CN105463623B - A kind of polyformaldehyde polylactic acid poly Lanthanum Isopropoxide tri compound fiber and preparation method thereof - Google Patents
A kind of polyformaldehyde polylactic acid poly Lanthanum Isopropoxide tri compound fiber and preparation method thereof Download PDFInfo
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- CN105463623B CN105463623B CN201510897924.0A CN201510897924A CN105463623B CN 105463623 B CN105463623 B CN 105463623B CN 201510897924 A CN201510897924 A CN 201510897924A CN 105463623 B CN105463623 B CN 105463623B
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- polyformaldehyde
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- tri compound
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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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
- D01D13/00—Complete machines for producing artificial threads
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
Abstract
The present invention relates to a kind of polyformaldehyde polylactic acid poly Lanthanum Isopropoxide tri compound fiber and preparation method thereof.Composite fibre of the present invention, its fiber bodies composition is polyformaldehyde（POM）, PLA（PLA）With PPDO, the mass ratio of three is followed successively by 60~80：12~30：3~15；Its preparation method is：Three kinds of polymer are separately dried to constant weight, after Screw Extrusion after prefilter, casing and component, is wound after the cooling of spinneret path, spun filament is obtained into composite fibre after after road hot gas spring, thermal finalization.Composite fibre of the present invention has the degradability of good mechanical property, heat resistance and appropriateness, has a good application prospect.
Description
Technical field
The present invention relates to a kind of composite fibre, more particularly to a kind of polyformaldehyde-PLA-PPDO ternary are multiple
Condensating fiber and preparation method thereof.
Background technology
Polyformaldehyde (polyoxymethylene, POM) fiber has adhered to the excellent properties of POM raw materials, with high-strength and high-modulus,
Excellent wear resistance, alkali resistance, high elongation recovery characteristic；The Impacting endurance of especially POM fibers is excellent, damage resistant fracture
Property is good.Meanwhile, substantial amounts of ehter bond is contained in POM fibrous molecular structures, has good compatibility, bond strength with multiple material
Height, therefore POM fibers are available for composite enhancing.
However, POM resins have the features such as heat endurance is poor, crystallization rate is fast, crystallinity is high, this is prepared by constraints on fiber
Bottleneck.Domestic and foreign scholars and scientific and technical personnel have carried out certain research work.Patent CN201010137926 is employed at least
Two grades of slow cooling (narrow area's slow cooling, compartment slow cooling)), the draft process of the road different mediums of Hou Dao tri-, but temperature is relatively low, thermal finalization
Temperature is 60-115 DEG C, and the time reaches 10-40min, and production efficiency is extremely low, while winding speed is 50-5000min, but is not known
This speed and the matching range of forward and backward spinning.CN201010588776.1 equally employs slow cooling-quenching, high pressure (50-
200atm), multistage many multiplying power stretchings obtain and always lead a times higher fiber at a slow speed, but spin fast fast (500-3500m/min), not
The characteristics of being adapted to POM rapid crystallizations.CN200710187055 mainly defines the ratio of ethylene oxide in spinning material copolymerized methanal
Example (1.8%-5.0%) and melting means (1.0-120).CN02818234 is equally the amount for controlling oxyalkylene, and fixed cooling is fast
Rate, keeps its longer flexible chain.CN200310119502.8 defines the sectional area of drafting multiple and drawing-off body, simultaneously
Also it is that 0.5~10%, melt index is 0.3~20g/10min to define oxyalkylene units content molar content.
CN02156329.2 defines the polyformaldehyde molecular structure and melt index for preparing fiber.CN200680002247 is referred to using molten
Body index is 0.3-30ml/10min (0.42-42g/10min) polyacetal copolymer, counter extensioin mode, drawing-off medium, is always led
When heat setting temperature is stretched to limit.
In terms of polyformaldehyde composite fibre preparation, patent CN200510081358 proposes to be prepared for core-skin composite fiber, core
It is respectively the copolymerized methanal of different characteristic with sheath.CN200710126318 define oxyalkylene units, melt index (MI) basis
On, by POM and caustic digestion resin, water-soluble resin and organic solvent-soluble resin compounded spinning, then by alkali process,
Water process or organic solvent processing remove thermoplastic resin, or dissolving removes POM fibers, obtains the microfibre containing POM.
From Outline of literature as can be seen that existing research focuses mostly in terms of POM fibrous raw materials and corresponding technique, and to multiple
It is related in terms of the composition of condensating fiber less.The higher crystalline rate of polyformaldehyde fibre ensure that its is excellent with crystallinity feature
Mechanical property, but its pliability is not enough.PLA (PLA) has preferable mechanical strength, modulus of elasticity and a degradability, it is hard and
The poor characteristic of crisp, pliability limits its application.PPDO (PPDO) is in crystalline polymer, its molecular structure
Containing ester bond and ehter bond, ehter bond is all contributed to PPDO hydrophily and compliance, in addition, contained-CH in molecule2-, it is also
PPDO has flexible reason.Polyformaldehyde has very close narrow processing temperature interval with PLA, meanwhile, PLA glass
Glass transition temperature occurs that crystallization peak temperature is close with PPDO, embodies good compatibility.Based on above-mentioned background and feature, sheet
Patent will invent a kind of polyformaldehyde-PLA-PPDO tri compound fiber.
The content of the invention
Using the interval close polyformaldehyde (POM) of processing temperature, PLA (PLA) and PPDO (PPDO) three
Polymer is planted, using the pliability of PPDO, suitably slows down the crystalline rate of polyformaldehyde, and improve the crisp of PLA
Property, so as to obtain polyformaldehyde-PLA-PPDO tri compound fiber of excellent performance of the present invention.
The present invention provides a kind of polyformaldehyde-PLA-PPDO tri compound fiber, the composite fibre sheet
Body composition is polyformaldehyde (POM), PLA (PLA) and PPDO (PPDO), the mass ratio of three is followed successively by 60~
80：12~30：3~15.
A kind of preparation method of polyformaldehyde-PLA-PPDO tri compound fiber of the present invention, including
Following steps：
(1) polyformaldehyde, PLA and PPDO these three polymer are separately dried to constant weight, polyformaldehyde,
The drying temperature of PLA and PPDO is respectively：60 DEG C~100 DEG C, 60 DEG C~80 DEG C and 40 DEG C~60 DEG C, do
The dry time is respectively：6h, 16~24h and 8h；
After (2) three kinds of polymer are well mixed in high-speed mixer in proportion, screw extruder is added, through filtering, case
After body component and spinneret, wound after being cooled down through path, wherein, the temperature of screw extruder feeding section, compression section and metering section
Respectively 60 DEG C~110 DEG C, 160 DEG C~220 DEG C, 180 DEG C~215 DEG C, the path in the range of 1 meter below spinneret leads to nitrogen
Protection, winding speed is 150~400m/min；
(3) by as-spun fibre, road drawing-off, thermal finalization are finished product with being wound after oiling after, and rear road drawing temperature control is 80
~150 DEG C, drawing-off general times are 2~10 times；
The polyformaldehyde raw materials melt index range is 3.5~15.0g/10min, the polylactic acid raw material weight average molecular weight
For 4~330,000, the molecular weight of the PPDO is 8~420,000.
Heat setting process described in step (3)：Temperature is 60 DEG C~115 DEG C, and the time is 5~720s.
Oiling process described in step (3)：Oil concentration is 5%~12.5%, oil tanker FREQUENCY CONTROL in 2~30Hz, into
Product silk oil applying rate is 0.1%~1.5%.
The major advantage of composite fibre of the present invention：
(1) using conventional polymer, respective mechanical property advantage is played, the compound fibre of high comprehensive performance is formed
Dimension；
The processing temperature interval of (2) three kinds of polymer is close, is conducive to the realization of processing technology；
(3) the degradable PLA component in addition part, assigns the more features of fiber.
Embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after present disclosure has been read, those skilled in the art
The present invention can be made various changes or modifications, these equivalent form of values equally fall within what the application appended claims were limited
Scope.
Polyformaldehyde is purchased from Shanghai Bluestar New Chemical Materials Co., Ltd., and two kinds of raw materials of PLA and PPDO are purchased from
Bo Li biomaterials Co., Ltd of Shenzhen.
Comparative example
Melting means is prepared into a diameter of 30 microns common POM fibers sample as a comparison for 9.0g/10min polyformaldehyde.Phase
Answer technique same as Example 1, labeled as comparative sample 1.
Embodiment 1
PLA that the polyformaldehyde for being 9.0g/10min by melting means, molecular weight are 150,000, molecular weight be 350,000 it is poly- to two
Oxygen cyclohexanone dries 6h, 16h and 8h under the conditions of 90 DEG C, 80 DEG C and 40 DEG C respectively.By 80：12：8 mass ratio is in mixed at high speed
After machine is well mixed, screw extruder is added, the temperature of screw extruder feeding section, compression section and metering section is respectively 90 DEG C,
200℃、195℃.After filtering, box assembly and spinneret, wound after being cooled down through path.In the range of 1 meter below spinneret
Path lead to nitrogen protection, winding speed is 150m/min.Road drawing-off, drawing-off after as-spun fibre is carried out at a temperature of 135 DEG C
General times are 6.5 times；Heat setting temperature is 70 DEG C, and the time is 300s.The oiling process used is 5% for oil concentration, oil tanker
Frequency is 15Hz, and finished silk oil applying rate is 0.8%.Fibre diameter is 30 microns, labeled as embodiment sample 1.
Embodiment 2
PLA that the polyformaldehyde for being 3.5g/10min by melting means, molecular weight are 330,000, molecular weight be 80,000 it is poly- to dioxy
Cyclohexanone dries 6h, 24h and 8h under the conditions of 100 DEG C, 60 DEG C and 60 DEG C respectively.By 60：25：15 mass ratio is in mixed at high speed
After machine is well mixed, screw extruder is added, the temperature of screw extruder feeding section, compression section and metering section is respectively 110 DEG C,
195℃、190℃.After filtering, box assembly and spinneret, wound after being cooled down through path.In the range of 1 meter below spinneret
Path lead to nitrogen protection, winding speed is 400m/min.Road drawing-off, drawing-off after as-spun fibre is carried out at a temperature of 150 DEG C
General times are 10 times；Heat setting temperature is 115 DEG C, and the time is 20s.The oiling process used is 12.5% for oil concentration, oil
Wheel frequency is 2Hz, and finished silk oil applying rate is 1.5%.Fibre diameter is 36 microns, labeled as embodiment sample 2.
Embodiment 3
PLA that the polyformaldehyde for being 15.0g/10min by melting means, molecular weight are 40,000, molecular weight be 420,000 it is poly- to two
Oxygen cyclohexanone dries 6h, 20h and 8h under the conditions of 85 DEG C, 72 DEG C and 55 DEG C respectively.By 68：22：10 mass ratio is mixed in high speed
After conjunction machine is well mixed, screw extruder is added, the temperature of screw extruder feeding section, compression section and metering section is respectively 100
℃、178℃、210℃.After filtering, box assembly and spinneret, wound after being cooled down through path.1 meter of scope below spinneret
Interior path leads to nitrogen protection, and winding speed is 320m/min.Road drawing-off after as-spun fibre is carried out at a temperature of 145 DEG C, leads
General times are stretched for 7.5 times；Heat setting temperature is 105 DEG C, and the time is 90s.The oiling process used is 8% for oil concentration, oil
Wheel frequency is 9Hz, and finished silk oil applying rate is 1.2%.Fibre diameter is 20 microns, labeled as embodiment sample 3.
Embodiment 4
PLA that the polyformaldehyde for being 7.5g/10min by melting means, molecular weight are 200,000, molecular weight be 120,000 it is poly- to two
Oxygen cyclohexanone dries 6h, 18h and 8h under the conditions of 95 DEG C, 65 DEG C and 45 DEG C respectively.By 65：24：11 mass ratio is mixed in high speed
After conjunction machine is well mixed, screw extruder is added, the temperature of screw extruder feeding section, compression section and metering section is respectively 105
℃、160℃、190℃.After filtering, box assembly and spinneret, wound after being cooled down through path.1 meter of scope below spinneret
Interior path leads to nitrogen protection, and winding speed is 270m/min.Road drawing-off, drawing-off after as-spun fibre is carried out at a temperature of 80 DEG C
General times are 2 times；Heat setting temperature is 60 DEG C, and the time is 240s.The oiling process used is 7.5% for oil concentration, oil tanker
Frequency is 12Hz, and finished silk oil applying rate is 0.6%.Fibre diameter is 40 microns, labeled as embodiment sample 4.
Embodiment 5
PLA that the polyformaldehyde for being 13.5g/10min by melting means, molecular weight are 120,000, molecular weight be 210,000 it is poly- to two
Oxygen cyclohexanone dries 6h, 21h and 8h under the conditions of 65 DEG C, 70 DEG C and 54 DEG C respectively.By 75：22：3 mass ratio is in mixed at high speed
After machine is well mixed, screw extruder is added, the temperature of screw extruder feeding section, compression section and metering section is respectively 110 DEG C,
185℃、215℃.After filtering, box assembly and spinneret, wound after being cooled down through path.In the range of 1 meter below spinneret
Path lead to nitrogen protection, winding speed is 360m/min.Road drawing-off, drawing-off after as-spun fibre is carried out at a temperature of 125 DEG C
General times are 4.8 times；Heat setting temperature is 95 DEG C, and the time is 180s.The oiling process used is 6.5% for oil concentration, oil
Wheel frequency is 4Hz, and finished silk oil applying rate is 0.1%.Fibre diameter is 25 microns, labeled as embodiment sample 5.
Application Example
According to this standard of GB/T14344-2008 chemical fiber filament Erichsen test methods, composite fibre is carried out
Mechanics Performance Testing, as a result such as table 1：
The fibre property of table 1
| Group | Fracture strength/MPa | Modulus of elasticity/GPa | Elongation at break/% |
| Comparative example 1 | 764 | 8.9 | 12.9 |
| Embodiment 1 | 882 | 8.2 | 27.5 |
| Embodiment 2 | 1090 | 12.7 | 25.4 |
| Embodiment 3 | 944 | 11.4 | 28.6 |
| Embodiment 4 | 569 | 6.3 | 36.7 |
| Embodiment 5 | 803 | 9.8 | 26.2 |
As can be seen from the above table, in the case where keeping fracture strength suitable, the fracture for the composite fibre that the present invention is obtained
Elongation improves 96.9%~284.5% compared with comparative example 1, and modulus of elasticity has obtained good holding or raising, realizes
The pliability of composite fibre of the present invention, improves POM fibers excessively firm shortcoming, embodies the technology of preparation method
Advantage and beneficial effect.
Claims (3)
1. a kind of polyformaldehyde-PLA-PPDO tri compound fiber, it is characterised in that：The composite fibre sheet
Body composition is polyformaldehyde (POM), PLA (PLA) and PPDO (PPDO), the mass ratio of three is followed successively by 60~
80：12~30：3~15；
The preparation method of described polyformaldehyde-PLA-PPDO tri compound fiber, comprises the following steps：
(1) by polyformaldehyde, PLA and PPDO, these three polymer are separately dried to constant weight, polyformaldehyde, poly- breast
Acid and the drying temperature of PPDO are respectively：60 DEG C~100 DEG C, 60 DEG C~80 DEG C and 40 DEG C~60 DEG C, when drying
Between be respectively：6h, 16~24h and 8h；
After (2) three kinds of polymer are well mixed in high-speed mixer in proportion, screw extruder is added, through filtering, casing group
After part and spinneret, wound after being cooled down through path, wherein, the temperature difference of screw extruder feeding section, compression section and metering section
For 60 DEG C~110 DEG C, 160 DEG C~220 DEG C, 180 DEG C~215 DEG C, the path in the range of 1 meter below spinneret, which leads to nitrogen, to be protected
Shield, winding speed is 150~400m/min；
(3) by as-spun fibre after road drawing-off, thermal finalization and after oiling winding be finished product, rear road drawing temperature control 80~
150 DEG C, drawing-off general times are 2~10 times；
The polyformaldehyde raw materials melt index range is 3.5~15.0g/10min, and the polylactic acid raw material weight average molecular weight is 4
~33 ten thousand, the molecular weight of the PPDO is 8~420,000.
2. polyformaldehyde-PLA according to claim 1-PPDO tri compound fiber, it is characterised in that
Heat setting process described in step (3)：Temperature is 60 DEG C~115 DEG C, and the time is 5~720s.
3. polyformaldehyde-PLA according to claim 1-PPDO tri compound fiber, it is characterised in that
Oiling process described in step (3)：Oil concentration is 5%~12.5%, and oil tanker FREQUENCY CONTROL oils in 2~30Hz, finished silk
Rate is 0.1%~1.5%.
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| CN106521704B (en) * | 2016-10-31 | 2019-03-08 | 江苏苏博特新材料股份有限公司 | A kind of preparation method of polyketone-polyformaldehyde composite fibre |
| CN107586373A (en) * | 2017-10-18 | 2018-01-16 | 江苏苏博特新材料股份有限公司 | A kind of crystal property adjustable spinning polyoxymethylene resin and its spinning process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3608044A (en) * | 1969-01-28 | 1971-09-21 | Celanese Corp | Process for melt spinning polyoxymethylene filaments having elastic recovery |
| CN102408558A (en) * | 2011-09-21 | 2012-04-11 | 四川大学 | Long-chain branched poly(p-dioxanone) and preparation method thereof |
| CN102677217A (en) * | 2012-05-18 | 2012-09-19 | 东华大学 | Modified POM (polyoxymethylene) fiber and preparation method thereof |
| CN104499087A (en) * | 2014-12-23 | 2015-04-08 | 江苏苏博特新材料股份有限公司 | Preparation method of novel polyoxymethylene fibers |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103865087B (en) * | 2014-03-10 | 2016-06-08 | 山东理工大学 | A kind of method that poly-peptide film kindliness is improved by poly(lactic acid) and PPDO |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3608044A (en) * | 1969-01-28 | 1971-09-21 | Celanese Corp | Process for melt spinning polyoxymethylene filaments having elastic recovery |
| CN102408558A (en) * | 2011-09-21 | 2012-04-11 | 四川大学 | Long-chain branched poly(p-dioxanone) and preparation method thereof |
| CN102677217A (en) * | 2012-05-18 | 2012-09-19 | 东华大学 | Modified POM (polyoxymethylene) fiber and preparation method thereof |
| CN104499087A (en) * | 2014-12-23 | 2015-04-08 | 江苏苏博特新材料股份有限公司 | Preparation method of novel polyoxymethylene fibers |
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