CN103993378B - A kind of preparation method of lignin modification pet fiber - Google Patents
A kind of preparation method of lignin modification pet fiber Download PDFInfo
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- CN103993378B CN103993378B CN201410239165.4A CN201410239165A CN103993378B CN 103993378 B CN103993378 B CN 103993378B CN 201410239165 A CN201410239165 A CN 201410239165A CN 103993378 B CN103993378 B CN 103993378B
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Abstract
The present invention relates to the preparation method of a kind of lignin modification pet fiber, including: after lignin is dried with polyethylene terephtalate, stirring and evenly mixing, melt blending, obtain nascent pellet；Wherein lignin and the mass ratio 5:95 20:80 of PET；Above-mentioned nascent pellet carries out melt spinning, thermal finalization, and winding obtains lignin modified PET (Polyethylene Terephthalate) as-spun fibre, then carries out dry method drawing-off, and winding to obtain final product.Present invention process is simple, and low cost can industrially be promoted, have a good application prospect.
Description
Technical field
The invention belongs to physical blending pet fiber method of modifying field, change particularly to a kind of lignin
The preparation method of property pet fiber.
Background technology
Polyethylene terephthalate is one of currently the most important ones synthetic material, have good thermostability, resistance to chemical reagents,
Mechanical property and electric property, the most transparent good, insulating properties is good, relatively low production cost and the higher ratio of performance to price.
It is mainly used in fiber, biaxially oriented film and polyester bottles, various packing containers etc.；Full-bodied PET also engineering plastics bearing,
It is used widely in the field such as gear, electric parts；In sedan-chair auto plastics, proportion is also continuously increased.PET engineering plastics
Have cheap, thermostability is high, mechanical strength good, water absorption rate is little, excellent electrical properties, resistance to various chemical drugss, molding
The advantages such as product good stability of the dimension, research and the application of carrying out PET engineering plastics have good development prospect.PET is a kind of
Semicrystalline polymeric, has crystallization and non-crystalline areas.Owing to its crystalline rate is relatively slow and vitrification point (Tg) is higher, note
Needing higher mold temperature (more than 100 DEG C) when moulding, molding cycle is oversize, causes certain energy loss, processing cost liter
High.People generally add crystallization nucleating agent in PET and improve the crystalline rate of PET, add crystallization promoter and reduce vitrification
Temperature, shortens molding cycle, reduces mold temperature, beneficially processing and forming.
In recent years, the research improving PET crystalline rate is got more and more by Chinese scholars, wherein by the method for physical blending more
More receive publicity.High polymer blending modification method is simple and easy to do, has the biggest advantage technically and economically, and it not only remains original
The advantage of high polymer, owing to the addition of new material, imparts, by changing aggregated structure, the performance that high polymer is new, has certain
Theoretical and practical values.
Summary of the invention
The technical problem to be solved is to provide the preparation side of a kind of lignin modification pet fiber
Method, this invented technology is simple, and operational approach is simple, and low cost has a good application prospect.
A kind of preparation method of the lignin modification pet fiber of the present invention, including:
(1) after lignin being dried with polyethylene terephtalate, stirring and evenly mixing, melt blending, obtain nascent pellet；
Wherein lignin and the mass ratio 5:95-20:80 of PET；
(2) above-mentioned nascent pellet carrying out melt spinning, thermal finalization, winding obtains lignin modified PET (Polyethylene Terephthalate) as-spun fibre, then enters
Row dry method drawing-off, winding, obtain lignin modification pet fiber.
In described step (1), lignin is that alkali lignin, sulfate-reducing conditions, kraft lignin, acetic acid lignin, enzymolysis are wooden
One in element.
Described step (1) is dried under the conditions of vacuum 50-90 DEG C, dry 24-36h.
In described step (1), melt blending temperature is 150-300 DEG C.
In described step (2), melt spinning is: nascent pellet, in the feed hopper of melt spinning machine, melts at 170-300 DEG C, at meter
Flowed out at spinneret orifice by filament spinning component under amount pump pressure.
Described dosing pump pressure is 20-100MPa, it is ensured that melt flows to filament spinning component and spinneret orifice.
In described step (2), thermal finalization is to carry out thermal finalization under warm air blowoff, and wherein hot air temperature is 20-90 DEG C.
In described step (2), the drawing-off atmosphere of dry method drawing-off is air, and drafting multiple is 2-10 times.
In described step (2), the degree of orientation of lignin modification pet fiber is 60%-98%, and degree of crystallinity is
55%-75%.
In described step (2), lignin modification pet fiber cross section is circular.
In the present invention, the addition of lignin makes the intermolecular force of polyethylene terephthalate change, and changes poly-to benzene two
The microstructure of formic acid glycol ester strand, lignin contains more active group simultaneously, can be with poly terephthalic acid second
Diol ester molecule forms hydrogen bond and has the fine compatibility, it is possible to is formed on polyethylene terephthalate matrix and preferably divides
Dissipate so that the degree of orientation and the crystallization rate of polyethylene terephthalate are improved.
Beneficial effect
(1) present invention process is simple, and operational approach is simple, and low cost can industrially be promoted, before having good application
Scape；
(2) present invention uses low-melting point PET, is the crystallization rate that nucleator changes PET by adding the lignin of biomass,
Shorten crystallization time, improve degree of crystallinity simultaneously.
Accompanying drawing explanation
Fig. 1 is the section SEM figure of lignin/PET mass ratio blend and m eltspinning fiber when being 10:90；
Fig. 2 be lignin/PET mass ratio when being 10:90 the local section of blend and m eltspinning fiber amplify SEM figure；
The DSC spectrogram of blend and m eltspinning fiber when Fig. 3 is pure PET and lignin/PET mass ratio is 15:85；
Blend and m eltspinning fiber infrared spectrum when Fig. 4 is pure PET, lignin and lignin/PET mass ratio are 15:85.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and not
For limiting the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art can
To make various changes or modifications the present invention, these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
To fully be dried the lignin powder after (baking temperature is 50 DEG C, and drying time is 36h) and PET 5:95 in mass ratio
Mix homogeneously in homogenizer, carries out mixed material melt blending in miniature blended instrument at a temperature of 180 DEG C, obtains
Nascent pellet；Above-mentioned nascent pellet is joined in the feed hopper of melt spinning machine and melt at 200 DEG C, at dosing pump pressure 20MPa
Under flowed out by spinneret orifice, thermal finalization under warm air blowoff (hot air temperature is 20 DEG C), by winder winding around obtaining wood
Polyethylene terephthalate as-spun fibre after quality blending and modifying；As-spun fibre carries out on dry method drafting machine dry method lead
Stretching, winding obtains the pet fiber that drafting multiple is at 5 times, finally winds to have stronger mechanical property
Pet fiber, wherein the degree of orientation of fiber is 65.4%, and degree of crystallinity is 31.3%.
Embodiment 2
By lignin powder and the PET 5:95 in mass ratio of fully dried (baking temperature is 70 DEG C, and drying time is 28h)
Mix homogeneously in homogenizer, carries out mixed material melt blending in miniature blended instrument at a temperature of 180 DEG C, obtains
Nascent pellet；Above-mentioned nascent pellet is joined in the feed hopper of melt spinning machine and melt at 200 DEG C, at dosing pump pressure 20MPa
Under flowed out by spinneret orifice, thermal finalization under warm air blowoff (hot air temperature is 50 DEG C), by winder winding around obtaining wood
Polyethylene terephthalate as-spun fibre after quality blending and modifying；As-spun fibre carries out on dry method drafting machine dry method lead
Stretching, winding obtains the pet fiber that drafting multiple is at 10 times, finally winds to have stronger mechanical property
Pet fiber, wherein the degree of orientation of fiber is 72.1%, and degree of crystallinity is 37.2%.
Embodiment 3
To fully be dried the lignin powder after (baking temperature is 90 DEG C, and drying time is 24h) and PET 10:90 in mass ratio
Mix homogeneously in homogenizer, carries out mixed material melt blending in miniature blended instrument at a temperature of 180 DEG C, obtains
Nascent pellet；Above-mentioned nascent pellet is joined in the feed hopper of melt spinning machine and melt at 200 DEG C, at dosing pump pressure 100MPa
Under flowed out by spinneret orifice, thermal finalization under warm air blowoff (hot air temperature is 90 DEG C), by winder winding around obtaining wood
Polyethylene terephthalate as-spun fibre after quality blending and modifying；As-spun fibre carries out on dry method drafting machine dry method lead
Stretching, winding obtains the pet fiber that drafting multiple is at 5 times, finally winds to have stronger mechanical property
Pet fiber, wherein the degree of orientation of fiber is 75.8%, and degree of crystallinity is 32.5%.
Embodiment 4
To fully be dried the lignin powder after (baking temperature is 70 DEG C, and drying time is 28h) and PET 10:90 in mass ratio
Mix homogeneously in homogenizer, carries out mixed material melt blending in miniature blended instrument at a temperature of 200 DEG C, obtains
Nascent pellet；Above-mentioned nascent pellet is joined in the feed hopper of melt spinning machine and melt at 230 DEG C, at dosing pump pressure 100
Flowed out by spinneret orifice under MPa, thermal finalization under warm air blowoff (hot air temperature is 50 DEG C), by winder winding around obtaining
Polyethylene terephthalate as-spun fibre after lignin blending and modifying；As-spun fibre is done on dry method drafting machine
Method drawing-off, winding obtains the pet fiber that drafting multiple is at 10 times, finally winds to have relatively strength and learns
The pet fiber of performance, wherein the degree of orientation of fiber is 87.6%, and degree of crystallinity is 39.3%.
Embodiment 5
To fully be dried the lignin powder after (baking temperature is 70 DEG C, and drying time is 28h) and PET 20:80 in mass ratio
Mix homogeneously in homogenizer, carries out mixed material melt blending in miniature blended instrument at a temperature of 230 DEG C, obtains
Nascent pellet；Above-mentioned nascent pellet is joined in the feed hopper of melt spinning machine and melt at 250 DEG C, at dosing pump pressure 50MPa
Under flowed out by spinneret orifice, thermal finalization under warm air blowoff (hot air temperature is 50 DEG C), by winder winding around obtaining wood
Polyethylene terephthalate as-spun fibre after quality blending and modifying；As-spun fibre carries out on dry method drafting machine dry method lead
Stretching, winding obtains the pet fiber that drafting multiple is at 10 times, finally winds to have stronger mechanical property
Pet fiber, wherein the degree of orientation of fiber is 91.6%, degree of crystallinity 51.2%.
Embodiment 6
To fully be dried the lignin powder after (baking temperature is 70 DEG C, and drying time is 28h) and PET 20:80 in mass ratio
Mix homogeneously in homogenizer, carries out mixed material melt blending in miniature blended instrument at a temperature of 230 DEG C, obtains
Nascent pellet；Above-mentioned nascent pellet is joined in the feed hopper of melt spinning machine and melt at 250 DEG C, at dosing pump pressure 50MPa
Under flowed out by spinneret orifice, thermal finalization under warm air blowoff (hot air temperature is 50 DEG C), by winder winding around obtaining wood
Polyethylene terephthalate as-spun fibre after quality blending and modifying；As-spun fibre carries out on dry method drafting machine dry method lead
Stretching, winding obtains the pet fiber that drafting multiple is at 10 times, finally winds to have stronger mechanical property
Pet fiber, wherein the degree of orientation of fiber is 92.3%, degree of crystallinity 55.2%.
Claims (6)
1. a preparation method for lignin modification pet fiber, including:
(1) after lignin being dried with polyethylene terephtalate, stirring and evenly mixing, melt blending, obtain nascent pellet；
Wherein lignin and the mass ratio 5:95-20:80 of PET；Wherein dry as under the conditions of vacuum 50-90 DEG C, dry
24-36h；Lignin is that alkali lignin, sulfate-reducing conditions, kraft lignin, acetic acid lignin, enzymolysis are wooden
One in element；
(2) above-mentioned nascent pellet carrying out melt spinning, thermal finalization, winding obtains lignin modified PET (Polyethylene Terephthalate) as-spun fibre, then enters
Row dry method drawing-off, winding, obtain lignin modification pet fiber；Wherein lignin modification gathers
The degree of orientation of ethylene glycol terephthalate fiber is 60%-98%, and degree of crystallinity is 55%-55.2%, and fibre section is circle
Shape.
The preparation method of a kind of lignin modification pet fiber the most according to claim 1, its feature exists
In: in described step (1), melt blending temperature is 150-300 DEG C.
The preparation method of a kind of lignin modification pet fiber the most according to claim 1, its feature exists
In: in described step (2), melt spinning is: nascent pellet, in the feed hopper of melt spinning machine, melts at 170-300 DEG C,
Flowed out at spinneret orifice by filament spinning component under dosing pump pressure.
The preparation method of a kind of lignin modification pet fiber the most according to claim 3, its feature exists
In: described dosing pump pressure is 20-100MPa.
The preparation method of a kind of lignin modification pet fiber the most according to claim 1, its feature exists
In: in described step (2), thermal finalization is to carry out thermal finalization under warm air blowoff, and wherein hot air temperature is 20-90 DEG C.
The preparation method of a kind of lignin modification pet fiber the most according to claim 1, its feature exists
In: in described step (2), the drawing-off atmosphere of dry method drawing-off is air, and drafting multiple is 2-10 times.
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| CN107869004B (en) * | 2017-11-30 | 2019-12-31 | 湖州科博信息科技有限公司 | Antibacterial and hygroscopic sock fabric |
| CN108677324B (en) * | 2018-05-15 | 2020-10-16 | 福建省锋源盛纺织科技有限公司 | Tensile flame-retardant composite mesh fabric and preparation method thereof |
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| CN101078137A (en) * | 2007-06-29 | 2007-11-28 | 东华大学 | Lignin-base nano carbon fibre and preparation method thereof |
| CN101525472A (en) * | 2008-03-04 | 2009-09-09 | 东丽纤维研究所（中国）有限公司 | Alkali soluble polyester and method for preparing same |
| CN102597105A (en) * | 2009-11-05 | 2012-07-18 | 诺瓦蒙特股份公司 | Mixtures of biodegradable polyesters with at least one polymer of natural origin |
| CN103774276A (en) * | 2014-01-13 | 2014-05-07 | 东华大学 | Method for preparing lignin/polyacrylonitrile blended melt-spun fiber by adopting physical blending |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2008106631A1 (en) * | 2007-03-01 | 2008-09-04 | Prs Mediterranean Ltd. | Process for producing compatibilized polymer blends |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101078137A (en) * | 2007-06-29 | 2007-11-28 | 东华大学 | Lignin-base nano carbon fibre and preparation method thereof |
| CN101525472A (en) * | 2008-03-04 | 2009-09-09 | 东丽纤维研究所（中国）有限公司 | Alkali soluble polyester and method for preparing same |
| CN102597105A (en) * | 2009-11-05 | 2012-07-18 | 诺瓦蒙特股份公司 | Mixtures of biodegradable polyesters with at least one polymer of natural origin |
| CN103774276A (en) * | 2014-01-13 | 2014-05-07 | 东华大学 | Method for preparing lignin/polyacrylonitrile blended melt-spun fiber by adopting physical blending |
Non-Patent Citations (2)
| Title |
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| Supermolecular structure and thermal properties of poly(ethylene terephthalate)/lignin composites;Maurizio Canetti等;《Composites Science and Technology》;20070510;第67卷;第3151-3157页 * |
| 木质素碳纤维的制备与结构和性能研究;许园;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20071115(第5期);B016-223页 * |
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Effective date of registration: 20191219 Address after: 314100 floor 3 and 4, workshop 3, No.9 Dongsheng Road, Huimin street, Jiashan County, Jiaxing City, Zhejiang Province Patentee after: Youju new material (Zhejiang) Co.,Ltd. Address before: 201620 No. 2999 Renmin Road North, Songjiang new town, Shanghai, Songjiang District Patentee before: Donghua University |
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Effective date of registration: 20230719 Address after: No. 19, Wutong East Road, the Taihu Lake Youth Science and Technology Pioneer Park, South Wutong Village, Meishan Town, Changxing County, Huzhou, Zhejiang Province 313000 Patentee after: Zhejiang Nova New Materials Co.,Ltd. Address before: 314100 Floor 3 and 4, Workshop 3, No. 9, Dongsheng Road, Huimin Street, Jiashan County, Jiaxing, Zhejiang Province Patentee before: Youju new material (Zhejiang) Co.,Ltd. |