CN107723844A - A kind of preparation method of high temperature resistant PLA fibers - Google Patents
A kind of preparation method of high temperature resistant PLA fibers Download PDFInfo
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- CN107723844A CN107723844A CN201711000152.1A CN201711000152A CN107723844A CN 107723844 A CN107723844 A CN 107723844A CN 201711000152 A CN201711000152 A CN 201711000152A CN 107723844 A CN107723844 A CN 107723844A
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- high temperature
- temperature resistant
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- pla
- pla fibers
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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
-
- 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
-
- 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
- D01F1/103—Agents inhibiting growth of microorganisms
-
- 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
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- 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
Abstract
The invention discloses a kind of preparation method of high temperature resistant PLA fibers, comprise the following steps：PLA, polyvinyl alcohol, poly butylene succinate, sepiolite powder, calcined kaolin, vaseline, glycerine polyoxyethylene polyoxypropylene blocked copolymer are stirred to obtain pretreatment PLA；Antibiotic complex, tricresyl phosphate, Masterbatch, epoxidized soybean oil, antioxidant are added into pretreatment PLA to stir, is sent into double screw extruder and extrudes, is cooled down, and melt spinning obtains high temperature resistant PLA fibers.Antibiotic complex is prepared using following technique：Calcium hydroxide, water are mixed, room temperature ageing, AEO grinding is added, is passed through air and pressurizes; heating stirring, add copper nitrate, magnesium stearate, atoleine stirring, under nitrogen protection, heating stirring; filtering, washing, is dried to obtain antibiotic complex.The inventive method is simple, and cost is cheap, can effectively improve the toughness and heat endurance of acid fiber by polylactic, and gained acid fiber by polylactic is green, degradable.
Description
Technical field
The present invention relates to textile fiber technology field, more particularly to a kind of preparation method of high temperature resistant PLA fibers.
Background technology
In order to form nonwoven web from Biodegradable polymeric, various trials are had been carried out.Although it can be dropped by biology
Fiber prepared by the polymer of solution is known, but their use has encountered problem.Polylactic acid PLA is to be used to be formed
One of the most common biodegradable of nonwoven web and sustainable (reproducible) polymer.
PLA fibers generally have low bonding pliability and high roughness, have attempted to drop using plasticizer at present
Lower glass transition temperatures simultaneously improve cohesive and pliability, but degraded, melt strength and stretching after causing melt spinning
Ability reduces obvious, it would be highly desirable to solves.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of preparation method of high temperature resistant PLA fibers, side
Method is simple, is easy to practical operation, and cost is cheap, can effectively improve the toughness and heat endurance of acid fiber by polylactic, and gained gathers
Acid fiber is green, degradable, can be applied to field of textile.
A kind of preparation method of high temperature resistant PLA fibers proposed by the present invention, comprises the following steps：
S1, by PLA, polyvinyl alcohol, poly butylene succinate, sepiolite powder, calcined kaolin, vaseline, the third three
Alcohol polyoxyethylene polyoxypropylene blocked copolymer stirs to obtain pretreatment PLA；
S2, add antibiotic complex, tricresyl phosphate, Masterbatch, epoxidized soybean oil, antioxygen into pretreatment PLA
Agent stirs, and is sent into double screw extruder and extrudes, and cools down, and melt spinning obtains high temperature resistant PLA fibers.
Preferably, in S1, mixing time 1-2h, mixing speed 300-400r/min.
Preferably, in S1, PLA, polyvinyl alcohol, poly butylene succinate, sepiolite powder, calcined kaolin, all scholars
Woods, the weight ratio of glycerine polyoxyethylene polyoxypropylene blocked copolymer are 50-60：15-25：1-2：5-10：2-6：1-3：
1-3。
Preferably, in S2, whipping temp is 140-155 DEG C, mixing speed 600-750r/min.
Preferably, in S2, extrusion temperature is 195-205 DEG C.
Preferably, it is pretreatment PLA, antibiotic complex, tricresyl phosphate, Masterbatch, epoxidized soybean oil, anti-in S2
The weight ratio of oxygen agent is 90-100：1-4：1-2：1-2：1-2：1-2.
Preferably, in S2, antibiotic complex is prepared using following technique：Calcium hydroxide, water are mixed, room temperature ageing, added
Enter AEO grinding, be passed through air and pressurize, heating stirring, add copper nitrate, magnesium stearate, atoleine and stir
Mix, under nitrogen protection, heating stirring, filter, washing, be dried to obtain antibiotic complex.
Preferably, in the preparation technology that S2 antibiotic complexes are adopted, milling time 5-15min, it is passed through air and is forced into
5-12Mpa。
Preferably, in S2, antibiotic complex is prepared using following technique：Calcium hydroxide, water are mixed, room temperature ageing, added
Enter AEO grinding 5-15min, be passed through air and be forced into 5-12Mpa, be warming up to 70-80 DEG C, stir 20-
30min, add copper nitrate, magnesium stearate, atoleine and stir 5-15min, mixing speed 2000-2400r/min, nitrogen is protected
Under shield, 200-240 DEG C is warming up to, stirs 5-15min, is filtered, washing, is dried to obtain antibiotic complex.
Preferably, it is calcium hydroxide, AEO, copper nitrate, hard in the preparation technology that S2 antibiotic complexes are adopted
Fatty acid magnesium, the weight ratio of atoleine are 20-30：1-3：5-10：0.5-1.2：20-30.
The inventive method is simple, is easy to practical operation, and cost is cheap, using PLA, polyvinyl alcohol composite, can effectively carry
The toughness and heat endurance of high acid fiber by polylactic, and it is green, it is degradable, it can be applied to field of textile.
In the antibiotic complex of the present invention, calcium hydroxide is after room temperature is aged, using AEO as nucleation
Agent, the calcium carbonate degree of scatter of formation is high, and particle coordinates up to nanoscale and adds copper nitrate effect, in magnesium stearate and liquid
In the presence of body paraffin, Nanometer Copper can be formed and be attached to calcium carbonate granule surface, not only particle diameter distribution is uniform, and in air not
It is oxidizable, it can be stably dispersed in antibiotic complex, antibacterial effect is fabulous；Antibiotic complex and pretreatment PLA compounding, point
It is good to dissipate property, it is well mixed each other, make acid fiber by polylactic resistance to elevated temperatures obtained by the present invention excellent, and can effectively strengthen poly- breast
The toughness of acid, it is not easy to break after spinning；And antibiotic complex compounds with sepiolite powder, calcined kaolin, bulk density is big, in body
Accounting is big in system, then vaseline, glycerine polyoxyethylene polyoxypropylene blocked copolymer cooperation under, with other raw materials point
Dissipate uniformly, further enhance acid fiber by polylactic resistance to elevated temperatures obtained by the present invention, and PLA dosage can be saved, reduce into
This.
The tensile strength of gained acid fiber by polylactic of the invention is 20-26MPa, elongation at break 420-460%, 200 DEG C
Heat-stable time is 240-260min, and hot elongation percentage is 185-193%, and quality weight-loss ratio is 35-42% after biodegradation, is expanded
The extents of spreading amd application of the polylactic acid fiber fabrics in field of textiles.
Embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of high temperature resistant PLA fibers, comprises the following steps：
S1, by 50g PLAs, 25g polyvinyl alcohol, 1g poly butylene succinates, 10g sepiolite powders, 2g calcine kaolinite
Soil, 3g vaseline, 1g glycerine polyoxyethylene polyoxypropylene blockeds copolymer stirring 2h, mixing speed 300r/min, are obtained
To pretreatment PLA；
S2, add 1g antibiotic complexes, 2g tricresyl phosphates, 1g Masterbatch, 2g rings into 100g pretreatment PLAs
Oxygen soybean oil, 1g antioxidant stir, and whipping temp is 155 DEG C, mixing speed 600r/min, is sent into double screw extruder
Middle extrusion, extrusion temperature are 205 DEG C, are cooled to room temperature, melt spinning obtains high temperature resistant PLA fibers.
Antibiotic complex is prepared using following technique：20g calcium hydroxides, 35g water are mixed, room temperature ageing, add 1g fat
Fat alcohol APEO grinds 15min, is passed through air and is forced into 5Mpa, is warming up to 80 DEG C, stirs 20min, adds 10g nitric acid
Copper, 0.5g magnesium stearates, 30g atoleines stirring 5min, mixing speed 2400r/min, under nitrogen protection, are warming up to 200
DEG C, 15min is stirred, is filtered, washing, is dried to obtain antibiotic complex.
The tensile strength of acid fiber by polylactic obtained by the present embodiment is 20MPa, elongation at break 460%, 200 DEG C of thermostabilizations
Time is 240min, and hot elongation percentage is 193%, and quality weight-loss ratio is 35% after biodegradation.
Embodiment 2
A kind of preparation method of high temperature resistant PLA fibers, comprises the following steps：
S1, by 60kg PLAs, 15kg polyvinyl alcohol, 2kg poly butylene succinates, 5kg sepiolite powders, 6kg calcine
Kaolin, 1kg vaseline, the stirring of 3kg glycerine polyoxyethylene polyoxypropylene blockeds copolymer 1h, mixing speed 400r/
Min, obtain pre-processing PLA；
S2, pre-process to 90kg added in PLA 4kg antibiotic complexes, 1kg tricresyl phosphates, 2kg Masterbatch,
1kg epoxidized soybean oils, 2kg antioxidant stir, and whipping temp is 140 DEG C, mixing speed 750r/min, is sent into twin-screw
Extruded in extruder, extrusion temperature is 195 DEG C, is cooled to room temperature, melt spinning obtains high temperature resistant PLA fibers.
Antibiotic complex is prepared using following technique：30g calcium hydroxides, 15g water are mixed, room temperature ageing, add 3g fat
Fat alcohol APEO grinds 5min, is passed through air and is forced into 12Mpa, is warming up to 70 DEG C, stirs 30min, adds 5g nitric acid
Copper, 1.2g magnesium stearates, 20g atoleines stirring 15min, mixing speed 2000r/min, under nitrogen protection, are warming up to 240
DEG C, 5min is stirred, is filtered, washing, is dried to obtain antibiotic complex.
The tensile strength of acid fiber by polylactic obtained by the present embodiment is 24MPa, elongation at break 430%, 200 DEG C of thermostabilizations
Time is 250min, and hot elongation percentage is 188%, and quality weight-loss ratio is 40% after biodegradation.
Embodiment 3
A kind of preparation method of high temperature resistant PLA fibers, comprises the following steps：
S1,52kg PLAs, 22kg polyvinyl alcohol, 1.2kg poly butylene succinates, 8kg sepiolite powders, 3kg forged
Burn kaolin, 2.5kg vaseline, 1.5kg glycerine polyoxyethylene polyoxypropylene blockeds copolymer stirring 1.8h, mixing speed
For 320r/min, obtain pre-processing PLA；
S2, add 2kg antibiotic complexes, 1.8kg tricresyl phosphates, 1.2kg color masterbatch into 98kg pretreatment PLAs
Grain, 1.8kg epoxidized soybean oils, 1.2kg antioxidant stir, and whipping temp is 150 DEG C, mixing speed 650r/min, is sent
Enter in double screw extruder and extrude, extrusion temperature is 202 DEG C, is cooled to room temperature, melt spinning obtains high temperature resistant PLA fibers.
Antibiotic complex is prepared using following technique：22kg calcium hydroxides, 30kg water are mixed, room temperature ageing, added
1.5kg AEOs grind 12min, are passed through air and are forced into 6Mpa, are warming up to 78 DEG C, stir 22min, add
8kg copper nitrates, 0.6kg magnesium stearates, the stirring of 28kg atoleines 8min, mixing speed 2300r/min, under nitrogen protection,
210 DEG C are warming up to, stirs 12min, is filtered, washing, is dried to obtain antibiotic complex.
The tensile strength of acid fiber by polylactic obtained by the present embodiment is 22MPa, elongation at break 450%, 200 DEG C of thermostabilizations
Time is 245min, and hot elongation percentage is 190%, and quality weight-loss ratio is 38% after biodegradation.
Embodiment 4
A kind of preparation method of high temperature resistant PLA fibers, comprises the following steps：
S1, by 58t PLAs, 18t polyvinyl alcohol, 1.8t poly butylene succinates, 6t sepiolite powders, 5t calcine kaolinite
Soil, 1.5t vaseline, the stirring of 2.5t glycerine polyoxyethylene polyoxypropylene blockeds copolymer 1.2h, mixing speed 380r/
Min, obtain pre-processing PLA；
S2, pre-process to 92t added in PLA 3t antibiotic complexes, 1.2t tricresyl phosphates, 1.8t Masterbatch,
1.2t epoxidized soybean oils, 1.8t antioxidant stir, and whipping temp is 145 DEG C, mixing speed 700r/min, are sent into double spiral shells
Extruded in bar extruder, extrusion temperature is 198 DEG C, is cooled to room temperature, melt spinning obtains high temperature resistant PLA fibers.
Antibiotic complex is prepared using following technique：28kg calcium hydroxides, 20kg water are mixed, room temperature ageing, added
2.5kg AEOs grind 8min, are passed through air and are forced into 10Mpa, are warming up to 72 DEG C, stir 28min, add
6kg copper nitrates, 1kg magnesium stearates, 22kg atoleines stirring 12min, mixing speed 2100r/min, under nitrogen protection, rise
Temperature stirs 8min to 230 DEG C, filters, and washing, is dried to obtain antibiotic complex.
The tensile strength of acid fiber by polylactic obtained by the present embodiment is 26MPa, elongation at break 420%, 200 DEG C of thermostabilizations
Time is 260min, and hot elongation percentage is 185%, and quality weight-loss ratio is 42% after biodegradation.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of high temperature resistant PLA fibers, it is characterised in that comprise the following steps：
S1, PLA, polyvinyl alcohol, poly butylene succinate, sepiolite powder, calcined kaolin, vaseline, glycerine gathered
Oxygen ethene oxypropylene block formula copolymer stirs to obtain pretreatment PLA；
S2, into pretreatment PLA, addition antibiotic complex, tricresyl phosphate, Masterbatch, epoxidized soybean oil, antioxidant stir
Mix uniformly, be sent into double screw extruder and extrude, cool down, melt spinning obtains high temperature resistant PLA fibers.
2. the preparation method of high temperature resistant PLA fibers according to claim 1, it is characterised in that in S1, mixing time 1-
2h, mixing speed 300-400r/min.
3. the preparation method of high temperature resistant PLA fibers according to claim 1 or claim 2, it is characterised in that in S1, PLA, poly- second
Enol, poly butylene succinate, sepiolite powder, calcined kaolin, vaseline, glycerine polyoxyethylene polyoxypropylene blocked
The weight ratio of copolymer is 50-60：15-25：1-2：5-10：2-6：1-3：1-3.
4. according to the preparation method of any one of the claim 1-3 high temperature resistant PLA fibers, it is characterised in that in S2, stirring temperature
Spend for 140-155 DEG C, mixing speed 600-750r/min.
5. according to the preparation method of any one of the claim 1-4 high temperature resistant PLA fibers, it is characterised in that in S2, extrusion temperature
Spend for 195-205 DEG C.
6. according to the preparation method of any one of the claim 1-5 high temperature resistant PLA fibers, it is characterised in that in S2, pretreatment
PLA, antibiotic complex, tricresyl phosphate, Masterbatch, epoxidized soybean oil, the weight ratio of antioxidant are 90-100：1-4：
1-2：1-2：1-2：1-2.
7. according to the preparation method of any one of the claim 1-6 high temperature resistant PLA fibers, it is characterised in that in S2, antibacterial is multiple
Compound is prepared using following technique：Calcium hydroxide, water are mixed, room temperature ageing, AEO grinding is added, is passed through
Air simultaneously pressurizes, heating stirring, adds copper nitrate, magnesium stearate, atoleine stirring, under nitrogen protection, heating stirring, and mistake
Filter, washing, is dried to obtain antibiotic complex.
8. according to the preparation method of any one of the claim 1-7 high temperature resistant PLA fibers, it is characterised in that S2 antibacterials are compound
In the preparation technology that thing is adopted, milling time 5-15min, it is passed through air and is forced into 5-12Mpa.
9. according to the preparation method of any one of the claim 1-8 high temperature resistant PLA fibers, it is characterised in that in S2, antibacterial is multiple
Compound is prepared using following technique：Calcium hydroxide, water are mixed, room temperature ageing, add AEO grinding 5-
15min, be passed through air and be forced into 5-12Mpa, be warming up to 70-80 DEG C, stir 20-30min, add copper nitrate, magnesium stearate,
Atoleine stirs 5-15min, mixing speed 2000-2400r/min, under nitrogen protection, is warming up to 200-240 DEG C, stirring
5-15min, filter, washing, be dried to obtain antibiotic complex.
10. according to the preparation method of any one of the claim 1-9 high temperature resistant PLA fibers, it is characterised in that S2 antibacterials are compound
In the preparation technology that thing is adopted, calcium hydroxide, AEO, copper nitrate, magnesium stearate, the weight ratio of atoleine are
20-30：1-3：5-10：0.5-1.2：20-30.
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| CN201711000152.1A CN107723844A (en) | 2017-10-24 | 2017-10-24 | A kind of preparation method of high temperature resistant PLA fibers |
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| CN201711000152.1A CN107723844A (en) | 2017-10-24 | 2017-10-24 | A kind of preparation method of high temperature resistant PLA fibers |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112920566A (en) * | 2021-03-05 | 2021-06-08 | 柳州塑友科技有限公司 | Modified PLA (polylactic acid) fully-degradable plastic and preparation method thereof |
| CN113279086A (en) * | 2021-05-07 | 2021-08-20 | 东部湾(扬州)生物新材料有限公司 | Preparation method of polylactic acid composite ultrashort non-crimped fiber precursor |
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| CN1891870A (en) * | 2005-07-05 | 2007-01-10 | 中国石化仪征化纤股份有限公司 | Method for producing antibacterial polylactic acid fiber |
| CN104206420A (en) * | 2014-08-07 | 2014-12-17 | 蔡惠萍 | Preparation method and application of silver-free powdery solid solution anti-bacterial agent |
| CN105696106A (en) * | 2014-11-27 | 2016-06-22 | 黑龙江鑫达企业集团有限公司 | Preparation method of antibiotic polylactic acid fibers |
| CN107090609A (en) * | 2017-05-27 | 2017-08-25 | 安徽桑尼旅游休闲用品有限公司 | A kind of acid fiber by polylactic preparation method for outdoor goods |
| CN107312261A (en) * | 2017-06-20 | 2017-11-03 | 安徽瑞侃电缆科技有限公司 | A kind of polyvinyl chloride cable sheathing compound for automotive wire bundle |
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2017
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1891870A (en) * | 2005-07-05 | 2007-01-10 | 中国石化仪征化纤股份有限公司 | Method for producing antibacterial polylactic acid fiber |
| CN104206420A (en) * | 2014-08-07 | 2014-12-17 | 蔡惠萍 | Preparation method and application of silver-free powdery solid solution anti-bacterial agent |
| CN105696106A (en) * | 2014-11-27 | 2016-06-22 | 黑龙江鑫达企业集团有限公司 | Preparation method of antibiotic polylactic acid fibers |
| CN107090609A (en) * | 2017-05-27 | 2017-08-25 | 安徽桑尼旅游休闲用品有限公司 | A kind of acid fiber by polylactic preparation method for outdoor goods |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112920566A (en) * | 2021-03-05 | 2021-06-08 | 柳州塑友科技有限公司 | Modified PLA (polylactic acid) fully-degradable plastic and preparation method thereof |
| CN113279086A (en) * | 2021-05-07 | 2021-08-20 | 东部湾(扬州)生物新材料有限公司 | Preparation method of polylactic acid composite ultrashort non-crimped fiber precursor |
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Application publication date: 20180223 |