
Technical field
The invention belongs to the preparation field of structural high strength fibre, more particularly to a kind of structure induction drawing-off prepares high-strength
Spend the method for biology base fatty acid polyglycol ester fiber.
Background technology
Biological poly ester fiber refers to mutually being tied with chemical synthesis through biofermentation or biology using renewable resource as raw material
The means of conjunction and a kind of new material obtained have many advantages, such as green, environmental protection, renewable, help to solve Present Global warp
The problems such as Ji social development faces serious resource and energy shortage, environmental pollution.But steric regularity is high, vitrifying temperature
It spends that low, crystalline rate is slow, spherulite size is big and the series of factors such as secondary crystallization results in Biopolvester fiber weakness problem, and
Limit the engineering application of Biopolvester fiber.
In order to obtain the biological poly ester fiber of high intensity, the method mostly induced at present with dry spinning and drawing-off improves fibre
The orientation texture of dimension.There is Japanology scholar that biology base fiber spun filament is immersed in ice-water bath, then carry out secondary drawing-off,
Obtain fiber (Macromolecular Bioscience, 2005,5 (8) of high intensity:689-
701.Macromolecules,2006,39(8):2940-2946).Unfortunately, this method needs the processing 24 in ice water small
When, then drawing-off is handled, and limits its application in actual production.
In order to obtain a kind of straightforward procedure of crystalline texture regulation and control, found by investigating, tungsten oxide or iron sulfide etc.
Nano material because of distinctive nanometer size effect, can be generated under infrared light heat (CN102921006B,
CN107381644A, document (J.Am.Chem.Soc.2012,134,3995-3998；Doctoral thesis：Hybrid nanometer
The synthesis of optical-thermal conversion material and its application study in oncotherapy, Meng Zhouqi)) and it is applied to thermotherapy and the change of cancer
In treatment.Therefore, the inorganic material of this nano-scale can be introduced into fiber, nano-particle of the control positioned at unformed area
Energy is converted under the action of near infrared light, accurately regulates and controls the unformed temperature of fiber, fine to promote at ambient temperature
The orientation of dimension.
Invention content
Technical problem to be solved by the invention is to provide a kind of induction drawing-offs of structure to prepare high intensity biology base aliphatic acid
The method of polyester fiber, this method are existed using being dispersed in the nano-powders such as nanometer tungsten oxide or the iron sulfide of fiber unformed area
Under the action of near infrared light, the temperature of fiber unformed area is preferentially induced to increase under room temperature environment, promotes point of unformed area
Subchain moves, and under external force drawing-off effect, makes crystalline region microfibrillar structure further in fiber axial orientation, unformed area ties up knot point
Subchain content improves, to improve the mechanical property of fiber.
The method that a kind of structure induction drawing-off of the present invention prepares high intensity biology base fatty acid polyglycol ester fiber, including：
(1) nano material tungsten oxide or iron sulfide are blended with biology base fatty acid polyester, obtain modification biological base fat
Acid polyester, then melt spinning, obtains modification biological base fatty acid polyglycol ester fiber, and wherein nano material accounts for biology base fatty acid polyglycol
0.05~1.0wt% of ester quality；Spinning temperature is 130~230 DEG C；
(2) secondary drawing-off is carried out to modification biological base fatty acid polyglycol ester fiber in step (1), to the first draw roll and second
Fiber between draw roll carries out continuous near infrared light, while the temperature that the first draw roll and the second draw roll is arranged is room
Temperature obtains high intensity biology base fatty acid polyglycol ester fiber；
Or multistage drafting is carried out to modification biological base fatty acid polyglycol ester fiber in step (1), to the first draw roll and second
Fiber between draw roll carries out continuous near infrared light, while the temperature that the first draw roll and the second draw roll is arranged is room
Temperature, remaining roll temperature are 30~70 DEG C, obtain high intensity biology base fatty acid polyglycol ester fiber.
Tungsten oxide referenced patent CN102921006B, CN107381644A and document (Tunable in the step (1)
Localized Surface Plasmon Resonances in Tungsten Oxide Nanocrystals,
J.Am.Chem.Soc.2012,134,3995-3998 it) prepares.For example, weighing 0.35g WCl6, it is put into the height that solvent is 100mL
It presses in inner liner of reaction kettle, the absolute ethyl alcohol of 24mL is added under agitation, be then added 56mL's under agitation
PEG400 continues to stir half an hour；It is transferred in autoclave, is reacted 24 hours under the conditions of 180 DEG C；After reaction, from
The heart detaches, you can obtains WO2.72Nano wire.
In the step (1) iron sulfide with reference to doctoral thesis (synthesis of hybrid nanometer optical-thermal conversion material and
Its application study in oncotherapy, Meng Zhouqi) it prepares：96g sulphur powders are dissolved in 5L diphenyl ether, and are stirred at 70 DEG C
Degassing 1 hour, is denoted as solution A；By 100g FeCl2·4H2O is dissolved in 10Kg octadecylamines, and is deaerated 1 hour in 120 DEG C, so
It is warming up to 220 DEG C under nitrogen protection afterwards, solution A is then added and reacts 3 hours, is cooled to 100 DEG C；Be added 9L chloroforms with
It prevents reaction system from solidifying, its 4400rpm is centrifuged and takes out within 5 minutes large-size particle, and obtains sheet after ethyl alcohol cleans
Vulcanize iron nano-particle.
Tungsten oxide is WOx in the step (1), and x is 2.72~3；Iron sulfide is FeS2。
The shape of tungsten oxide is that nanometer is linear in the step (1)；The shape of iron sulfide is nano-sheet；Tungsten oxide or sulphur
The grain size for changing iron is about 1~200nm.
Biology base fatty acid polyester is poly- (3-hydroxybutyrate ester) PHB, poly- (3-hydroxybutyrate ester-in the step (1)
Co-3- hydroxyl valerates) PHBV, poly- (3-hydroxybutyrate ester-co-4- butyric esters) P (3HB-co-4HB), poly- (3- hydroxyls
Butyrate-co-3- hydroxycaproic esters) PHBHHx, polylactic acid PLA or poly butylene succinate PBS.
The technological parameter of melt spinning is in the step (1)：Spin speed be 500~3000m/min, heat roller temperature be 50~
60 DEG C, draw ratio is 1~3.
Near infrared light power is 25.0~200.0W/cm in the step (2)2, near infrared light distance for 2~
30 centimetres.
The first draw roll draw ratio is 1.01~1.10 in drafting process in the step (2), the second draw roll draw ratio
It is 1.20~1.70, remaining roller draw ratio is 1~2.
The fracture strength of high intensity biology base fatty acid polyglycol ester fiber is 2.5~5.5cN/dtex in the step (2), is broken
It is 15.0~25.0% to split elongation.
The present invention is according to patent CN102921006B, CN107381644A, document (J.Am.Chem.Soc.2012,134,
3995-3998) and doctoral thesis (hybrid nanometer optical-thermal conversion material synthesis and its answering in oncotherapy
With research, Meng Zhouqi) in nanometer tungsten oxide and iron sulfide technology of preparing, be prepared for the nano material of certain size range, so
After be added in biology base fiber, explore by fiber unformed area temperature control draw orientation prepare high intensity biology base fiber
Method improves thinking for the high intensity processing of typical zolymerization fibres.
The present invention breaches the traditional draft process of standard biologic base polyester fiber, is crystallized and is tied to fiber using near infrared light
The amorphous region of structure carries out accurate temperature control, realizes the high order drawing-off of fiber, it will be apparent that improve the drawing of biological poly ester fiber
Stretch fracture strength.
Advantageous effect
(1) present invention is simple to operation, by the accurate temperature control of fiber unformed area, reaches the effect of fiber height orientation
Fruit.
(2) the melt-spun high intensity biology base fatty acid polyester fiber mechanics intensity that the present invention obtains is high, fracture strength 2.5
~5.5cN/dtex, elongation at break are 15.0~25.0%.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) it is prepared for tungsten oxide WO with reference to patent CN102921006B2.72Nano wire.
(2) the tungsten oxide WO by PHBV powder (HV molar contents are 10~25mol%) with 200nm sizes2.72Nano wire
(tungsten oxide WO2.72Account for the 1wt% of PHBV mass) after mixing, it is blended through twin-screw at 175 DEG C, obtains modified PHBV.
It is 16 hours dry under 80 DEG C of rotary-drum vacuum dry environments, fast spinning technique is spun through 500m/min at 180 DEG C, obtains modified PHBV
Fiber, wherein heat roller temperature are 50 DEG C, draw ratio 2.
(3) by modified PHBV fibers drawing-off on level Four draft apparatus in step (2), the first, second drawing-off roller temperature is set
Degree is 20 DEG C, and third drawing-off roll temperature is 35 DEG C, and the 4th sizing roll temperature is 60 DEG C.First draw roll and the second draw roll use
200W/cm2Near-infrared light source Continuous irradiation fiber, irradiation distance control 2cm, and nano-powder, which generates instantaneous heat quantity, makes local microcell
Heat reaches 85~95 DEG C.Wherein, the first draw roll draw ratio is 1.05, and the second draw roll draw ratio is 1.50, third drawing-off
Roller draw ratio is 2.0, and setting roller draw ratio is 1.01, and after multistage drafting, fiber tensile break strength reaches fiber
2.5cN/dtex (CV values 3%), fibrous fracture elongation reach 15% (CV values 6%).
Embodiment 2
(1) it is prepared for tungsten oxide WO with reference to patent of invention CN107381644A3Nano wire.
(2) by the tungsten oxide WO of PLA slice and about 100nm sizes3.0Nano wire (tungsten oxide WO3.0Account for PLA mass
0.5wt%) after mixing, it is blended through twin-screw at 225 DEG C and obtains modified PLA.It is done under 70 DEG C of rotary-drum vacuum dry environments
Dry 24 hours, fast spinning technique is spun through 3000m/min at 230 DEG C, obtains modified PLA fibers, wherein heat roller temperature is 60 DEG C,
Draw ratio is 3.
(3) by modified PLA fibers drawing-off on level Four draft apparatus in step (2), the first, second drawing-off roll temperature is set
It it is 20 DEG C, third drawing-off roll temperature is 45 DEG C, and the 4th sizing roll temperature is 70 DEG C.First draw roll and the second draw roll use
100W/cm2Near-infrared light source Continuous irradiation fiber, irradiation distance control 30cm, and nano-powder, which generates instantaneous heat quantity, keeps part micro-
Area's heat reaches 70~85 DEG C.Wherein, the first draw roll draw ratio is 1.05, and the second draw roll draw ratio is 1.30, and third is led
It is 2.0 to stretch roller draw ratio, and setting roller draw ratio is 1.01, and after multistage drafting, fiber tensile break strength reaches fiber
5.5cN/dtex (CV values 5%), fibrous fracture elongation reach 15% (CV values 7%).
Embodiment 3
(1) reference literature (Tunable Localized Surface Plasmon Resonances in Tungsten
Oxide Nanocrystals, J.Am.Chem.Soc.2012,134,3995-3998) it is prepared for tungsten oxide WO2.80Nano wire.
(2) by the tungsten oxide WO of PHBHHx slice and about 50nm sizes2.80Nano wire (tungsten oxide WO2.80Account for PHBHHx mass
0.05wt%) after mixing, obtain modified PHBHHx through 150 DEG C of melt blendings of rotating speed 50rpm screw rods.It is true in 80 DEG C of rotary drums
It is 24 hours dry under empty dry environment, fast spinning technique is spun through 800m/min at 170 DEG C, obtains modified PHBHHx fibers,
Middle heat roller temperature is 50 DEG C, draw ratio 1.5.
(3) by modified PHBHHx fibers drawing-off on level Four draft apparatus in step (2), the first, second draw roll is set
Temperature is 20 DEG C, and third drawing-off roll temperature is 45 DEG C, and the 4th sizing roll temperature is 50 DEG C.First draw roll and the second draw roll are adopted
Use 25W/cm2Near-infrared light source Continuous irradiation fiber, irradiation distance control 10cm, and nano-powder, which generates instantaneous heat quantity, keeps part micro-
Area's heat reaches 70~80 DEG C.Wherein, the first draw roll draw ratio is 1.10, and the second draw roll draw ratio is 1.70, and third is led
It is 2.0 to stretch roller draw ratio, and setting roller draw ratio is 1.02, and for fiber after multistage drafting, PHBHHx fiber tension failures are strong
Degree reaches 2.5cN/dtex (CV values 6%), and fibrous fracture elongation reaches 25% (CV values 8%).
Embodiment 4
(1) with reference to doctoral thesis (hybrid nanometer optical-thermal conversion material synthesis and its in oncotherapy
Application study, Meng Zhouqi) it is prepared for nano-sheet iron sulfide FeS2。
(2) by the nano-sheet iron sulfide FeS of PBS and about 150nm sizes2(iron sulfide FeS2Account for the 1wt% of PBS mass)
After mixing, 125 DEG C are heated to, is blended through twin-screw, modified PBS is obtained.It is dry under 80 DEG C of rotary-drum vacuum dry environments
24 hours, fast spinning technique is spun through 1000m/min at 130 DEG C, obtains modified PBS fibers, wherein heat roller temperature is 60 DEG C, is led
It stretches than being 2.
(3) by modified PBS fibers drawing-off on level Four draft apparatus in step (2), the first, second drawing-off roll temperature is set
It it is 20 DEG C, third drawing-off roll temperature is 30 DEG C, and the 4th sizing roll temperature is 70 DEG C.First draw roll and the second draw roll use
30W/cm2Near-infrared light source Continuous irradiation fiber, irradiation distance control 5cm, and nano-powder, which generates instantaneous heat quantity, makes local microcell
Heat reaches 75~85 DEG C.Wherein, the first draw roll draw ratio is 1.05, and the second draw roll draw ratio is 1.70, third drawing-off
Roller draw ratio is 2.0, and setting roller draw ratio is 1.01, and after multistage drafting, fiber tensile break strength reaches fiber
3.5cN/dtex (CV values 7%), fibrous fracture elongation reach 18% (CV values 7%).
Claims (7)
1. a kind of method that structure induction drawing-off prepares high intensity biology base fatty acid polyglycol ester fiber, including：
(1) nano material tungsten oxide or iron sulfide are blended, then melt spinning with biology base fatty acid polyester, obtain modified life
Object base fatty acid polyglycol ester fiber, wherein nano material account for 0.05~1.0wt% of biology base fatty acid polyester quality；Melt spinning
Temperature is 130~230 DEG C；
(2) secondary drawing-off is carried out to modification biological base fatty acid polyglycol ester fiber in step (1), to the first draw roll and the second drawing-off
Fiber between roller carries out continuous near infrared light, while the temperature that the first draw roll and the second draw roll is arranged is room temperature,
Obtain high intensity biology base fatty acid polyglycol ester fiber；
Or multistage drafting is carried out to modification biological base fatty acid polyglycol ester fiber in step (1), to the first draw roll and the second drawing-off
Fiber between roller carries out continuous near infrared light, while the temperature that the first draw roll and the second draw roll is arranged is room temperature,
Remaining roll temperature is 30~70 DEG C, obtains high intensity biology base fatty acid polyglycol ester fiber.
2. a kind of structure induction drawing-off described in accordance with the claim 1 prepares the side of high intensity biology base fatty acid polyglycol ester fiber
Method, which is characterized in that tungsten oxide is WOx in the step (1), and x is 2.72~3；Iron sulfide is FeS2。
3. a kind of structure induction drawing-off described in accordance with the claim 1 prepares the side of high intensity biology base fatty acid polyglycol ester fiber
Method, which is characterized in that the shape of tungsten oxide is that nanometer is linear in the step (1)；The shape of iron sulfide is nano-sheet；Oxidation
The grain size of tungsten or iron sulfide is 1~200nm.
4. a kind of structure induction drawing-off described in accordance with the claim 1 prepares the side of high intensity biology base fatty acid polyglycol ester fiber
Method, which is characterized in that biology base fatty acid polyester is poly- (3-hydroxybutyrate ester) PHB, poly- (3- hydroxyl fourths in the step (1)
Acid esters-co-3- hydroxyl valerates) PHBV, poly- (3-hydroxybutyrate ester-co-4- butyric esters) P (3HB-co-4HB), poly- (3-
Butyric ester-co-3- hydroxycaproic esters) PHBHHx, polylactic acid PLA or poly butylene succinate PBS.
5. a kind of structure induction drawing-off described in accordance with the claim 1 prepares the side of high intensity biology base fatty acid polyglycol ester fiber
Method, which is characterized in that the technological parameter of melt spinning is in the step (1)：It is 500~3000m/min, heat roller temperature to spin speed
It it is 50~60 DEG C, draw ratio is 1~3.
6. a kind of structure induction drawing-off described in accordance with the claim 1 prepares the side of high intensity biology base fatty acid polyglycol ester fiber
Method, which is characterized in that near infrared light power is 25.0~200.0W/cm in the step (2)2, near infrared light away from
From being 2~30 centimetres.
7. a kind of structure induction drawing-off described in accordance with the claim 1 prepares the side of high intensity biology base fatty acid polyglycol ester fiber
Method, which is characterized in that the first draw roll draw ratio is 1.01~1.10 in drafting process in the step (2), the second draw roll
Draw ratio is 1.20~1.70, remaining roller draw ratio is 1~2.
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| JPH05321025A (en) * | 1992-01-09 | 1993-12-07 | Chuko Kasei Kogyo Kk | Production of yarn |
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| CN102108562A (en) * | 2010-11-16 | 2011-06-29 | 清华大学 | Method for preparing polyhydroxyalkanoate (PHA) fibers |
| CN102921006A (en) * | 2012-11-13 | 2013-02-13 | 东华大学 | Application of tungsten oxide matrix nanometer materials in preparation of near-infrared light heat treatment drugs |
| CN103088460A (en) * | 2013-01-04 | 2013-05-08 | 东华大学 | High-strength industrial polyester fiber and preparation method thereof |
| CN105603569A (en) * | 2016-03-07 | 2016-05-25 | 天津工业大学 | Polyhydroxyalkanoate fibers, preparing method and application thereof |
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2018
- 2018-04-26 CN CN201810387685.8A patent/CN108642580B/en active Active
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| JPH05321025A (en) * | 1992-01-09 | 1993-12-07 | Chuko Kasei Kogyo Kk | Production of yarn |
| CN101538750A (en) * | 2008-03-18 | 2009-09-23 | 天津国韵生物材料有限公司 | Polyhydroxyalkanoates fiber and preparation method thereof |
| CN102108562A (en) * | 2010-11-16 | 2011-06-29 | 清华大学 | Method for preparing polyhydroxyalkanoate (PHA) fibers |
| CN102921006A (en) * | 2012-11-13 | 2013-02-13 | 东华大学 | Application of tungsten oxide matrix nanometer materials in preparation of near-infrared light heat treatment drugs |
| CN103088460A (en) * | 2013-01-04 | 2013-05-08 | 东华大学 | High-strength industrial polyester fiber and preparation method thereof |
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| 陈姿晔等: "异相成核和拉伸诱导对生物基PHBV复合纤维结晶结构与力学性能的影响", 《高分子学报》 * |
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