CN101215728A - Isosorbide modified polyester fiber and preparing method thereof - Google Patents
Isosorbide modified polyester fiber and preparing method thereof Download PDFInfo
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- CN101215728A CN101215728A CNA2008100326462A CN200810032646A CN101215728A CN 101215728 A CN101215728 A CN 101215728A CN A2008100326462 A CNA2008100326462 A CN A2008100326462A CN 200810032646 A CN200810032646 A CN 200810032646A CN 101215728 A CN101215728 A CN 101215728A
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- modified polyester
- polyester fiber
- isosorbide modified
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- polycondensation
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Abstract
The invention relates to modified polyester fiber of hydronol and a process for preparation. The fiber which takes DMT or PTA, ethandiol, hydronol and auxiliary agent as raw material is prepared through spinning, which comprises according to mass percent DMT or PTA 50-70%, ethandiol 10-49%, hydronol 0-39% and auxiliary agent 0.01-1%. The process for preparation comprises preparing DMT (or PTA), ethandiol and hydronol into polyester through copolymerization method by utilizing polymeric device, and then preparing fiber through spinning by utilizing the existing spinning device. The invention can utilize the existing polymeric device and spinning device to polymerize or spin, polyester which is prepared has good toughness, rigidity and thermal property, fiber has good spinning performance, and particularly dyeing behavior is greatly improved.
Description
Technical field
The present invention relates to the polyester fiber field, particularly relate to a kind of isosorbide modified polyester fiber and preparation method.
Background technology
Polyethylene terephthalate (PET) is one of present most important synthetic material, has good heat resistance, resistance to chemical reagents, mechanical property and electric property, especially transparent good, insulating properties is good, production cost is lower and cost performance is higher.PET is mainly used in fiber, biaxially oriented film and polyester bottles and various packing containers etc., full-bodied PET also is used widely in fields such as the bearing of engineering plastics, gear, electric parts, in addition, also constantly increase with PET proportion in the plastics at car.But because PET also exists down problem such as slow excessively, impact property difference of crystallization rate and easy moisture absorption of processing mould temperature (70~110 ℃), therefore, how to prepare have high toughness and rigidity, the modified PET of good processability become one of hot subject of domestic and international research.
The high polymer blending modification method is simple and easy to do, very big advantage is arranged technically and economically, and it has not only kept the advantage of original high polymer, more owing to added new material, give high polymer new performance by changing aggregated structure, had certain theory and practical value.So blending and modifying is that nearly 2 years polymer modifications are used one of maximum method.The mechanical property etc. of rheological property, crystal property and the material of co-mixing system can be improved by blending and modifying, especially shock resistance can be improved.At present, blending and modifying mainly contains PET/PEN (PEN) blending and modifying, PET/ECDP (the atmospheric cation dyestuff boils and dyes polyester)/PEG (polyethylene glycol) blending and modifying, PET/PP blending and modifying etc.
Chemical modification is meant in a kind of component and adds another kind of or chemical reactions such as several component generation copolymerization, polycondensation, forms a kind of method of modifying of new polymer.Chemical modification is to improve the means that the fusing point of polymer, vitrification point and morphosis etc. are provided convenience, and also provides thinking for the problems such as crystal property, morphosis, shock resistance and processing characteristics that solve PET.
Nano particle is meant elementide or the particulate of particle diameter at 1nm~100nm.Compare with ordinary particle, have unique light, electricity, magnetic and chemical characteristic, be mainly reflected in aspects such as quantum size effect, skin effect, interfacial effect.Have the scholar to think, nano particle will be 21 century one of the most promising material.All it has been done a large amount of research reports both at home and abroad.It is applied in the macromolecular material, has produced great effect for the through engineering approaches and the functionalization of material.Nano modification mainly contains PET/ nanometer SiO
2Composite modified, inorganic ultramicro powder (SiO
2/ TiO
2/ imvite)/PET is composite modified, PET/ nanometer MMT (imvite) is composite modified etc.
Summary of the invention
The purpose of this invention is to provide a kind of isosorbide modified polyester fiber and preparation method, the polyester of preparation has good toughness, rigidity and hot property, and fiber has good spinning property, and particularly dyeability improves a lot.
A kind of isosorbide modified polyester fiber of the present invention, be to be that raw material is made through spinning with DMT (dimethyl terephthalate (DMT)) or PTA (p-phthalic acid), ethylene glycol, isobide and auxiliary agent, its component that constitutes by mass percentage is DMT or PTA 50~70%, ethylene glycol 10~49%, isobide 0~39%, auxiliary agent 0.01~1%.
Described auxiliary agent is one or more of antioxidant, esterification catalyst, polycondensation catalyst.
Described antioxidant is 1010 antioxidant [four [methyl-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters];
Described esterification catalyst is alkali metal acetates such as zinc acetate, manganese acetate, cobalt acetate, lead acetate;
Described polycondensation catalyst is alkali metal oxides such as antimonous oxide, titanium oxide, cobalt oxide, chromium oxide.
The preparation method of isosorbide modified polyester fiber of the present invention, comprise the preparation of isosorbide modified polyester and having isosorbide modified polyester now on spinning equipment spinning, the preparation of isosorbide modified polyester wherein is to utilize existing polymerization unit to prepare by copolymerization process, and its polymerization comprises the Esterification Stage of polyester and the polycondensation phase of polyester.
The preparation method of a kind of isosorbide modified polyester fiber of the present invention:
1. the preparation of isosorbide modified polyester
(1) Esterification Stage of polyester
DMT (or PTA), ethylene glycol, isobide and esterification auxiliary agent are added the esterification polymeric kettle by a certain percentage, its mass percent is DMT or PTA 50~70%, ethylene glycol 10~49%, isobide 0~39%, esterification auxiliary agent 0.01~1%, wherein, the Esterification Stage heating-up temperature is 200~240 ℃, and be 60~120min heat time heating time;
(2) polycondensation phase of polyester
With esterification completely intermediate change the polycondensation polymeric kettle over to, add the polycondensation auxiliary agent by a certain percentage, the polycondensation auxiliary agent constitutes 0.01~1% by mass percentage, the polycondensation phase heating-up temperature is 270~290 ℃, be 45~90min heat time heating time, polycondensation phase vacuum is 0~70Pa, gets isosorbide modified polyester (synthetic terephthalic acid (TPA) ethylene glycol isobide polyester);
2. the preparation of isosorbide modified polyester fiber
Isosorbide modified polyester spinning on existing spinning equipment is got final product, and wherein spinning temperature is 240~290 ℃, and spinning speed is 3000~3500m/min.
Beneficial effect of the present invention:
Isosorbide modified polyester fiber of the present invention can utilize existing polymerization unit and spinning equipment polymerization and spinning, and the polyester of preparation has good toughness, rigidity and hot property, and fiber has good spinning property, and particularly dyeability improves a lot.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
1. raw material
DMT 194g, ethylene glycol 113g, isobide 10g, 1010 antioxidant 60mg, zinc acetate 60mg, antimonous oxide 65mg.
2. preparation method
1. the preparation of isosorbide modified polyester
(1) DMT, ethylene glycol, isobide, zinc acetate and 1010 antioxidant are added the esterification polymeric kettle, and it is added thermal agitation and vacuumizes, the Esterification Stage heating-up temperature of polyester is 200 ℃, and be 60min heat time heating time;
(2) the esterification rear center body is added the polycondensation polymeric kettle, antimonous oxide is added the polycondensation polymeric kettle again, and it is added thermal agitation and vacuumizes, the polycondensation phase heating-up temperature of polyester is 270 ℃, and be 90min heat time heating time, and polycondensation phase vacuum is 30Pa.
2. the preparation of isosorbide modified polyester fiber
(1) utilize synthetic isosorbide modified polyester to prepare a kind of isosorbide modified polyester fiber by existing spinning equipment;
(2) spinning temperature is 240 ℃ in the spinning process, and spinning speed is 3000m/min.
Embodiment 2
1. raw material
DMT 194g, ethylene glycol 101g, isobide 20g, 1010 antioxidant 60mg, zinc acetate 62mg, antimonous oxide 62mg.
2. preparation method
1. the preparation of isosorbide modified polyester
(1) DMT, ethylene glycol, isobide, zinc acetate and 1010 antioxidant are added the esterification polymeric kettle, and it is added thermal agitation and vacuumizes, the Esterification Stage heating-up temperature of polyester is 210 ℃, and be 80min heat time heating time;
(2) the esterification rear center body is added the polycondensation polymeric kettle, antimonous oxide is added the polycondensation polymeric kettle again, and it is added thermal agitation and vacuumizes, the polycondensation phase heating-up temperature of polyester is 280 ℃, and be 45min heat time heating time; Polycondensation phase vacuum is 45Pa.
2. the preparation of isosorbide modified polyester fiber
(1) utilize synthetic isosorbide modified polyester to prepare a kind of isosorbide modified polyester fiber by existing spinning equipment;
(2) spinning temperature is 260 ℃ in the spinning process, and spinning speed is 3200m/min.
Embodiment 3
1. raw material
DMT 194g, ethylene glycol 113g, isobide 10g, 1010 antioxidant 60mg, zinc acetate 60mg, antimonous oxide 65mg.
2. preparation method
1. the preparation of isosorbide modified polyester
(1) DMT, ethylene glycol, isobide, zinc acetate and 1010 antioxidant are added the esterification polymeric kettle, and it is added thermal agitation and vacuumizes, the Esterification Stage heating-up temperature is 220 ℃, and be 100min heat time heating time;
(2) the esterification rear center body is added the polycondensation polymeric kettle, antimonous oxide is added the polycondensation polymeric kettle again, and it is added thermal agitation and vacuumizes, the polycondensation phase heating-up temperature is 280 ℃, and be 60min heat time heating time, and polycondensation phase vacuum is 60Pa.
2. the preparation of isosorbide modified polyester fiber
(1) utilize synthetic isosorbide modified polyester to prepare a kind of isosorbide modified polyester fiber by existing spinning equipment;
(2) spinning temperature is 280 ℃ in the spinning process, and spinning speed is 3500m/min.
Embodiment 4
1. raw material
DMT 194g, ethylene glycol 64g, isobide 58g, 1010 antioxidant 63mg, zinc acetate 61mg, antimonous oxide 61mg.
2. preparation method
1. the preparation of isosorbide modified polyester
(1) DMT, ethylene glycol, isobide, zinc acetate and 1010 antioxidant are added the esterification polymeric kettle, and it is added thermal agitation and vacuumizes, the Esterification Stage heating-up temperature is 240 ℃, and be 120min heat time heating time;
(2) the esterification rear center body is added the polycondensation polymeric kettle, antimonous oxide is added the polycondensation polymeric kettle again, and it is added thermal agitation and vacuumizes, the polycondensation phase heating-up temperature is 280 ℃, and be 80min heat time heating time, and polycondensation phase vacuum is 30Pa.
2. the preparation of isosorbide modified polyester fiber
(1) utilize synthetic isosorbide modified polyester to prepare a kind of isosorbide modified polyester fiber by existing spinning equipment;
(2) spinning temperature is 290 ℃ in the spinning process, and spinning speed is 3500m/min.
Claims (8)
1. isosorbide modified polyester fiber, it is characterized in that: this fiber is to be that raw material is made through spinning with dimethyl terephthalate (DMT) DMT or p-phthalic acid PTA, ethylene glycol, isobide and auxiliary agent, and it constitutes DMT or PTA 50~70%, ethylene glycol 10~49%, isobide 0~39%, auxiliary agent 0.01~1% by mass percentage.
2. isosorbide modified polyester fiber according to claim 1 is characterized in that: described auxiliary agent is one or more of antioxidant, esterification catalyst or polycondensation catalyst.
3. isosorbide modified polyester fiber according to claim 2 is characterized in that: described antioxidant is four [methyl-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester.
4. isosorbide modified polyester fiber according to claim 2 is characterized in that: described esterification catalyst is zinc acetate, manganese acetate, cobalt acetate or lead acetate.
5. isosorbide modified polyester fiber according to claim 2 is characterized in that: described polycondensation catalyst is antimony oxide, titanium oxide, cobalt oxide or chromium oxide.
6. the preparation method of an isosorbide modified polyester fiber comprises step:
1. the preparation of isosorbide modified polyester
(1) Esterification Stage of polyester
DMT or PTA, ethylene glycol, isobide and esterification auxiliary agent are added the reaction of esterification polymeric kettle by a certain percentage, and its mass percent is DMT or PTA 50~70%, ethylene glycol 10~49%, isobide 0~39%, esterification auxiliary agent 0.01~1%;
(2) polycondensation phase of polyester
With esterification completely intermediate change the polycondensation polymeric kettle over to, add the polycondensation auxiliary agent by a certain percentage, the polycondensation auxiliary agent constitutes 0.01~1% by mass percentage, the reaction, isosorbide modified polyester;
2. the preparation of isosorbide modified polyester fiber
Isosorbide modified polyester spinning on existing spinning equipment is got final product.
7. the preparation method of isosorbide modified polyester fiber according to claim 6, it is characterized in that: described Esterification Stage heating-up temperature is 200~240 ℃, be 60~120min heat time heating time; The polycondensation phase heating-up temperature is 270~290 ℃, and be 45~90min heat time heating time, and polycondensation phase vacuum is 0~70Pa.
8. the preparation method of isosorbide modified polyester fiber according to claim 6, it is characterized in that: described spinning temperature is 240~290 ℃, spinning speed is 3000~3500m/min.
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Cited By (7)
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CN102250330A (en) * | 2011-05-05 | 2011-11-23 | 常州大学 | Highly transparent copolyester synthesized by biomass-resource-derived monomers and preparation method for highly transparent copolyester |
CN103014906A (en) * | 2012-11-16 | 2013-04-03 | 东华大学 | Preparation method of inflaming retarding hydrophilic polyester fiber |
CN103044671A (en) * | 2012-12-19 | 2013-04-17 | 中国纺织科学研究院 | Preparation method for bis-anhydro sugar alcohol contained copolyester |
CN103820879A (en) * | 2012-11-16 | 2014-05-28 | 东华大学 | Hydrophilic polyester fiber containing coffee carbon and preparation method of hydrophilic polyester fiber |
CN103820878A (en) * | 2012-11-16 | 2014-05-28 | 东华大学 | Preparation method for multi-functional hydrophilic polyester fibers |
CN111206300A (en) * | 2018-11-22 | 2020-05-29 | 厦门翔鹭化纤股份有限公司 | Elastic composite fiber and preparation method thereof |
FR3104179A1 (en) * | 2019-12-10 | 2021-06-11 | Roquette Freres | Colored synthetic fiber |
-
2008
- 2008-01-15 CN CNA2008100326462A patent/CN101215728A/en active Pending
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102250330B (en) * | 2011-05-05 | 2013-03-13 | 常州大学 | Highly transparent copolyester synthesized by biomass-resource-derived monomers and preparation method for highly transparent copolyester |
CN102250330A (en) * | 2011-05-05 | 2011-11-23 | 常州大学 | Highly transparent copolyester synthesized by biomass-resource-derived monomers and preparation method for highly transparent copolyester |
CN103820879B (en) * | 2012-11-16 | 2015-10-28 | 东华大学 | A kind of hydrophilic polyesters fiber containing coffee carbon and preparation method thereof |
CN103014906A (en) * | 2012-11-16 | 2013-04-03 | 东华大学 | Preparation method of inflaming retarding hydrophilic polyester fiber |
CN103820879A (en) * | 2012-11-16 | 2014-05-28 | 东华大学 | Hydrophilic polyester fiber containing coffee carbon and preparation method of hydrophilic polyester fiber |
CN103820878A (en) * | 2012-11-16 | 2014-05-28 | 东华大学 | Preparation method for multi-functional hydrophilic polyester fibers |
CN103820878B (en) * | 2012-11-16 | 2015-10-28 | 东华大学 | A kind of preparation method of multifunctional hydrophilic polyester fiber |
CN103014906B (en) * | 2012-11-16 | 2014-10-15 | 东华大学 | Preparation method of inflaming retarding hydrophilic polyester fiber |
CN103044671A (en) * | 2012-12-19 | 2013-04-17 | 中国纺织科学研究院 | Preparation method for bis-anhydro sugar alcohol contained copolyester |
CN103044671B (en) * | 2012-12-19 | 2014-10-08 | 中国纺织科学研究院 | Preparation method for bis-anhydro sugar alcohol contained copolyester |
CN111206300A (en) * | 2018-11-22 | 2020-05-29 | 厦门翔鹭化纤股份有限公司 | Elastic composite fiber and preparation method thereof |
FR3104179A1 (en) * | 2019-12-10 | 2021-06-11 | Roquette Freres | Colored synthetic fiber |
WO2021116614A1 (en) * | 2019-12-10 | 2021-06-17 | Roquette Freres | Colored synthetic fiber |
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