CN1304655C - Method for preparing poly lactic acid - Google Patents

Method for preparing poly lactic acid Download PDF

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Publication number
CN1304655C
CN1304655C CNB2005100247698A CN200510024769A CN1304655C CN 1304655 C CN1304655 C CN 1304655C CN B2005100247698 A CNB2005100247698 A CN B2005100247698A CN 200510024769 A CN200510024769 A CN 200510024769A CN 1304655 C CN1304655 C CN 1304655C
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CN
China
Prior art keywords
lactic acid
polylactic acid
fibers
preparation
poly lactic
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CNB2005100247698A
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Chinese (zh)
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CN1670273A (en
Inventor
张秀芳
程正迪
赵炯心
沈新元
杨庆
郯志清
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Donghua University
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Donghua University
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Publication of CN1670273A publication Critical patent/CN1670273A/en
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Publication of CN1304655C publication Critical patent/CN1304655C/en
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Abstract

The present invention provides a method for preparing polylactic acid fiber by using a dry and wet method, which comprises the following steps: 1, polylactic acid slices are dissolved in trichloromethane solvent and then are mixed to be dissolved to form a polylactic acid solution of which the concentration is from 2.5% to 6%; the polylactic acid solution is extruded by orifices of which the length-diameter ratio is from 3 to 7:1 after debubbled and filtered to form fibers with holes; 2, the polylactic acid fibers enter a coagulating bath after flowing in the air by 1 to 5cm to be solidified and shaped; thereby, the fibers containing holes are obtained; 3, the fibers containing holes are washed in hot water; 4, the fibers are stretched in hot air or hot silicon oil; 5, the stretched fibers are coiled on a full bobbin in the form of filament; 6, the stretched fibers are thermally shaped. The produced fibers have the characteristics of fibers produced by the wet method and the dry method and are especially suitable for preparing medical organism macromolecular materials and tissue engineering materials.

Description

A kind of preparation method of poly lactic acid
Technical field
The present invention relates to a kind of preparation method of poly lactic acid, relate in particular to the method that a kind of dried wet method prepares poly lactic acid.
Background technology
In the prior art, prepare polylactic acid-based (Poly-L-lactic acid, dextrorotation PLA, left-handed-50: 50 polymer blends of dextrorotation PLA) fiber dry method commonly used and wet method.
Polylactic acid-based (the Poly-L-lactic acid of dry process, the dextrorotation PLA, left-handed-50: 50 polymer blends of dextrorotation PLA) fiber, be to adopt high-pressure hot air in the technical process, equipment is required high, and the important point is the necessary low boiling of solvent in the technical process of dry process fiber, and volatilization easily is so the requirement of solvent is very high.
And polylactic acid-based (Poly-L-lactic acid, dextrorotation PLA, left-handed-50: 50 polymer blends of dextrorotation PLA) fiber of wet method preparation because physical and mechanical properties is relatively poor, can not satisfy normal needs.
Summary of the invention
Problem to be solved by this invention is to provide a kind of preparation method of poly lactic acid, requires the shortcoming of the fibre property difference of height or preparation gained with preparation technology in the solution prior art.
The invention provides a kind of preparation method of poly lactic acid, this preparation method's bag
Draw together following steps:
1. polylactic acid-based section is dissolved in the chloroform solvent, stirring and dissolving, forming concentration is the polylactic acid-based solution of 2.5-6%, through deaeration, after the filtration, is 3-7 by draw ratio: 1 spinneret orifice pushes out and forms the fiber that has hole;
2. poly lactic acid is flowed in air behind the 1-5cm, enter solidified forming in the coagulating bath, obtain containing the fiber of hole;
3. in hot water, wash;
4. in hot-air or hot silicone oil, described silk is stretched;
5. the fiber after will stretching is wound on the bobbin with the form of long filament;
6. the fiber after will stretching carries out HEAT SETTING to be handled.
Wherein said polylactic acid-based be a kind of in 50: 50 polymer blends of Poly-L-lactic acid, dextrorotation PLA or left-handed-dextrorotation PLA, step 1. in polylactic acid-based section molecular weight IV 〉=2; The 2. middle used coagulating agent of coagulating bath of step is an alcohol, and the temperature of alcohol is 35-60 ℃; Step 3. in, washing temperature is 45-60 ℃; Step 4. in, draft temperature is 120-160 ℃; The step 6. temperature of middle HEAT SETTING is 120-160 ℃.
In stretching process, disposable stretching can reach 2 to 20 times to described fiber.
The present invention compared with prior art has following advantage:
This technology can make the choice of Solvent expanded range, spinning temperature does not rely on the temperature of coagulating bath, as-spun fibre is not vulnerable to high pressure on the spinnerets surface, be applicable to the technology that requires to be higher than normal solution concentration and high spinning speed, also be applicable to and produce special fiber product, especially for preparation medical bio macromolecular material and tissue engineering material.The structural behaviour of fiber can be regulated and control under required requirement, can have wet method simultaneously and the characteristics of dry process polylactic acid-based (left-handed, dextrorotation PLA, left-handed-50: 50 polymer blends of dextrorotation PLA) fiber.
Specific embodiment:
1. with the polylactic acid-based (Poly-L-lactic acid of molecular weight IV=2, the dextrorotation PLA, left-handed-50: 50 polymer blends of dextrorotation PLA) section be dissolved in the chloroform solvent, stirring and dissolving, formation concentration is 5% polylactic acid-based solution, through deaeration, after the filtration, be that 3: 1 spinneret orifice pushes out and forms the fiber that has irregular holes by draw ratio;
2. poly lactic acid is flowed in air behind the 5cm, enter solidified forming in the coagulating bath that contains 35% alcohol, obtain containing the fiber of irregular holes;
3. in 60 ℃ of hot water, wash;
4. in 120 ℃ of hot-airs, described fiber is stretched;
5. the fiber after will stretching is wound on the bobbin with the form of long filament;
6. the fiber after will stretching carries out 160 ℃ of HEAT SETTING to be handled.

Claims (6)

1. the preparation method of a poly lactic acid is characterized in that this preparation method comprises the steps:
1. polylactic acid-based section is dissolved in the chloroform solvent, stirring and dissolving, forming concentration is the polylactic acid-based solution of 2.5-6%, through deaeration, after the filtration, is 3-7 by draw ratio: 1 spinneret orifice pushes out and forms the fiber that has hole;
2. poly lactic acid is flowed in air behind the 1-5cm, enter solidified forming in the coagulating bath, obtain containing the fiber of hole;
3. in hot water, wash;
4. in hot-air or hot silicone oil, described silk is stretched;
5. the fiber after will stretching is wound on the bobbin with the form of long filament;
6. the fiber after will stretching carries out HEAT SETTING to be handled.
2. the preparation method of poly lactic acid according to claim 1, it is characterized in that described polylactic acid-based a kind of in 50: 50 polymer blends of Poly-L-lactic acid, dextrorotation PLA or left-handed-dextrorotation PLA, step 1. in polylactic acid-based section molecular weight IV 〉=2.
3. the preparation method of poly lactic acid according to claim 1 it is characterized in that the 2. middle used coagulating agent of coagulating bath of step is an alcohol, and the temperature of alcohol is 35-60 ℃.
4. the preparation method of poly lactic acid according to claim 1 is characterized in that step 3., and washing temperature is 45-60 ℃.
5. the preparation method of poly lactic acid according to claim 1 is characterized in that step 4., and draft temperature is 120-160 ℃.
6. the preparation method of poly lactic acid according to claim 1 is characterized in that the temperature of HEAT SETTING was 120-160 ℃ during step 6..
CNB2005100247698A 2005-03-30 2005-03-30 Method for preparing poly lactic acid Expired - Fee Related CN1304655C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB2005100247698A CN1304655C (en) 2005-03-30 2005-03-30 Method for preparing poly lactic acid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB2005100247698A CN1304655C (en) 2005-03-30 2005-03-30 Method for preparing poly lactic acid

Publications (2)

Publication Number Publication Date
CN1670273A CN1670273A (en) 2005-09-21
CN1304655C true CN1304655C (en) 2007-03-14

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Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009045877A1 (en) * 2007-09-28 2009-04-09 Natureworks Llc Methods for making polylactic acid stereocomplex fibers
CN101608346B (en) * 2009-07-24 2011-01-19 中国科学院宁波材料技术与工程研究所 Profiled polylactic acid fiber and preparation method thereof
CN104878458A (en) * 2015-05-27 2015-09-02 中国水产科学研究院东海水产研究所 Fishing polylactic acid monofilament manufacturing method
CN107761187B (en) * 2017-09-30 2021-03-26 同济大学 Method for preparing polylactic acid fiber through solution spinning

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1259176A (en) * 1997-05-02 2000-07-05 卡吉尔公司 Degradable polymer fibers, preparation, product, and methods of use

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1259176A (en) * 1997-05-02 2000-07-05 卡吉尔公司 Degradable polymer fibers, preparation, product, and methods of use

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Granted publication date: 20070314

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