CN106757772B - The preparation method of the three-dimensional porous unordered holder of fiber heat bonding solidification is spun in a kind of polylactic acid melting - Google Patents
The preparation method of the three-dimensional porous unordered holder of fiber heat bonding solidification is spun in a kind of polylactic acid melting Download PDFInfo
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- CN106757772B CN106757772B CN201611039705.XA CN201611039705A CN106757772B CN 106757772 B CN106757772 B CN 106757772B CN 201611039705 A CN201611039705 A CN 201611039705A CN 106757772 B CN106757772 B CN 106757772B
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- unordered
- spun
- polylactic acid
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Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4326—Condensation or reaction polymers
- D04H1/435—Polyesters
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D13/00—Complete machines for producing artificial threads
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/542—Adhesive fibres
- D04H1/55—Polyesters
Abstract
The preparation method that fiber heat bonding cures three-dimensional porous unordered holder is spun in polylactic acid melting disclosed by the invention, and steps are as follows：By the polylactic acid slice with good biodegradability properties and biocompatibility, using single-screw extruder, three-dimensional porous unordered holder is obtained using itself heat bonding by melt-blown process.PLA meltings prepared by the method for the present invention are spun the porous unordered supporting structure of fibre three-dimensional and are stablized, and have preferable internal pore structure, physical property and mechanical property.The unordered holder can be applied in bio-medical fields such as bone tissue engineers, have preferable application potential and foreground.
Description
The application is divisional application, original application day：2015.1.27 application number：201510040458.4
Invention and created name：The preparation method that fiber heat bonding cures three-dimensional porous unordered holder is spun in polylactic acid melting
Technical field
The present invention relates to polylactic acid to melt the preparation method spun fiber heat bonding and cure three-dimensional porous unordered holder.
Background technology
North Carolina State University's Nonwovens Research Consortium Fedorova et al. [Fedorova N,
Pourdeyhimi B:High strength nylon micro-and nanofiber based nonwovens via
spunbonding.J Appl Polym Sci 2007,104(5):3434-3442.] utilize polyamide fibre 6 (N6) and PLA
(Natureworks) different sea-island fibre (polyamide fibre 6 is island, and PLA is sea), the water that then web passes through 30m/min are prepared
Thorn is reinforced into fabric.The NaOH solution that fabric is utilized to 3% again handles 10min at 100 DEG C and gets rid of PLA ingredients.By dissolving away
After PLA components, micron and nanofiber can be obtained, and fibre diameter can reach 0.36-1.3mm.
It is melted about PLA and spins fiber, also Polypropylene/Poly (lactic acid) (PP/PLA) two-component is fine
Tie up [Arvidson SA, Roskov KE, Pate JJ, Spontak RJ, Khan SA, Gorga RE:Modification of
Melt-Spun Isotactic Polypropylene and Poly(lactic acid)Bicomponent Filaments
with a Premade Block Copolymer.Macromolecules 2012,45(2):913-925.；Liu Y,Tovia
F,Pierce JD:Consumer Acceptability of Scent-infused Knitting Scarves Using
Functional Melt-spun PP/PLA Bicomponent Fibers.Text Res J 2009,79(6):566-
573.]、poly(lactic acid)/hydroxyapatite(PLA/HA)[Persson M,Lorite GS,Cho SW,
Tuukkanen J,Skrifvars M:Melt Spinning of Poly(lactic acid)and Hydroxyapatite
Composite Fibers:Influence of the Filler Content on the Fiber Properties.Acs
Appl Mater Inter 2013,5(15):6864-6872.]、poly(lactic acid)/Poly(R)-3-
hydroxybutyrate-co-R-3-hydroxyvalerate(PLA/PHBV)[Pivsa-Art S,Srisawat N,O-
Charoen N,Pavasupree S,Pivsa-Art W:Preparation of Knitting Socks from Poly
(lactic acid)and Poly[(R)-3-hydroxybutyrate-co-(R)-3-hydroxyvalerate](PHBV)
blends for Textile Industrials.Enrgy Proced 2011,9.]、poly(lactic acid)/
polyvinylidene fluoride(PLA/PVDF)[Fryczkowski R,Fryczkowska B,Binias W,
Janicki J:Morphology of fibrous composites of PLA and PVDF.Compos Sci Technol
2013,89:186-193.]、Polylactide/Multiwall Carbon Nanotube(PLA/MWNT)[Rizvi R,
Tong L,Naguib H:Processing and Properties of Melt Spun Polylactide-Multiwall
Carbon Nanotube Fiber Composites.J Polym Sci Pol Phys 2014,52(6):477-484.]、
Polylactide/poly(vinyl alcohol)(PLA/PVA)[Tran NHA,Brunig H,Hinuber C,Heinrich
G:Melt Spinning of Biodegradable Nanofibrillary Structures from Poly(lactic
acid)and Poly(vinyl alcohol)Blends.Macromol Mater Eng 2014,299(2):219-227.]、
Polylactide/poly(butylene succinate)(PLA/PBS)[Jompang L,Thumsorn S,On JW,
Surin P,Apawet C,Chaichalermwong T,Kaabbuathong N,O-Charoen N,Srisawat N:Poly
(lactic acid)and Poly(butylene succinate)Blend Fibers Prepared by Melt
Spinning Technique.10th Eco-Energy and Materials Science and Engineering
Symposium 2013,34:493-499.]。
In addition, also there is researcher that PLA is processed into fabric (woven fabric, knitted fabric, three-dimensional orthogonal fabric), non-woven cloth
(melt-blow nonwoven, spun-bonded non-woven, needle fabric, thermal non-woven fabric and electrostatic spinning nano fiber are non-woven
Cloth), composite material, the forms such as film.
Dai et al.[Dai XJJ,du Plessis J,Kyratzis IL,Maurdev G,Huson MG,Coombs
C:Controlled Amine Functionalization and Hydrophilicity of a Poly(lactic
acid)Fabric.Plasma Process Polym 2009,6(8):490-497.] by PLA melt spin fiber be prepared into knitting
Then object carries out corona treatment.Bae et al.[Bae GY,Jang J,Jeong YG,Lyoo WS,Min BG:
Superhydrophobic PLA fabrics prepared by UV photo-grafting of hydrophobic
silica particles possessing vinyl groups.J Colloid Interf Sci 2010,344(2):
584-587.] silicon dioxide granule using ultraviolet irradiation technology in PLA fabric surface grafted hydrophobics prepares superhydrophobic fabric.
Nodo et al.[Nodo K,Leong YW,Hamada H:Effect of knitted and woven textile
structures on the mechanical performance of poly(lactic acid)textile insert
injection-compression moldings.J Appl Polym Sci 2012,125:E200-E207. PLA machines] are studied
The load performance of fabric and knitted fabric impact test, the results showed that have by PLA fabrics prepared by compression forming preferable tough
Property and extensibility.In addition, also PLA three-dimensional orthogonals fabric [Zhou NT, Geng XY, Ye MQ, Yao L, Shan ZD, Qiu
YP:Mechanical and sound adsorption properties of cellular poly(lactic acid)
matrix composites reinforced with 3D ramie fabrics woven with co-wrapped
yarns.Ind Crop Prod 2014,56:1-8.]。
Melt blown technology is that thermoplastic polymer is prepared into not weaving fabric of superfine fiber by high-speed flow, this non-woven
Cloth has smaller aperture and larger porosity.Liu et al.[Liu Y,Cheng BW,Cheng GX:Development
and Filtration Performance of Polylactic Acid Meltblowns.Text Res J 2010,80
(9):771-779.] PLA of U.S. Natureworks is sliced (Tg=52 DEG C, Tm=168 DEG C) it is squeezed successively by dry, melting
Go out, filter, metering gear, spinning, hot-air stretch, cooling and winding receipt prepares PLA melt-blow nonwovens.Wherein receive
Distance is 20cm, and heat air pressure 0.15MPa, spinning temperature is 220 DEG C, hot air temperature is respectively 250,260,270,
280,290 and 300 DEG C, slit width is respectively 0.3,0.4,0.5 and 0.6cm.And hot air temperature (250- is had studied respectively
290 DEG C) and slit width (0.3-0.6cm) variation to the fibre diameter of PLA melt-blow nonwovens, porosity, average pore size,
The filter efficiency of 0.3 μm and 0.5 μm particle and influence and the changing rule of Air permenbility.Majchrzycka[Majchrzycka
K:Evaluation of a New Bioactive Nonwoven Fabric for Respiratory
Protection.Fibres Text East Eur 2014,22(1):81-88.] utilize the PLA slices (T of Natureworksm
=160-170 DEG C), 270 DEG C of spinning temperature, 270 DEG C of hot air temperature, 8.8m3The air velocity of/h, the reception of 300mm
Distance prepares PLA melt-blow nonwovens, and is modified using biological active matter confrontation PLA melt-blow nonwovens, grinds simultaneously
Study carefully the filter efficiency of viability and aerosol of the bacterium on the bioactivity non-woven cloth.Cerkez et al.[Cerkez
I,Worley SD,Broughton RM,Huang TS:Rechargeable antimicrobial coatings for
poly(lactic acid)nonwoven fabrics.Polymer 2013,54(2):536-541.] spin University of Tennessee
PLA melt-blow nonwovens (the 30g/m that fabric and non-woven cloth centre of development provide2) utilize heterocyclic N-halamine for the equal of amine acetate
Polymers (1.5wt%, 40 DEG C, 10min) carries out coating.The experimental results showed that coating is highly stable, and with efficiently to gold
The antibiotic property of staphylococcus aureus and Escherichia coli.This coating bracket can be used in antibacterial food packaging, filter and health
In terms of product.Krucinska et al.[Krucinska I,Surma B,Chrzanowski M,Skrzetuska E,
Puchalski M:Application of melt-blown technology in the manufacturing of a
solvent vapor-sensitive,non-woven fabric composed of poly(lactic acid)loaded
with multi-walled carbon nanotubes.Text Res J 2013,83(8):859-870.] be prepared for for the first time
98%PLA/2% multiple-wall carbon nanotubes (MWCNTs) melt-blow nonwoven.
Puchalski et al.[Puchalski M,Krucinska I,Sulak K,Chrzanowski M,
Wrzosek H:Influence of the calender temperature on the crystallization
behaviors of polylactide spun-bonded non-woven fabrics.Text Res J 2013,83
(17):1775-1785.] by the PLA of U.S. Natureworks slice 6251D (Mn=45800g/mol, Tg=61 DEG C, Tm=
168 DEG C), in 80 DEG C of dry 4h, spinning temperature is 205-216 DEG C, and the output of polymer is 0.10-0.43g/min/Hole,
A total of 467 hole of spinneret, hot pressing temperature are 60-130 DEG C.And have studied PLA spun-bonded non-wovens under different hot pressing temperatures
External morphology, crystallinity, physical-mechanical properties and thermal degradation performance.Gutowska et al.[Gutowska A,
Jozwicka J,Sobczak S,Tomaszewski W,Sulak K,Miros P,Owczarek M,Szalczynska M,
Ciechanska D,Krucinska I:In-Compost Biodegradation of PLA Nonwovens.Fibres
Text East Eur 2014,22(5):99-106.] utilize the PLA slices (T of Natureworksm=160-170 DEG C), 212
± 1 DEG C of spinning temperature, the work beam of 2.9-6.8m/min rotating speeds, the extrusion amount of 42.4-101.8g/min, 60-105 DEG C
Bonding temperature and 1500-2000Pa pressure prepare PLA spun-bonded non-wovens and study its 58 ± 2 DEG C, pH=7 and
Degradation property in 52.6% humidity environment.Wang et al.[Wang HB,Wei QF,Wang X,Gao WD,Zhao XY:
Antibacterial properties of PLA nonwoven medical dressings coated with
nanostructured silver.Fiber Polym 2008,9(5):556-560.] it is furnished with first by Jiangxi state bridge is non-woven
PLA spun-bonded non-wovens (the 35g/m that limit company provides2) be immersed in acetone soln, then ultrasonic irrigation removal in 30 minutes has
Solvent, then cleaned twice with plasma water, it is dry in 30-35 DEG C of baking oven.Recycle the magnetron sputtering of argon plasma
Membranous system is silver-plated on it, obtains the PLA spun-bonded non-wovens of nanometer silver coating, and studies nano coating thickness to non-woven
The influence of cloth anti-microbial property.The experimental results showed that when coating layer thickness is in 1nm, to staphylococcus aureus and Escherichia coli
Antibacterial effect can reach 100%.
Yilmaz et al.[Yilmaz ND,Banks-Lee P,Powell NB,Michielsen S:Effects of
Porosity,Fiber Size,and Layering Sequence on Sound Absorption Performance of
Needle-Punched Nonwovens.J Appl Polym Sci 2011,121(5):3056-3069.] by U.S. Johnson
The PLA fibers of fiber innovative technology pass through Truetzschler fiber openings, air-laid and pinprick reinforcement process and prepare successively
MULTILAYER COMPOSITE PLA needle fabrics, and study its thickness, weight, porosity and gas-flow resistance.Pelto et al.
[Tingaut P,Zimmermann T,Lopez-Suevos F:Synthesis and Characterization of
Bionanocomposites with Tunable Properties from Poly(lactic acid)and
Acetylated Microfibrillated Cellulose.Biomacromolecules 2010,11(2):454-464.]
PLA needle fabrics are prepared using pinprick reinforcement after the PLA meltings of 10-20mm are spun monofilament cut-out, combed, are then reused
Chondroitin sulfate and conductive poly- pyrrole (polypyrrole, PPy), which are coughed up, coating modified prepares skeletonization holder.The experimental results showed that with
The PLA needle fabrics of non-coating are compared, and it is dry that the conducting bracket after coating can improve body fat under electro photoluminescence effect
The proliferation of cell and the differentiation of skeletonization.And the conducting bracket after coating is hydrolyzing electric conductivity when starting than more significant, but
Hatching is begun to decline after a week.The conducting bracket of this coating can be applied in bone tissue engineer.
Bhat et al.[Bhat GS,Gulgunje P,Desai K:Development of structure and
properties during thermal calendering of polylactic acid(PLA)fiber
webs.Express Polym Lett 2008,2(1):49-56.] by PLA staple fibers, (fibre length 76mm, fineness are
It is 35g/m that weight is formed after 3denier) SDS Atlas carding machines being utilized to comb2Web, web size be 120cm ×
30cm, then to web, by method hot rolling, (hot-rolled temperature is less than fusing point higher than the glass transition temperature of fiber, is 130-
150℃).In the hot rolling, the speed and pressure of hot-pressing roller remain unchanged, to prepare PLA staple fiber nonwoven cloth.
Wakita et al.[Wakita T,Obata A,Poologasundarampillai G,Jones JR,
Kasuga T:Preparation of electrospun siloxane-poly(lactic acid)-vaterite
hybrid fibrous membranes for guided bone regeneration.Compos Sci Technol
2010,70(13):1889-1893.] using electrospinning process it is prepared for siloxane-poly (lactic acid) (PLA)-
Holder of the vaterite composite non-weaving cloths as Guided Bone Regeneration, and improved using hydroxyapatite (HA) coatings
The cell compatibility of fabric.The experimental results showed that composite non-weaving cloth after coating has release soluble silicon and calcium
Ability can stimulate osteoblast in gene level.And there is this porous support smaller aperture can prevent soft tissue
Entrance, the release of promoting bone growing and ion, while enhancing bone growth.Chen et al.[Chen HC,Tsai CH,
Yang MC:Mechanical properties and biocompatibility of electrospun
polylactide/poly(vinylidene fluoride)mats.J Polym Res 2011,18(3):319-327.] it will
PLA is dissolved in cosolvent N,N-dimethylformamide and third after being mixed with poly (vinylidene fluoride) (PVDF)
Electrostatic spinning is carried out in ketone, prepares the nano-fiber for production of non-woven of different mixing proportion respectively, and studies fibre morphology, contact
Angle, thermal property, tensile property, blood compatibility and cell compatibility.The experimental results showed that with PLA and PVDF non-woven cloths
It compares, PLA/PVDF composite non-weaving cloths have preferable fibroblast proliferation ability and application potential.Au et al.
[Chen HC,Tsai CH,Yang MC:Mechanical properties and biocompatibility of
electrospun polylactide/poly(vinylidene fluoride)mats.J Polym Res 2011,18(3):
319-327.] it is prepared for polylactic acid/chitosan (PLA/CS) and polylactic acid/chitosan/nanometer respectively using electrostatic spinning technique
Silver-colored (PLA/CS/Ag) non-woven cloth, the experimental results showed that the Static Spinning non-woven cloth containing nano silver have to Escherichia coli and
The preferable anti-microbial property of staphylococcus aureus.Haroosh et al.[Haroosh HJ,Dong Y,Ingram GD:
Synthesis,Morphological Structures,and Material Characterization of
Electrospun PLA:PCL/Magnetic Nanoparticle Composites for Drug Delivery.J
Polym Sci Pol Phys 2013,51(22):1607-1617.] magnetic nanoparticle (MPs) is added to poly
(lactic acid)(PLA):Electrostatic spinning is carried out in poly (e-caprolactone) (PCL) solution prepares complex nonwoven
Cloth, and quadracycline is added in compound and studies medicine-releasing performance.Experimental result is consistent with forefathers' research theory,
Show that the composite non-weaving cloth has preferable medicine-releasing performance, can apply in terms of drug delivery.Casasola et
al.[Casasola R,Thomas NL,Trybala A,Georgiadou S:Electrospun poly lactic acid
(PLA)fibres:Effect of different solvent systems on fibre morphology and
diameter.Polymer 2014,55(18):4728-4737.] systematic research Static Spinnings of the PLA in different solvents can
The property spun, fibre morphology, the viscosity of spinning solution, electric conductivity and surface tension.The experimental results showed that in all solvents, acetone/bis-
Methylformamide has higher production efficiency, can prepare the best nanofiber without defect (beading pattern).Parwe
et al.[Parwe SP,Chaudhari PN,Mohite KK,Selukar BS,Nande SS,Garnaik B:
Synthesis of ciprofloxacin-conjugated poly(L-lactic acid)polymer for
nanofiber fabrication and antibacterial evaluation.Int J Nanomed 2014,9:1463-
1477.] Ciprofloxacin and PLA are passed through into electrospun nanofibers composite membrane, fibre diameter 150-400nm, hole
Diameter is 62-102nm.The experimental results showed that the composite membrane has preferably to the releasability of Ciprofloxacin and inhibition golden yellow
The growth ability of staphylococcus and Escherichia coli.This biodegradable Ciprofloxacin-nano-fiber for production of non-woven can answer
In terms of drug conveying.Li et al.[Li DP,Frey MW,Baeumner AJ:Electrospun polylactic
acid nanofiber membranes as substrates for biosensor assemblies.J Membrane
Sci 2006,279(1-2):354-363.] it biotin is added in PLA spinning solutions carries out electrostatic spinning, prepare bio-sensing
Device nano fibrous membrane.
Moran et al.[Moran JM,Pazzano D,Bonassar LJ:Characterization of
polylactic acid polyglycolic acid composites for cartilage tissue
engineering.Tissue Eng 2003,9(1):63-70.] by polyglycolic acid (PGA) non-woven cloth (fiber
A diameter of 15mm, porosity ＞ 95%) it is cut into small pieces respectively, then use 0.5,1.0,2.0 and 3.0% PLA of 1mL molten respectively
Then holder test performance and is studied ox articular chondrocytes and existed by liquid (PLA is dissolved in dichloromethane) coating after drying
Growing state on polylactic acid (PLA)/polyglycolic acid (PGA) composite material.The experimental results showed that cell shown on PGA it is flat
Flat shape shape, and it is more close round on PLA.This holder can be used in cartilage tissue engineered aspect.In addition, also PLA/ is sub-
Numb complex nonwoven cloth material [Alimuzzaman S, Gong RH, Akonda M:Nonwoven Polylactic Acid
and Flax Biocomposites.Polym Composite 2013,34(10):1611-1619.；Alimuzzaman S,
Gong RH,Akonda M:Three-dimensional nonwoven flax fiber reinforced polylactic
acid biocomposites.Polym Composite 2014,35(7):1244-1252.], PLA/ hemps are laminated composite wood
Expect [Song YS, Lee JT, Ji DS, Kim MW, Lee SH, Youn JR:Viscoelastic and thermal
behavior of woven hemp fiber reinforced poly(lactic acid)composites.Compos
Part B-Eng 2012,43(3):856-860.], PLA/ bamboo fibers laminar composite [Porras A, Maranon
A:Development and characterization of a laminate composite material from
polylactic acid(PLA)and woven bamboo fabric.Compos Part B-Eng 2012,43(7):
2782-2788.], cocoanut fiber/PLA fibrous composites [Jang JY, Jeong TK, Oh HJ, Youn JR, Song YS:
Thermal stability and flammability of coconut fiber reinforced poly(lactic
acid)composites.Compos Part B-Eng 2012,43(5):2434-2438.], ramie fabric/PLA film lamination is multiple
Condensation material [Zhou NT, Yao L, Liang YZ, Yu B, Ye MQ, Shan ZD, Qiu YP:Improvement of
mechanical properties of ramie/poly(lactic acid)(PLA)laminated composites
using a cyclic load pre-treatment method.Ind Crop Prod 2013,45:94-99.], bluish dogbane/
PLA composite electrons material [Serizawa S, Inoue K, Iji M:Kenaf-fiber-reinforced poly(lactic
acid)used for electronic products.J Appl Polym Sci 2006,100(1):618-624.], greatly
Fiber crops/PLA biological degradable composite materials [Hu R, Lim JK:Fabrication and mechanical properties of
completely biodegradable hemp fiber reinforced polylactic acid composites.J
Compos Mater 2007,41(13):1655-1669.]。
Tingaut et al.[Tingaut P,Zimmermann T,Lopez-Suevos F:Synthesis and
Characterization of Bionanocomposites with Tunable Properties from Poly
(lactic acid)and Acetylated Microfibrillated Cellulose.Biomacromolecules
2010,11(2):454-464.] PLA is dissolved in chloroform (2%w/w), and using PLA as matrix, micro- original of acetylation
Fine (MFC) is that reinforcement prepares Biological nanocomposite.The experimental results showed that this Biocomposite material has preferable heat
Stability and hygroscopicity.
Due to preparing the deficiency of unordered stent Methods in the development prospect and application potential and forefathers' document of unordered holder
Place, the present invention attempt PLA melting spinning fibers being prepared as unordered holder using bonding method.
Invention content
The object of the present invention is to provide a kind of simple and practicable, meet environment protection requirement, and fiber is spun in polylactic acid melting
Between bond it is close, will not decoherence, the preferable polylactic acid melting of formability spins fiber heat bonding and cures three-dimensional porous unordered holder
Preparation method.
The preparation method that fiber heat bonding cures three-dimensional porous unordered holder is spun in the polylactic acid melting of the present invention, there is following two
Kind technical solution：
Scheme 1：
The preparation method that fiber heat bonding cures three-dimensional porous unordered holder is spun in polylactic acid melting, is included the following steps：
1) polylactic acid slice with good biodegradability properties and biocompatibility is prepared by melt spinning method fine
Dimension；
2) acid fiber by polylactic for preparing step 1), with measuring reel in Zhou Changwei 999-1001mm, width 3-4cm
Ryce parallel winded is carried out to fiber, it is orderly to obtain polylactic acid with the initial tension of the rotating speed of 1-300r/min and 100cN
Fibre bundle；
3) polylactic acid ordered fiber beam prepared by step 2) is cut into the staple fiber that length is 1-4cm, then by staple fiber
Aggregate be uniformly paved into it is netted, in 60-140 DEG C of temperature, 13 × 106Under Pa pressure, hot pressing 1-60min obtains three-dimensional porous nothing
Sequence holder；
Or polylactic acid ordered fiber beam prepared by step 2) is cut into the staple fiber that length is 1-4cm, then by short fibre
Dimension aggregate be uniformly paved into it is netted, in 60-140 DEG C of temperature, 13 × 106Under Pa pressure, hot pressing 1-60min, then at 0 DEG C, 1-13
×106It is cold-pressed 1-5min under Pa pressure conditions to be bonded, then cooled to room temperature, obtains three-dimensional porous unordered holder.
Scheme 2：
The preparation method that fiber heat bonding cures three-dimensional porous unordered holder is spun in polylactic acid melting, is included the following steps：
By the polylactic acid slice with good biodegradability properties and biocompatibility, single-screw extruder, spiral shell are utilized
Bar draw ratio L/D=28：1, drum rotation speed 21.0rpm, traversing speed be 38.8cm/min, screw speed 5.65r/min,
Orifice diameter is 0.02mm, and spinning die head temperature is 250 DEG C, and hot air temperature is 320 DEG C, heat air pressure 0.3MPa,
Spinning nozzle is 75-200mm to the reception distance received between roller, is thermally bonded by itself, obtains three-dimensional porous unordered holder.
In the present invention, the molecular weight of the polylactic acid (PLA) is 170000-200000.
The beneficial effects of the present invention are：
The method of the present invention is simple and practicable, does not pollute, and bonding is close, will not take off between polylactic acid melting spinning fiber
Dissipate, formability it is preferable, the needs of commercial application can be met.It is three-dimensional that spinning fiber heat bonding solidification preparation is melted using polylactic acid
The method of porous unordered holder, can be to other high polymers (such as polycaprolactone, polyglycolic acid, polyethylene glycol, polyurethane etc.)
Melting spin fiber and prepare similar holder reference is provided.The unordered holder of fiber is spun in polylactic acid melting prepared by the preparation method to be had
Preferable internal pore structure, physical property and mechanical property, and there is preferable application potential, biomaterial can be used as
It applies in terms of bone tissue engineer.
Description of the drawings
Fig. 1 is the stereoscan photograph that the unordered rack surface of fiber is spun in PLA meltings prepared by embodiment 1.
Fig. 2 is the stereoscan photograph that the unordered holder cross section shapes of fiber are spun in PLA meltings prepared by embodiment 1.
Fig. 3 is the stereoscan photograph that the unordered rack surface of fiber is spun in PLA meltings prepared by embodiment 2.
Fig. 4 is the stereoscan photograph that the unordered holder cross section shapes of fiber are spun in PLA meltings prepared by embodiment 2.
Fig. 5 is the stereoscan photograph that the unordered rack surface of fiber is spun in PLA meltings prepared by embodiment 3.
Fig. 6 is the stereoscan photograph that the unordered holder cross section shapes of fiber are spun in PLA meltings prepared by embodiment 3.
Fig. 7 is the stereoscan photograph that the unordered rack surface of fiber is spun in PLA meltings prepared by embodiment 4.
Fig. 8 is the stereoscan photograph that the unordered holder cross section shapes of fiber are spun in PLA meltings prepared by embodiment 4.
Fig. 9 is the stereoscan photograph that the unordered rack surface of fiber is spun in PLA meltings prepared by embodiment 5.
Figure 10 is the stereoscan photograph that the unordered holder cross section shapes of fiber are spun in PLA meltings prepared by embodiment 5.
Figure 11 is the stereoscan photograph that the unordered rack surface of fiber is spun in PLA meltings prepared by embodiment 6.
Figure 12 is the stereoscan photograph that the unordered holder cross section shapes of fiber are spun in PLA meltings prepared by embodiment 6.
Specific implementation mode
It further illustrates the present invention with reference to embodiments.
Embodiment 1：
The PLA slices that molecular weight is 170000 are prepared into the PLA fibres that average diameter is 12.41 μm by melt spinning method
Dimension；Utilize YG086 type measuring reels 1000 aggregates arranged in parallel of coiling, rotating speed 300r/min, ryce Zhou Changwei
1000mm, width 3.5cm, initial tension 100cN.Fibre bundle is spun in orderly PLA meltings arranged in parallel to be cut with scissors
10 times, it is 1cm staple fibers 10000 to be cut into length.Then it by 10000 uniform lappings of 1cm staple fiber aggregates, then carries out
Hot pressing and cold pressing, hot pressing temperature are 60 DEG C, hot pressing time 5min, and hot pressing pressure is 13 × 106Pa, temperature of colding pressing is 0 DEG C, cold
The pressure time is 5min, and cold pressing pressure is 13 × 106Pa.Then cooled to room temperature obtains three-dimensional porous unordered holder.
Surface and cross section shapes such as Fig. 1 and 2 of the porous unordered holder of fibre three-dimensional are spun in PLA meltings prepared by the embodiment
It is shown.As seen from the figure, PLA meltings spin fiber and random mixed and disorderly disorderly arranged, average thickness are presented in this three-dimensional porous unordered holder
Degree is 0.02cm, weight 0.0054g/cm2, the degree of order is 81.7 °, and the average pore size of hole is 17.8 μm, and porosity is
54.4%, connectivity is preferable between hole.Holder along fiber direction tensile stress and strain be respectively 0.0026MPa and
48.9%.Embodiment 2：
Method is 2cm difference lies in PLA melting spinning short fiber length is changed with embodiment 1.PLA prepared by the embodiment
The surface of the melting spinning porous unordered holder of fibre three-dimensional and cross section shapes are as shown in Figures 3 and 4.As seen from the figure, this unordered branch
PLA meltings spin fiber and random mixed and disorderly disorderly arranged, average thickness 0.056cm, weight 0.019g/cm are presented in frame2, orderly
Degree is 70.2 °, and the average pore size of hole is 20.9 μm, porosity 65.9%, and connectivity is preferable between hole.Holder is along fiber alignment
The tensile stress in direction and strain are respectively 0.04MPa and 73.3%.
Embodiment 3：
Method is 4cm difference lies in PLA melting spinning short fiber length is changed with embodiment 1.PLA prepared by the embodiment
The surface of the melting spinning porous unordered holder of fibre three-dimensional and cross section shapes are as illustrated in Figures 5 and 6.As seen from the figure, this unordered branch
PLA meltings spin fiber and random mixed and disorderly disorderly arranged, average thickness 0.092cm, weight 0.039g/cm are presented in frame2, orderly
Degree is 37.3 °, and the average pore size of hole is 19.8 μm, porosity 74%, and connectivity is preferable between hole.Holder is along fiber alignment side
To tensile stress and strain be respectively 0.16MPa and 126.2%.
Embodiment 4：
The PLA that molecular weight is 170000 is sliced, SJ-30/28 single-screw extruders, screw slenderness ratio L/D are utilized
=28：1.Drum rotation speed is 21.0rpm, and traversing speed is 38.8cm/min, screw speed 5.65r/min, orifice diameter
For 0.02mm.Spinning die head temperature is 250 DEG C, and hot air temperature is 320 DEG C, heat air pressure 0.3MPa, spinning nozzle to rolling
Reception distance between cylinder is 75mm.It without hot pressing and cold pressure procedure, is thermally bonded by itself, it is 3 μm to obtain fibre diameter
The three-dimensional porous unordered holders of PLA.
Surface and cross section shapes such as Fig. 7 and 8 of the porous unordered holder of fibre three-dimensional are spun in PLA meltings prepared by the embodiment
It is shown.As seen from the figure, PLA meltings spinning fiber presentation is random mixed and disorderly disorderly arranged in this unordered holder, and average thickness is
0.12cm, weight 0.014g/cm2, the degree of order is 73.5 °, and the average pore size of hole is 19.7 μm, porosity 59.8%,
Connectivity is preferable between hole.Holder is respectively 0.059MPa and 70.7% along the tensile stress of fiber direction and strain.
Embodiment 5:
For method with embodiment 4, difference lies in change to receive distance as 100mm.Obtain the PLA tri- that fibre diameter is 5.3 μm
Tie up porous unordered holder.Surface and cross section shapes such as Fig. 9 and 10 of the unordered holder of fiber are spun in PLA meltings prepared by the embodiment
It is shown.As seen from the figure, PLA meltings spinning fiber presentation is random mixed and disorderly disorderly arranged in this unordered holder, and average thickness is
0.072cm, weight 0.0093g/cm2, the degree of order is 60.2 °, and the average pore size of hole is 17.8 μm, and porosity is
65.4%, connectivity is preferable between hole.Holder along fiber direction tensile stress and strain be respectively 0.028MPa and
58.5%.
Embodiment 6:
For method with embodiment 4, difference lies in change to receive distance as 200mm.Obtain the PLA tri- that fibre diameter is 5.3 μm
Tie up porous unordered holder.The embodiment prepare PLA melting spin the unordered holder of fiber surface and cross section shapes such as Figure 11 and
Shown in 12.As seen from the figure, PLA meltings spinning fiber presentation is random mixed and disorderly disorderly arranged in this unordered holder, and average thickness is
0.13cm, weight 0.012g/cm2, the degree of order is 79.2 °, and the average pore size of hole is 13 μm, porosity 51.2%, hole
Between connectivity it is preferable.Holder is respectively 0.035MPa and 53.5% along the tensile stress of fiber direction and strain.
Claims (2)
1. the preparation method that fiber heat bonding cures three-dimensional porous unordered holder is spun in a kind of polylactic acid melting, it is characterized in that including such as
Lower step：
By the polylactic acid slice with good biodegradability properties and biocompatibility, using single-screw extruder, screw rod is long
Diameter ratio L/D=28：1, drum rotation speed 21.0rpm, traversing speed are 38.8cm/min, screw speed 5.65r/min, spinneret
Bore dia is 0.02mm, and spinning die head temperature is 250 DEG C, and hot air temperature is 320 DEG C, heat air pressure 0.3MPa, spinneret
Mouth is 75-200mm to the reception distance received between roller, by itself heat bonding, obtains three-dimensional porous unordered holder.
2. the preparation side that fiber heat bonding cures three-dimensional porous unordered holder is spun in polylactic acid melting according to claim 1
Method, it is characterized in that the polylactic acid molecule amount is 170000-200000.
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| CN201510040458.4A CN104674454B (en) | 2015-01-27 | 2015-01-27 | Method for manufacturing three-dimensional porous disorder scaffolds from polylactic acid molten spinning fibers by means of thermal bonding and solidifying |
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| WO2021229111A1 (en) * | 2020-05-12 | 2021-11-18 | Laboratorios Farmacéuticos Rovi, S.A. | Method for purifying biodegradable thermoplastic polymer particles for medical and/or pharmaceutical use |
| CN113293517B (en) * | 2021-05-27 | 2022-05-13 | 河南驼人医疗器械研究院有限公司 | Polylactic acid elastic superfine fiber non-woven material and preparation method and application thereof |
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