CN1304655C - Method for preparing poly lactic acid - Google Patents
Method for preparing poly lactic acid Download PDFInfo
- 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
- Authority
- CN
- China
- Prior art keywords
- lactic acid
- polylactic acid
- fibers
- preparation
- poly lactic
- Prior art date
- 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
Links
Landscapes
- Artificial Filaments (AREA)
- Biological Depolymerization Polymers (AREA)
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
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..
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 |
Family
ID=35041701
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100247698A Expired - Fee Related CN1304655C (en) | 2005-03-30 | 2005-03-30 | Method for preparing poly lactic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1304655C (en) |
Families Citing this family (4)
| 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)
| 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 |
-
2005
- 2005-03-30 CN CNB2005100247698A patent/CN1304655C/en not_active Expired - Fee Related
Patent Citations (1)
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1670273A (en) | 2005-09-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9365955B2 (en) | Fiber composition comprising 1,3-glucan and a method of preparing same | |
| RU2625306C2 (en) | Method of manufacture of lignin-containing prediminary fiber, and also of carbon fibers | |
| JP4018152B2 (en) | Lyocell fiber and method for producing the same | |
| CN1247838C (en) | Preparation method of polyacrylonitrile carbon raw yarn | |
| CN101492837B (en) | Process for producing bacteria cellulose fibre with high degree of polymerization | |
| AU707988B2 (en) | Apparatus and method for spinning hollow polymeric fibres | |
| Ozipek et al. | Wet spinning of synthetic polymer fibers | |
| CN110172740B (en) | Preparation method of flame-retardant cellulose fiber | |
| US20110156303A1 (en) | Spunbond wetlaid method for producing non-woven fabrics from natural cellulose | |
| CN104018294A (en) | Polylactic acid nanofiber membrane and preparation method thereof | |
| WO2012003070A1 (en) | Lignin/polyacrylonitrile-containing dopes, fibers, and methods of making same | |
| KR102062033B1 (en) | Method for producing moulded articles | |
| CN101942705B (en) | Preparation method of regenerated bacterial cellulose fiber | |
| CN107059150B (en) | A kind of preparation method of high intensity regenerated fibroin fiber | |
| CN1304655C (en) | Method for preparing poly lactic acid | |
| CN102453970B (en) | Low acetated cellulose fibers and preparation method thereof | |
| CN1687497A (en) | Method for preparing polymer blend fiber of poly lactic acids | |
| CN104032399A (en) | Preparation method for acetate fiber through dry-wet process | |
| CN109161973A (en) | The production technology of acid fiber by polylactic | |
| CN103060939B (en) | Preparation method of cellulose acetate fiber through polybasic carboxylic acid crosslinking | |
| CN107475782B (en) | A kind of acetate fiber and preparation method thereof | |
| CN104674358B (en) | Specially-shaped spinneret plate | |
| CN101736412A (en) | Preparation method of high-density regenerated fibre spinning solution | |
| WO2015049040A1 (en) | Method for producing moulded bodies | |
| KR101472097B1 (en) | Manufacturing method of cellulose fiber using ionic liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070314 Termination date: 20100330 |