CN104667343A - Preparation method of ordered scaffold employing thermal bonding curing of polylactic acid melt spinning fiber - Google Patents
Preparation method of ordered scaffold employing thermal bonding curing of polylactic acid melt spinning fiber Download PDFInfo
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Abstract
The invention discloses a preparation method of an ordered scaffold employing thermal bonding curing of a polylactic acid melt spinning fiber. The method comprises the following steps: preparing a melt spinning fiber from polylactic acid (PLA) slices with good biodegradability and biocompatibility by a melt spinning method; preparing fiber assemblies which are arranged in parallel by a winding process; and forming an ordered scaffold with a stable structure by PLA fiber assemblies which are loose and are arranged in parallel by a thermal bonding curing manner. The ordered scaffold produced by the PLA melt spinning fiber prepared by the method is stable in structure, and has a relatively good internal hole structure, physical property and mechanical property; and the ordered scaffold can be applied to the biomedical fields of bone tissue engineering and the like, and has relatively good application potential and prospect. According to the preparation method, a reference can be provided for preparation of similar structure brackets employing the melt spinning fibers of other high polymers, such as polycaprolactone, polyglycolic acid and polyurethane.
Description
Technical field
The present invention relates to polylactic acid melting and spin the preparation method that orderly support is solidified in fiber heat bonding.
Background technology
By the subject matter [Langer R, Vacanti JP:Tissue Engineering.Science 1993,260 (5110): 920-926.] that the loss of wound or the aging organ or tissue caused and fault are health cares.The main purpose of organizational project creates the organ or tissue [Risbud M:Tissue engineering:implications in the treatment of organ and tissue defects.Biogerontology 2001,2 (2): 117-125.] that defect was repaired or replaced to biologic replacement materials.Wherein, Cranial defect is a kind of common clinical disease, cause one of middle-aged and elderly people pain and disabled most common cause [Buckwalter JA, Mankin HJ:Articular cartilage:Degeneration and osteoarthritis, repair, regeneration, and transplantation.Aaos Instr Cours Lec 1998,47:487-504.].Because autotransplantation and heteroplastic transplantation method exist many defects [Shin H, Jo S, Mikos AG:Biomimetic materials for tissue engineering.Biomaterials 2003,24 (24): 4353-4364.], therefore, be necessary to adopt some biologic replacement materials to repair Cranial defect.
Design and manufacture ideal stent is the subject matter that organizational project faces.Because ideal stent can promote cell adhesion, sustenticular cell growth, propagation and differentiation, and promote formation [the Gross KA of extracellular matrix (ECM), Rodriguez-Lorenzo LM:Biodegradable composite scaffolds with an interconnected spherical network for bone tissue engineering.Biomaterials 2004,25 (20): 4955-4962.].This just requires that support must have suitable internal pore structure and surface nature, the mechanical property consistent with host tissue, and there is biocompatibility, degradability and sterilizability [Ma PX:Scaffolds for tissue fabrication.Mater Today 2004,7 (5): 30-40.].
At present, the preparation method of support mainly contains two classes, that is: traditional preparation method and advanced preparation method.Traditional preparation method comprises fibres bond, solvent cast/particle leaching, gas foaming, is separated and lyophilization [Yang SF, Leong KF, Du ZH, Chua CK:The design of scaffolds for use in tissue engineering.Part 1.Traditional factors.Tissue Eng 2001,7 (6): 679-689.].Advanced preparation method mainly computer Aided Design (CAD) and rapid shaping technique, comprise fusion sediment, 3D printing, 3D drawing, finite element device technique and selective laser sintering [Leong KF, Chua CK, Sudarmadji N, Yeong WY:Engineering functionally graded tissue engineering scaffolds.J Mech Behav Biomed 2008,1 (2): 140-152.].And select suitable biomaterial to be the key building tissue engineering bracket.These biomaterials that can be used for creating support have natural macromolecular material (collagen and chitosan), synthesized polymer material (Poly-L-lactic acid (Poly (L-lactic acid), PLLA), polyglycolic acid (Poly (glycolic acid, and polycaprolactone (Poly (caprolactone) PGA), and bioceramic (hydroxyapatite (Hydroxyapatite PCL), and tricalcium phosphate (Tricalcium phosphate HA), TCP) [Leong KF, Chua CK, Sudarmadji N, Yeong WY:Engineering functionally graded tissue engineering scaffolds.J Mech Behav Biomed 2008, 1 (2): 140-152.] etc.
The directivity of its medium-height trestle mesopore is another important parameter.This is because extracellular matrix is the internal structure with high-sequential, this ordered structure can allow cell realize differentiation function [Hunziker EB better, Quinn TM, Hauselmann HJ:Quantitative structural organization of normal adult human articular cartilage.Osteoarthr Cartilage 2002,10 (7): 564-572.].And extracellular matrix can provide machinery to support and biochemical signals, thus can affect cytoskeletal structure, chromatin organization and genetic transcription.Therefore, it may be necessary orderly support to natural environment [the Ma ZW of the orientation texture and cell of simulating natural tissues, Kotaki M, Inai R, Ramakrishna S:Potential of nanofiber matrix as tissue-engineering scaffolds.Tissue Eng 2005, 11 (1-2): 101-109.], and the growth of normal tissue and function carry out regulating and controlling [Bissell MJ, Hall HG, Parry G:How Does the Extracellular-Matrix Direct Gene-Expression.J Theor Biol1982, 99 (1): 31-68.].
At present, the method preparing orderly support mainly concentrates on electrostatic spinning technique.Xu et al. [the Xu CY of NUS, Inai R, Kotaki M, Ramakrishna S:Aligned biodegradable nanotibrous structure:a potential scaffold for blood vessel engineering.Biomaterials2004, 25 (5): 877-886.], Li et al. [the Li D of University of Washington, Wang YL, Xia YN:Electrospinning of polymeric and ceramic nanofibers as uniaxially aligned arrays.Nano Lett 2003, 3 (8): 1167-1171.], Katta et al. [the Katta P of Akron university, Alessandro M, Ramsier RD, Chase GG:Continuous electrospinning of aligned polymer nanofibers onto a wire drum collector.Nano Lett 2004, 4 (11): 2215-2218.], Choi et al. [the Choi JS of Wake Forest University of U.S. regenerative medicine institute, Lee SJ, Christ GJ, Atala A, Yoo JJ:The influence of electrospun aligned poly (epsilon-caprolactone)/collagen nanofiber meshes on the formation of self-aligned skeletal muscle myotubes.Biomaterials 2008, 29 (19): 2899-2906.] and Carnell et al. [the Carnell LS of US National Aeronautics and Space Administration's Langley Research Center, Siochi EJ, Holloway NM, Stephens RM, Rhim C, Niklason LE, Clark RL:Aligned mats from electrospun single fibers.Macromolecules 2008, 41 (14): 5345-5349.] electrostatic spinning technique is utilized to prepare orderly support respectively.In addition, research worker is also had to adopt unidirectional heat pulling method [Zong XH, Ran SF, Fang DF, Hsiao BS, Chu B:Control of structure, morphology and property in electrospun poly (glycolide-co-lactide) non-woven membranes via post-draw treatments.Polymer 2003, 44 (17): 4959-4967.] and fusion sediment method [Zein I, Hutmacher DW, Tan KC, Teoh SH:Fused deposition modeling of novel scaffold architectures for tissue engineering applications.Biomaterials 2002, 23 (4): 1169-1185.] orderly support is prepared, and the domestic research to orderly support is less.Utilize electrostatic spinning technique to prepare orderly support Shortcomings part, cannot meet the requirement of practical application, current research is only in the experimental stage.Unidirectional heat drawing process is easy to cause the fracture of fiber and the out-of-flatness of rack surface in drawing process.Fusion sediment method be computer ancillary technique to realize the ordered arrangement of fiber, operating process more complicated.
Polylactic acid (Poly (lactic acid), PLA) belongs to aliphatic polyester, is derived from 'alpha '-hydroxy acids, and basic material is that Lactic acid is present in optically active D-or L-enantiomer.According to the ratio of enantiomer, the different materials of PLA can be obtained.With existing take oil as the polymer phase ratio of raw material, PLA has goodish optics, physics, machinery and barrier property [Auras RA, Harte B, Selke S, Hernandez R:Mechanical, physical, and barrier properties of poly (lactide) films.J Plast Film Sheet 2003,19 (2): 123-135.].Because polylactic acid has good mechanical property, thermoplasticity, machinability biocompatibility and biodegradability, there are better prospect and potentiality as biomaterial at medical square mask.
About the melt spinning of PLA, some adopt Single screw extrusion method, and some are double screw extrusion methods.Wherein there is spinning 100%PLA fiber, also have the composite spinning of PLA and other raw material.Schmack et al. [Schmack G, Tandler B, Vogel R, Beyreuther R, Jacobsen S, Fritz HG:Biodegradable fibers of poly (L-lactide) produced by high-speed melt spinning and spin drawing.J Appl Polym Sci 1999, 73 (14): 2785-2797.] with Mw=164, 000g/mol, Mn=76, 000g/mol, Mz=288, the PLA polymer of 000g/mol carries out melt spinning, the diameter of screw extruder used is for being 8mm, coiling speed is 1000-5000m/min, the flow of dosing pump is 16.2g/min, melt temperature is 185 DEG C, spinneret contains 12 spinneret orifices, each orifice diameter is 0.3mm, length is 0.6mm.Then the as-spun fibre of preparation is carried out 4-6 drawing-off doubly by two heat conduction rollers, prepared fibre diameter is, vitrification point Tg=57 DEG C.
Cicero et al. [Cicero JA, Dorgan JR:Physical properties and fiber morphology of poly (lactic acid) obtained from continuous two-step melt spinning.J Polym Environ 2001, 9 (1): 1-10.] PLA of the Dow Chemical Company (Cargill Dow) is adopted, the Mn=547 of two Lot samples, 600 and Mn=558, 100, need PLA raw material before spinning at 82 DEG C of dry 14h, Killion KL-125 single screw extrusion machine is utilized to carry out two step melt spinnings, spinnerette diameters is 2.16mm.By the fiber of preparation first through water-bath cooling, then through the first godet, radiation heating district, the second godet, pressure roller and spiral filament forming machine.Research draw ratio is on the impact of fusing point, fiber temperature, shrinkage, modulus, elongation at break, tensile strength and Changing Pattern, and prepared fiber strength is 0.10-0.35GPa.
Cicero et al. [Cicero JA, Dorgan JR, Janzen J, Garrett J, Runt J, Lin JS:Supramolecular morphology of two-step, melt-spun poly (lactic acid) fibers.J Appl Polym Sci 2002,86 (11): 2828-2838.] single screw extrusion machine is utilized, PLA fiber is prepared by two step melt spinning methods, the Tg=61.7-70.2 DEG C of fiber, Tm=160.6-165.1 DEG C, fiber diameter range is 25-65nm.And study draw ratio (2-8) to the impact of vitrification point, modulus, fibre diameter and shrinkage factor.
Fambri et al. [Fambri L, Pegoretti A, Fenner R, Incardona SD, Migliaresi C:Biodegradable fibres of poly (L-lactic acid) produced by melt spinning.Polymer 1997, 38 (1): 79-85.] by Boehringer (Ingelheim, Germany) molecular weight provided is the PLLA of 330000, utilize Estru 13 single-screw extrusion machine (Friulfiliere, Italy) (first step utilizes different rates to melt extrude to carry out two step melt spinnings, second step is 160 DEG C of hot gas spring), need section dry 48h in 50 DEG C of vacuum drying ovens before spinning, orifice diameter is 1mm, the inbound pacing of glass roll is 1.8-20m/min.The as-spun fibre diameter that spins is 133-480 μm, and after drawing-off, gained fibre diameter is 48-106 μm, and modulus and tensile strength are respectively 9.2GPa and 0.87GPa.
Yuan et al. [Yuan XY, Mak AFT, Kwok KW, Yung BKO, Yao KD:Characterization of poly (L-lactic acid) fibers produced by melt spinning.J Appl Polym Sci 2001, 81 (1): 251-260.] by PLLA, (viscosity-average molecular weight is respectively 494600, 304700 and 262800, RUPAC provides) section, utilize single screw extrusion machine (RANDCASTLE Microtruder, orifice diameter is 1.0mm, screw speed is 9.5 revs/min), carry out two step melt spinnings (melt extruding and hot gas spring), need section dry 48h in 50 DEG C of vacuum drying ovens before spinning, spinning temperature is 200-240 DEG C, fiber collecting speed is 3.20m/min, hot gas spring temperature is 120 DEG C, drafting rate is 0.26m/min, winding rate is 1.09m/min.Fibre diameter before non-drawing-off and modulus are respectively 250-360 μm and 1.2-2.4GPa, and the fibre diameter after hot gas spring is 110-160 μm, and after drawing-off, the modulus of fiber is 3.6-5.4GPa, and brute force is 300-600MPa.
Cicero et al. [Cicero JA, Dorgan JR, Garrett J, Runt J, Lin JS:Effects of molecular architecture on two-step, melt-spun poly (lactic acid) fibers.J Appl Polym Sci 2002, 86 (11): 2839-2846.] two step melt spinning methods are utilized to prepare PLA fiber (L:D=96:4), and research research draw ratio (1-8) to linear and branching PLA polymer spin the fusing point of fiber, degree of crystallinity, shrinkage, modulus, the impact of tensile strength, experimental result shows, along with draw ratio increases, the fusing point of fiber and shrinkage have reduction in various degree, and degree of crystallinity, modulus and tensile strength increase.Spin linear polymer microfiber diameter be 23-30nm, and the microfiber diameter of branched polymer is 19-32nm.
Persson et al. [Persson M, Cho SW, Skrifvars M:The effect of process variables on the properties of melt-spun poly (lactic acid) fibres for potential use as scaffold matrix materials.J Mater Sci 2013, 48 (8): 3055-3066.] other PLA and PLLA of medical grade (is provided by NatureWorks, the viscosity-average molecular weight Mv=178300 of PLA, the Mv=545600 of PLLA) carry out melt spinning, utilize piston spinning-drawing machine (Fourne ' Polymertechnik, Germany) by two step spinning (melt extruding and solid-state drawing-off), need before spinning at 80 DEG C of dry 4h.Utilize circular jetting filament plate (30 holes, each orifice diameter is 1mm, length is 0.3mm) obtain monofilament and multifilament fiber, spinning temperature is 180-220 DEG C, fiber accepts speed is 8.9m/min, the melt-draw ratio (melt-draw ratio is coiling speed and the melt velocity leaving spinning head) of monfil is 5.3, and the melt-draw ratio of multifilament fiber is 14.2, then fiber is carried out drawing-off by one group of heat conduction roller.These fibers have higher hot strength, can be applied to the woven fabric of three-dimensional porous structure, knitted fabric and non-weaving cloth support.
Pegoretti et al. [Pegoretti A, Fambri L, Migliaresi C:In vitro degradation of poly (L-lactic acid) fibers produced by melt spinning.J Appl Polym Sci 1997, 64 (2): 213-223.] by PLLA (Mv=330000, fusing point is 187 DEG C, degree of crystallinity is 75.3%, thered is provided by the Boehringer Ingelheim of Germany) by two-step method (melt extruding and hot gas spring) experiment extruder spinning (Friulfiliere, Italy. screw diameter is 14mm, orifice diameter is 1.0mm), spinning temperature is 200-240 DEG C, screw speed is 15 revs/min, the temperature of glass draw roll is 160 DEG C, the fibre diameter that spins is 120 ± 10 μm, 72 ± 7 μm.
Solarski et al. [Solarski S, Ferreira M, Devaux E:Characterization of the thermal properties of PLA fibers by modulated differential scanning calorimetry.Polymer2005, 46 (25): 11187-11192.] by PLA (by Galactic, Belgium provides), pass through single screw extrusion machine, spinning temperature is 220-225 DEG C, the spinneret in 40 holes, orifice diameter is 400 μm, spinning PLA multifilament, then different hot-pressing rollers is utilized to carry out drawing-off, fibre diameter is 45.5-56.4 μm.
Fang et al. [Fang Q, Hanna MA:Rheological properties of amorphous and semicrystalline polylactic acid polymers.Ind Crop Prod 1999,10 (1): 47-53.] two kinds of PLA (are provided by Cargill, Mn=88000), one is unbodied polymer, one is hemicrystalline polymer, and the laboratory single screw extruder utilizing draw ratio to be 20:1 carries out spinning.
Schmack et al. [Schmack G, Jehnichen D, Vogel R, Tandler B, Beyreuther R, Jacobsen S, Fritz HG:Biodegradable fibres spun from poly (lactide) generated by reactive extrusion.J Biotechnol 2001, 86 (2): 151-160.] by PLA (being provided by IKT Stuttgart) by melt extruding, screw diameter is 18mm, extrusion temperature is 170-185 DEG C, 12 hole spinnerets, each orifice diameter is 0.3mm, length is 0.6mm, coiling speed is 1000-5000m/min, prepare the PLA fiber of different coiling speed (1000-5000m/min) and drafting multiple (4-6), and study coiling speed and drafting multiple to the elongation at break of fiber, stress, modulus, the impact of degree of crystallinity and fusing point and Changing Pattern.Spin fiber maximum modulus be 460MPa, stress is 6.3GPa, and elongation at break is 24%.
Rentenberger et al. [Rentenberger R, Cayla A, Villmow T, Jehnichen D, Campagne C, Rochery M, Devaux E, Potschke P:Multifilament fibres of poly (epsilon-caprolactone)/poly (lactic acid) blends with multiwalled carbon nanotubes as sensor materials for ethyl acetate and acetone.Sensor Actuat B-Chem2011, 160 (1): 22-31.] apparatus for melt spinning is utilized to prepare PLA multifilament, preparation process has two steps, the first step is joined in PCL by 4wt%MWCNT to put into twin (double) screw extruder (screw diameter is 16mm, draw ratio is 25, screw speed is 100 revs/min) extrude, obtain the line that diameter is 1.5mm.Second step is mixed by PCL+4%MWCNT/PLA=50/50wt%, after Single screw extrusion, utilizes the melt blending of getting to know of 1.2mm diameter.Two bundle monofilament are cooled rear compound in atmosphere and becomes multifilament containing 80 monofilament, after twisting, the fineness of multifilament is 1270tex.Multifilament is obtained woven fabric after woven.
Nam et al. [Nam JY, Okamoto M, Okamoto H, Nakano M, Usuki A, Matsuda M:Morphology and crystallization kinetics in a mixture of low-molecular weight aliphatic amide and polylactide.Polymer 2006, 47 (4): 1340-1347.] by PLA (being provided by Toyota Motor Corporation) and N, N-Ethylenebis is blended, utilize TEX30 α twin screw (Nippon Steel Engineering Co., Ltd) melt spinning, spinning temperature is 200 DEG C, screw speed is 300 revs/min, charging rate is 120g/min.Prepared composite fibre vitrification point is 52 DEG C, and fusing point is 173.5 DEG C.
Solarski S et al. [Solarski S, Ferreira M, Devaux E, Fontaine G, Bachelet P, Bourbigot S, Delobel R, Coszach P, Murariu M, Ferreira ADS et al:Designing polylactide/clay nanocomposites for textile applications:Effect of processing conditions, spinning, and characterization.J Appl Polym Sci 2008, 109 (2): 841-851.] PLA (is provided by Galactic S.A., Mn=74500) and Bentone 104 utilize the spinning of double screw extruder melt blending, screw diameter is 16mm, draw ratio is 25, spinning temperature is 140-190 DEG C, screw speed is 150 revs/min, 40 hole spinnerets, orifice diameter is 400 μm.By the multifilament of preparation again by one group of heat-stretching roller drawing-off, drafting multiple is 2-3.5, and the rotating speed of feeding roller is 200m/min, and temperature is 70 DEG C, the rotating speed 400-750m/min of draw roll, and temperature is 110 DEG C.Prepared multifilament fineness is 1600dtex, then multifilament is formed knitted fabric, and weight is 1000g/m
2, thickness is 3mm.
Potschke et al. [Potschke P, Andres T, Villmow T, Pegel S, Brunig H, Kobashi K, Fischer D, Haussler L:Liquid sensing properties of fibres prepared by melt spinning from poly (lactic acid) containing multi-walled carbon nanotubes.Compos Sci Technol 2010, 70 (2): 343-349.] by PLA, (Germany provides, Tg=60 DEG C, Tm=170 DEG C) and multi-walled carbon nano-tubes (Nanocyl S.A., Belgium provides) by ZE25 twin screw spinning (Berstorff, Germany), screw diameter is 25mm, draw ratio is 36.Before spinning, PLA section and powdery multi-wall carbon nano-tube tube material are loaded hopper simultaneously, screw speed is 500 revs/min, spinning temperature is 180-220 DEG C, coiling speed is respectively 20,50 and 100m/min, draw ratio is respectively 7.3,18.2 and 36.5, preparation PLA and multi-walled carbon nano-tubes composite fibre.
Due to development prospect and the application potential of orderly support, and prepare the weak point of orderly stent Methods in forefathers' document, the present invention attempts PLA melting to spin fiber, utilizes bonding method, is prepared as orderly support.
Summary of the invention
The object of this invention is to provide a kind of simple, meet environment protection requirement, and polylactic acid melting to spin between fiber bonding closely, can not decoherence, the melting of formability good polylactic acid spins the preparation method that orderly support is solidified in fiber heat bonding.
The preparation method that orderly support is solidified in fiber heat bonding is spun in polylactic acid melting of the present invention, comprises the steps:
1) polylactic acid slice with good biodegradability properties and biocompatibility is prepared into fiber by melt spinning method;
2) by step 1) acid fiber by polylactic prepared, with thread yarn horizontal metroscope girth be 999-1001mm, width is the ryce of 3-4cm, with the initial tension of the rotating speed of 1-300r/min and 100cN, parallel winded is carried out to fiber, obtains polylactic acid ordered fiber bundle;
3) by step 2) the polylactic acid ordered fiber bundle prepared, 60-140 DEG C of temperature, 1119.8-13 × 10
6under Pa pressure, hot pressing 1-60min, obtains orderly support;
Or by step 2) the polylactic acid ordered fiber bundle prepared, 60-140 DEG C of temperature, 1119.8-13 × 10
6under Pa pressure, after hot pressing 1-60min, then in 0 DEG C of temperature, 1-13 × 10
6the 1-5min that colds pressing under Pa pressure condition bonds, and then naturally cools to room temperature, obtains orderly support.
The molecular weight of the polylactic acid (PLA) described in the present invention is 170000-200000.
Beneficial effect of the present invention is:
The inventive method is simple, does not pollute, meets environment protection requirement, and polylactic acid melting to spin between fiber bonding closely, can not decoherence, formability is better, can meet the needs of commercial application.The method utilizing polylactic acid melting to spin fiber to prepare orderly support, can spin fiber to the melting of other high polymer (such as polycaprolactone, polyglycolic acid, polyurethane etc.) and prepare similar support and provide reference.Polylactic acid melting prepared by this preparation method is spun the orderly support of fiber and is had good internal pore structure, physical property and mechanical property.This orderly support can be applied in the bio-medical fields such as bone tissue engineer, has good application potential and prospect.
Accompanying drawing explanation
Fig. 1 is that the stereoscan photograph of the orderly rack surface of fiber is spun in PLA melting prepared by embodiment 1.
Fig. 2 is that the stereoscan photograph of the orderly support cross section shapes of fiber is spun in PLA melting prepared by embodiment 1.
Fig. 3 is that the stereoscan photograph of the orderly rack surface of fiber is spun in PLA melting prepared by embodiment 2.
Fig. 4 is that the stereoscan photograph of the orderly support cross section shapes of fiber is spun in PLA melting prepared by embodiment 2.
Fig. 5 is that the stereoscan photograph of the orderly rack surface of fiber is spun in PLA melting prepared by embodiment 3.
Fig. 6 is that the stereoscan photograph of the orderly support cross section shapes of fiber is spun in PLA melting prepared by embodiment 3.
Fig. 7 is that the stereoscan photograph of the orderly rack surface of fiber is spun in PLA melting prepared by embodiment 4.
Fig. 8 is that the stereoscan photograph of the orderly support cross section shapes of fiber is spun in PLA melting prepared by embodiment 4.
Fig. 9 is that the stereoscan photograph of the orderly rack surface of fiber is spun in PLA melting prepared by embodiment 5.
Figure 10 is that the stereoscan photograph of the orderly support cross section shapes of fiber is spun in PLA melting prepared by embodiment 5.
Detailed description of the invention
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1:
By molecular weight be 170000 PLA section prepare by melt spinning method the PLA fiber that average diameter is 12.41 μm; With the aggregation that YG086 type thread yarn horizontal metroscope coiling 1000 is arranged in parallel, rotating speed is 300r/min, and ryce girth is 1000mm, and width is 3.5cm, and initial tension is 100cN.Utilize vulcanizing press successively to carry out hot pressing and adhering and solidifying of colding pressing, hot pressing temperature is 60 DEG C, and hot pressing time is 5min, and hot pressing pressure is 13 × 10
6pa, temperature of colding pressing is 0 DEG C, and the time of colding pressing is 5min, and pressure of colding pressing is 13 × 10
6pa.Cold pressing after terminating, take out from vulcanizing press, naturally cool to room temperature, obtain orderly support.PLA melting prepared by this embodiment spins the surface of the orderly support of fiber and cross section shapes as illustrated in fig. 1 and 2.
As seen from the figure, in this orderly support, PLA melting is spun fiber and is presented parallel ordered arrangement, and average thickness is 0.396cm, and weight is 0.02908g/cm
2, the degree of order is 88.2722 °, and the average pore size of hole is 6.986 μm, and porosity is 53.33%, better connective between hole.Support is respectively 1.156209MPa and 0.988501% along the tensile stress of fiber direction and strain.
Embodiment 2:
Method is with embodiment 1, and difference is that changing hot pressing temperature is 140 DEG C.PLA melting prepared by this embodiment spins the surface of the orderly support of fiber and cross section shapes as shown in Figures 3 and 4.As seen from the figure, in this orderly support, PLA melting is spun fiber and is presented parallel ordered arrangement, and average thickness is 0.304cm, and weight is 0.02822g/cm
2, the degree of order is 87.6182 °, and the average pore size of hole is 1.3569 μm, and porosity is 44.15263%.Support is respectively 1.134945MPa and 0.904015% along the tensile stress of fiber direction and strain.
Embodiment 3:
By molecular weight be 200000 PLA section prepare by melt spinning method the PLA fiber that average diameter is 12.41 μm; Utilize the aggregation that YG086 type thread yarn horizontal metroscope coiling 1000 is arranged in parallel, rotating speed is 300r/min, and ryce girth is 1000mm, and width is 3.5cm, and initial tension is 100cN.Utilize vulcanizing press successively to carry out hot pressing and adhering and solidifying of colding pressing, hot pressing temperature is 60 DEG C, and hot pressing time is 1min, and hot pressing pressure is 13 × 10
6pa, temperature of colding pressing is 0 DEG C, and the time of colding pressing is 5min, and pressure of colding pressing is 13 × 10
6pa.Cold pressing after terminating, take out from vulcanizing press, naturally cool to room temperature, obtain orderly support.PLA melting prepared by this embodiment spins the surface of the orderly support of fiber and cross section shapes as illustrated in Figures 5 and 6.
As seen from the figure, in this orderly support, PLA melting is spun fiber and is presented parallel ordered arrangement, and average thickness is 0.404cm, and weight is 0.03112g/cm
2, the degree of order is 89.6345 °, and the average pore size of hole is 4.5382 μm, and porosity is 61.51515%, better connective between hole.Support is respectively 1.178873MPa and 1.134549% along the tensile stress of fiber direction and strain.
Embodiment 4:
Method is with embodiment 3, and difference is that changing hot pressing time is 30min.PLA melting prepared by this embodiment spins the surface of the orderly support of fiber and cross section shapes as shown in FIG. 7 and 8.In this orderly support, PLA melting is spun fiber and is presented parallel ordered arrangement, and average thickness is 0.36cm, and weight is 0.03066g/cm
2, the degree of order is 86.4194 °, and the average pore size of hole is 2.8335 μm, and porosity is 56.32824%.Support is respectively 1.187487MPa and 1.693421% along the tensile stress of fiber direction and strain.
Embodiment 5:
By molecular weight be 170000 PLA section prepare by melt spinning method the PLA fiber that average diameter is 12.41 μm; Utilize the aggregation that YG086 type thread yarn horizontal metroscope coiling 1000 is arranged in parallel, rotating speed is 300r/min, and ryce girth is 1000mm, and width is 3.5cm, and initial tension is 100cN.By the PLA ordered fiber bundle of preparation, at 60 DEG C, under 1119.8Pa pressure, hot pressing 1h, obtains orderly support.
PLA melting prepared by this embodiment spins the surface of the orderly support of fiber and cross section shapes as shown in Figures 9 and 10.As seen from the figure, in this orderly support, PLA melting is spun fiber and is presented parallel ordered arrangement, and average thickness is 0.07cm, and weight is 0.03972g/cm
2, the degree of order is 81.7351 °, and the average pore size of hole is 17.8497 μm, and porosity is 46.67%, better connective between hole.Support is respectively 1.080633MPa and 2.20075% along the tensile stress of fiber direction and strain.
Claims (2)
1. the preparation method that orderly support is solidified in fiber heat bonding is spun in polylactic acid melting, it is characterized in that comprising the steps:
1) polylactic acid slice with good biodegradability properties and biocompatibility is prepared into fiber by melt spinning method;
2) by step 1) acid fiber by polylactic prepared, with thread yarn horizontal metroscope girth be 999-1001mm, width is the ryce of 3-4cm, with the initial tension of the rotating speed of 1-300 r/min and 100cN, parallel winded is carried out to fiber, obtains polylactic acid ordered fiber bundle;
3) by step 2) the polylactic acid ordered fiber bundle prepared, 60-140 DEG C of temperature, 1119.8-13 × 10
6under Pa pressure, hot pressing 1-60min, obtains orderly support;
Or by step 2) the polylactic acid ordered fiber bundle prepared, 60-140 DEG C of temperature, 1119.8-13 × 10
6under Pa pressure, after hot pressing 1-60min, then in 0 DEG C of temperature, 1-13 × 10
6the 1-5 min that colds pressing under Pa pressure condition bonds, and then naturally cools to room temperature, obtains orderly support.
2. the preparation method that orderly support is solidified in fiber heat bonding is spun in polylactic acid melting according to claim 1, it is characterized in that described polylactic acid molecule amount is 170000-200000.
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| CN101444641A (en) * | 2008-12-24 | 2009-06-03 | 浙江大学 | Three-dimensional large aperture tissue engineering scaffold based on nano-fibers and application thereof |
| WO2009152349A1 (en) * | 2008-06-12 | 2009-12-17 | 3M Innovative Properties Company | Melt blown fine fibers and methods of manufacture |
| CN104258473A (en) * | 2014-09-29 | 2015-01-07 | 上海交通大学 | Spinning-enhanced poly-p-xylene composite film and preparation method thereof |
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| WO2009152349A1 (en) * | 2008-06-12 | 2009-12-17 | 3M Innovative Properties Company | Melt blown fine fibers and methods of manufacture |
| CN101444641A (en) * | 2008-12-24 | 2009-06-03 | 浙江大学 | Three-dimensional large aperture tissue engineering scaffold based on nano-fibers and application thereof |
| CN104258473A (en) * | 2014-09-29 | 2015-01-07 | 上海交通大学 | Spinning-enhanced poly-p-xylene composite film and preparation method thereof |
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| CN105233340A (en) * | 2015-10-22 | 2016-01-13 | 浙江大学 | Method for preparing medical polylactic acid melt-spun fiber porous ordered scaffold |
| CN105233340B (en) * | 2015-10-22 | 2018-09-21 | 浙江大学 | The preparation method of the orderly holder of fiber multihole is spun in medical polylactic acid melting |
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