CN1670273A - Method for preparing poly lactic acid - Google Patents

Method for preparing poly lactic acid Download PDF

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Publication number
CN1670273A
CN1670273A CN 200510024769 CN200510024769A CN1670273A CN 1670273 A CN1670273 A CN 1670273A CN 200510024769 CN200510024769 CN 200510024769 CN 200510024769 A CN200510024769 A CN 200510024769A CN 1670273 A CN1670273 A CN 1670273A
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CN
China
Prior art keywords
lactic acid
fiber
preparation
poly
poly lactic
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Application number
CN 200510024769
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Chinese (zh)
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CN1304655C (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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Priority to CNB2005100247698A priority Critical patent/CN1304655C/en
Publication of CN1670273A publication Critical patent/CN1670273A/en
Application granted granted Critical
Publication of CN1304655C publication Critical patent/CN1304655C/en
Expired - Fee Related legal-status Critical Current
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Abstract

The invention supplies a method to manufacturing poly-lactic acid fiber by dry-wet method. It includes the following steps: dissolving the slice up of the poly-lactic acid into trichloromethane solvent to form poly-lactic acid solution that the consistence is 2.5-6%, and forming fiber carrying holes after pressing from silk spraying hole that the length-width ratio is 3-7:1 after doffing and filtrating; putting the poly-lactic acid fiber flowing in the air for 1-5cm, sending into the concretion liquid for concreting and shaping then the fiber carrying holes would be available; washing in hot water; extending in hot air or hot silicone oil, rolling the extended fiber onto canister in filament type; taking heat shaping process to the extended fiber. The fiber has the feature of the fiber that manufactured by dry-wet method.

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 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.
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 true CN1670273A (en) 2005-09-21
CN1304655C CN1304655C (en) 2007-03-14

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN101878330B (en) * 2007-09-28 2014-07-23 自然工作有限责任公司 Methods for making polylactic acid stereocomplex fibers
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
CN107761187A (en) * 2017-09-30 2018-03-06 同济大学 A kind of method that acid fiber by polylactic is prepared by solution-polymerized SBR

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE69826457T2 (en) * 1997-05-02 2005-10-13 Cargill, Inc., Minneapolis DEGRADABLE POLYMER FIBERS: MANUFACTURE, PRODUCTS AND USE PROCESSES

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101878330B (en) * 2007-09-28 2014-07-23 自然工作有限责任公司 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
CN107761187A (en) * 2017-09-30 2018-03-06 同济大学 A kind of method that acid fiber by polylactic is prepared by solution-polymerized SBR
CN107761187B (en) * 2017-09-30 2021-03-26 同济大学 Method for preparing polylactic acid fiber through solution spinning

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Publication number Publication date
CN1304655C (en) 2007-03-14

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Granted publication date: 20070314

Termination date: 20100330