CN1974893A - Prepn process of paraphthalic acid-butanediol succinate copolymer fiber - Google Patents
Prepn process of paraphthalic acid-butanediol succinate copolymer fiber Download PDFInfo
- Publication number
- CN1974893A CN1974893A CN 200610118400 CN200610118400A CN1974893A CN 1974893 A CN1974893 A CN 1974893A CN 200610118400 CN200610118400 CN 200610118400 CN 200610118400 A CN200610118400 A CN 200610118400A CN 1974893 A CN1974893 A CN 1974893A
- Authority
- CN
- China
- Prior art keywords
- temperature
- spinning
- pbst
- finish
- representative
- 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.)
- Granted
Links
Landscapes
- Artificial Filaments (AREA)
Abstract
The present invention discloses preparation process of paraphthalic acid-butanediol succinate copolymer fiber. The present invention features: 1. spinning temperature C1=200 deg.c, C2=220-230 deg.c, C3=220-230 deg.c, C4=220-230 deg.c, GP2=220-230 deg.c, PP2=220-230 deg.c, SP=225-240 deg.c; 2. lateral blowing temperature of 20-35 deg.c and air speed of 0.5 m/min; and 3. the distance between the spinning jet and the winding disc of 2-5 m. The present invention is process capable of preparing industrial fiber with paraphthalic acid-butanediol succinate copolymer and has excellent industrial application foreground.
Description
Technical field
The present invention relates to a kind of high molecular polymer fiber preparation method, be specifically related to poly terephthalic acid-common-succinic acid-butanediol ester fiber preparation method.
Background technology
Macromolecular material is since coming out, because its excellent function superiority and practicality be the new material that people produce, life provides many function admirables, yet the flourish of it have also been brought white elephant to environment, caused the aggravation of environmental pollution.The discarded object of macromolecular material be difficult to decompose (common plastics need 100～150 years ability to divide fully take off), and present refuse processing method is buried, burned and reclaim all and can not well solve its root problem.In order to solve an above-mentioned difficult problem, the research and development biodegradation material becomes a big focus.
In recent decades, biodegradated polymer materal has obtained development fast, has worked out a large amount of biodegradated polymer materals and progressively has been applied to every field, as aviation, medicine, film, fiber, injection moulding, blowing product and fields such as sheet material or coating.These biodegradation materials mainly comprise polyhydroxyalkanoate (PHA), PLA (PLA) and this three bulk of poly butylene succinate (PBS) class.At present, with respect to the research work of external Biodegradable material, domesticly still belong to the starting stage.Wherein PBS is because its fusing point is lower, and the general character with aliphatic polyester is the not high characteristic of physical and mechanical properties, be difficult to satisfy the requirement in some field, thereby its practical application is restricted.In conjunction with polybutylene terephthalate (PBT) (PBT) fusing point height, characteristics such as the fast and mechanical performance excellence of crystallization rate, relevant scientific and technical personnel have researched and developed a kind of copolymer poly terephthalic acid-common-succinic acid-butanediol ester (PBST).It has had the good mechanical mechanical performance again when possessing original PBS biodegradable performance, be a kind of prospect biodegradation material preferably.PBST (poly terephthalic acid-altogether-succinic acid-butanediol ester) be by dimethyl terephthalate (DMT), dimethyl succinate, the butanediol three forms by polycondensation addition reaction copolymerization.It is a kind of biodegradable polyesters of novelty, is a kind of modification by copolymerization product to biodegradable polyesters PBS (poly butylene succinate).
But, how said PBST is adopted suitable method preparation to become fiber, to be applied to field of textiles, be the very problem of concern of people institute.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of poly terephthalic acid-common-succinic acid-butanediol ester fiber preparation method, to satisfy the needs of relevant field development.
Technical conceive of the present invention is such:
Because PBST is by dimethyl terephthalate (DMT), dimethyl succinate, the butanediol three forms by polycondensation addition reaction copolymerization, it is a kind of biodegradable polyesters of novelty, it has and the conventional different rheological behavior of polyester, be the thinning type non-newtonian fluid of typical shear force under molten condition, its apparent viscosity reduces with the increase of shear rate; Along with the rising of melt temperature and reducing of molecular weight of copolymer, flow curve moves down, and apparent viscosity reduces; The degree that departs from Newtonianism along with the increase melt of copolymerization molecular weight increases, and promptly n reduces; And, depart from the Newtonianism degree to reduce along with the rising of temperature; Therefore, adopt the fiber preparation method of conventional polyester, can not obtain high performance PBST, need be according to the rheological property of PBST, research is suitable for the process conditions of PBST fiber production.
Method of the present invention comprises the steps:
Copolymer poly terephthalic acid-common-succinic acid-butanediol ester section is put into and is heated into melt in the spinning machine, extrude the formation strand from the spinnerets of spinning machine then, through the lateral blowing cooling of spray silk path,, oil and become a branch of multifilament through upper oil-pan by last draw-off godet bunchy, again through following draw-off godet, regulate strand tension force by clips and be wound into the silk tube, obtained the PBST as-spun fibre, then the PBST as-spun fibre that is obtained is deposited 5h～13h through friction roller, carry out drawing-off again, obtain product;
It is characterized in that:
(1) spinning temperature is:
C1＝200℃，C2＝220℃～230℃，C3＝220℃～230℃，C4＝220℃～230℃，GP2＝220℃～230℃，PP2＝220℃～230℃，SP＝225℃～240℃；
Wherein:
C1～C4 representative: the temperature in 4 districts of screw rod, GP2: the temperature of measuring pump, PP2 representative: the temperature of bend pipe, SP representative: the temperature of casing;
Spinning temperature is little to the influence of spinning moulding, but the quality of formation tow is had considerable influence;
(2) the lateral blowing temperature is: 20 ℃～35 ℃; Wind speed: 0.5m/min
(3) distance between spinnerets and the last winder, i.e. the distance of strand cooling is 2m～5m, if strand cooling distance too short (cooling is not enough) can cause tow to be clamminess, the tow unwinding is not got off during the coiling first break draft, has a strong impact on back processing;
(4) spinning speed (winding speed): V
Spin=800m/min～1000m/min; Jet stretch ratio is 70～120;
(5) said finish has played very important effect in spinning process, here volumetric concentration that used is is the mixture of the silicone oil of 8～12% shared finish of terylene polypropylene fibre and finish gross weight 1～5%, if do not add 1～5% silicone oil, then the coherent of tow is relatively poor, be unfavorable for that (the improper meeting of finish causes the tow cohesive force poor, and 36 hole silks can scatter, and are easy to generate lousiness during drawing-off in the drawing-off post processing, cause drawing-off unwinding difficulty, finally make the drafted fibre quality descend).
(6) the drawing-off temperature of heat plate is 70 ℃～80 ℃, and hot plate temperature is 140 ℃～160 ℃, and drafting multiple is 1.5 times～2.2 times.
PBST is a kind of semi-crystalline polymer, and the degree of crystallinity that has improved PBST by drawing-off makes it have certain mechanical property.
The PBST as-spun fibre of spinning silk winding gained is not have orientation substantially, degree of crystallinity is lower, its mechanical strength is relatively poor (powerful low, elongation is big), by the one-level draft process make the macromolecular chain of PBST as-spun fibre unfold and along fiber axis to oriented, thereby play degree of crystallinity and be improved, mechanical property also increases, certain intensity can be arranged, be applicable to the industry production application.
Fibrous mechanical property after the PBST drawing-off:
Fiber number: 126.88dtex～292.41dtex
Intensity: 1.899cN/dtex～3.478cN/dtex
Elongation at break: 15.997%～109.577%
A rebound degree:
The rebound degree of anxious resilience: 78.67%～85.33%
The rebound degree of slow resilience: 95.33%～99.33%
Boiling water shrinkage: 65%～76.4%
By above-mentioned disclosed technical scheme as seen, method of the present invention can become copolymer poly terephthalic acid-common-succinic acid-butanediol ester preparation industrial fiber easy to use, have bigger industrial applications prospect.
The specific embodiment
Embodiment 1
Section molecular weight: Mw=1.38 * 10
5
Spinning process condition:
Spinning temperature (seven districts):
| C1 (℃) | C2 (℃) | C3 (℃) | C4 (℃) | GP2 (℃) | PP2 (℃) | SP (℃) |
| 200 | 230 | 230 | 230 | 228 | 230 | 240 |
Spinning speed (winding speed): V
Spin=800m/min;
Jet stretch ratio: Φ=70.686;
Finish: the shared finish 1000ml+1% of 10% terylene polypropylene fibre silicone oil;
Spinnerets: 36f[hole] (aperture: d=0.3mm);
Baking material equipment, time and temperature: rotary drum, 12 hours, 100 ℃ (moisture content＜30ppm);
Lateral blowing: 30 ℃, wind speed: 0.5m/min;
Just stretch fiber resting period: 5.5h
Drawing-off: temperature of heat plate: 80 ℃, hot plate temperature: 160 ℃, drafting multiple: 1.5 times
Fiber number: 240.50dtex, intensity: 1.89938cN/dtex, extension at break: 49.364%, boiling water shrinkage: 71%, rebound degree: the rebound degree of anxious resilience: 79.33%, the rebound degree of slow resilience: 96.33%.
Above-mentioned fibre property adopts China. and State Standard of the People's Republic of China (GB) detects.
Embodiment 2
Section: molecular weight: Mw=2.03 * 10
5
Spinning temperature (seven districts):
| C1 (℃) | C2 (℃) | C3 (℃) | C4 (℃) | GP2 (℃) | PP2 (℃) | SP (℃) |
| 200 | 223 | 223 | 223 | 223 | 220 | 225 |
Spinning speed (winding speed): V
Spin=1000m/min (coiling chamber room temperature: 23 ℃);
Jet stretch ratio: Φ=116.196
Finish: the shared finish 1000ml+1.5% of 10% terylene polypropylene fibre silicone oil;
Spinnerets: 36f[hole] (aperture: d=0.3mm);
Baking material equipment, time and temperature: rotary drum, 24 hours, 100 ℃ (moisture content＜30ppm);
Lateral blowing: 20 ℃, wind speed: 0.5m/min;
Just stretch fiber resting period: 13h
Drawing-off: temperature of heat plate: 80 ℃, hot plate temperature: 140 ℃, drafting multiple: 1.9 times;
Fiber: fiber number: 128.60dtex, intensity: 2.97289cN/dtex, extension at break: 31.435% boiling water shrinkage: 74%, rebound degree: the rebound degree of anxious resilience: 82.33%, the rebound degree of slow resilience: 97.33%.
Claims (5)
1. poly terephthalic acid-altogether-succinic acid-butanediol ester fiber preparation method, comprise the steps: copolymer poly terephthalic acid-common-succinic acid-butanediol ester section is put into and is heated into melt in the spinning machine, extrude the formation strand from the spinnerets of spinning machine then, through the lateral blowing cooling of spray silk path, by last draw-off godet bunchy, oil and become a branch of multifilament through upper oil-pan, again through following draw-off godet, regulate strand tension force by clips and be wound into the silk tube through friction roller, obtained the PBST as-spun fibre, then the PBST as-spun fibre that is obtained is deposited 5h～13h, carry out drawing-off again, obtain product; It is characterized in that:
(1) spinning temperature is:
C1＝200℃，C2＝220℃～230℃，C3＝220℃～230℃，C4＝220℃～230℃，GP2＝220℃～230℃，PP2＝220℃～230℃，SP＝225℃～240℃；
Wherein:
C1～C4 representative: the temperature in 4 districts of screw rod, GP2: the temperature of measuring pump, PP2 representative: the temperature of bend pipe, SP representative: the temperature of casing;
(2) the lateral blowing temperature is: 20 ℃～35 ℃; Wind speed: 0.5m/min;
(3) distance between spinnerets and the last winder is 2m～5m.
2. method according to claim 1 is characterized in that, spinning speed V
Spin=800m/min～1000m/min.
3. method according to claim 1 is characterized in that, jet stretch ratio is 70～120.
4. method according to claim 1 is characterized in that, said finish is that volumetric concentration is the mixture of the silicone oil of 8～12% shared finish of terylene polypropylene fibre and finish gross weight 1～5%.
5. method according to claim 1 is characterized in that, the drawing-off temperature of heat plate is 70 ℃～80 ℃, and hot plate temperature is 140 ℃～160 ℃, and drafting multiple is 1.5 times～2.2 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101184008A CN100412242C (en) | 2006-11-16 | 2006-11-16 | Prepn process of paraphthalic acid-butanediol succinate copolymer fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101184008A CN100412242C (en) | 2006-11-16 | 2006-11-16 | Prepn process of paraphthalic acid-butanediol succinate copolymer fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1974893A true CN1974893A (en) | 2007-06-06 |
| CN100412242C CN100412242C (en) | 2008-08-20 |
Family
ID=38125233
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101184008A Active CN100412242C (en) | 2006-11-16 | 2006-11-16 | Prepn process of paraphthalic acid-butanediol succinate copolymer fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100412242C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660218B (en) * | 2009-08-24 | 2011-08-10 | 江苏鹰翔化纤股份有限公司 | Preparation method of chinlon and olybuthylenesuccinate collateral fiber |
| CN106480535A (en) * | 2016-10-31 | 2017-03-08 | 江苏苏博特新材料股份有限公司 | A kind of method that polyformaldehyde fibre prepared by melt spinning |
| CN114016158A (en) * | 2021-11-23 | 2022-02-08 | 中国纺织科学研究院有限公司 | Broad PBST and polylactic acid composite fiber, preparation method and application thereof, and surgical clothing |
| CN114540983A (en) * | 2022-03-22 | 2022-05-27 | 中国纺织科学研究院有限公司 | Low-cost biodegradable composite fiber and preparation method and application thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002173827A (en) * | 2000-12-05 | 2002-06-21 | Kureha Chem Ind Co Ltd | Monofilament, method for manufacturing monofilament and fishing line |
| JP2003213529A (en) * | 2002-01-11 | 2003-07-30 | Chisso Corp | Biodegradable conjugated fiber and fiber structure and absorption article using the same |
-
2006
- 2006-11-16 CN CNB2006101184008A patent/CN100412242C/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660218B (en) * | 2009-08-24 | 2011-08-10 | 江苏鹰翔化纤股份有限公司 | Preparation method of chinlon and olybuthylenesuccinate collateral fiber |
| CN106480535A (en) * | 2016-10-31 | 2017-03-08 | 江苏苏博特新材料股份有限公司 | A kind of method that polyformaldehyde fibre prepared by melt spinning |
| CN114016158A (en) * | 2021-11-23 | 2022-02-08 | 中国纺织科学研究院有限公司 | Broad PBST and polylactic acid composite fiber, preparation method and application thereof, and surgical clothing |
| CN114540983A (en) * | 2022-03-22 | 2022-05-27 | 中国纺织科学研究院有限公司 | Low-cost biodegradable composite fiber and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100412242C (en) | 2008-08-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110468468A (en) | Polyglycolic acid complete biodegradable composite fibre and preparation method thereof | |
| CN107805856B (en) | Polylactic acid composite fiber and preparation method thereof | |
| CN105220264B (en) | A kind of modified polylactic acid fiber and preparation method thereof | |
| US20120107527A1 (en) | Use of polymer blends for producing slit film tapes | |
| CN104514041B (en) | A kind of biodegradable fiber and preparation method thereof | |
| KR20160094836A (en) | Bicomponent conjugate fibers, complex yarns and fabrics having high crimping property | |
| CN112048783A (en) | Biodegradable brush wire and preparation method thereof | |
| CN104762695A (en) | Biodegradable polyester/recycled polyester sheath-core fiber and preparation method thereof | |
| JP2013542292A (en) | Use of polymer mixtures to produce slit film tape | |
| US20060058441A1 (en) | Polyester fibers, their production and their use | |
| CN110552079A (en) | Preparation method of super-hydrophobic polyester fiber | |
| CN111733474A (en) | Full-biodegradable dental floss and preparation method thereof | |
| CN1974893A (en) | Prepn process of paraphthalic acid-butanediol succinate copolymer fiber | |
| CN1051586C (en) | High modulus polyester yarn for tire cords and composites | |
| CN1932092A (en) | Prepn process of degradable aliphatic/aromatic copolymer fiber | |
| CN111101226A (en) | Bio-based degradable polyester fiber and preparation method thereof | |
| CN102586935B (en) | Preparation method of elastic fiber based on biomass polyester | |
| CN115679469B (en) | Preparation method and application of P34HB fiber | |
| JP4758317B2 (en) | Polyester core-sheath composite fiber | |
| JP2005299067A (en) | Polylactic acid fiber | |
| CN1220801C (en) | High viscosity poly ester monofilament and its producing method and use | |
| CN1696363A (en) | Composite fiber and its mfg. method | |
| CN110184678A (en) | A kind of preparation method of graphene and liquid crystal polyester co-reinforced polymer fiber | |
| CN113249815A (en) | Biodegradable PGA melt spinning forming method | |
| JP4207807B2 (en) | Method for producing cellulose fatty acid ester fiber |
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 | ||
| ASS | Succession or assignment of patent right |
Owner name: SHANGHAI SHUIXING DOMESTIC TEXTILE CO., LTD. Free format text: FORMER OWNER: DONGHUA UNIV. Effective date: 20090605 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20090605 Address after: No. 1487, Shanghai Hangzhou highway, Shanghai, Fengxian District Patentee after: Shuixing Domestic Textile Products Co., Ltd., Shanghai Address before: Shanghai City, West Yan'an Road No. 1882 Patentee before: Donghua University |
|
| C56 | Change in the name or address of the patentee |
Owner name: SHANGHAI SHUIXING HOME TEXTILE CO., LTD. Free format text: FORMER NAME: SHUIXING DOMESTIC TEXTILE PRODUCTS CO., LTD., SHANGHAI |
|
| CP03 | Change of name, title or address |
Address after: 201401, No. 1487, Shanghai Hangzhou highway, Shanghai, Fengxian District Patentee after: Shanghai Shuixing Home Textile Co., Ltd. Address before: 201401 No. 1487 Shanghai Fengxian District Shanghai Hangzhou highway Patentee before: Shuixing Domestic Textile Products Co., Ltd., Shanghai |