PHBV神經(jīng)導(dǎo)管的靜電紡絲法制備
發(fā)布時間：2018-07-25 11:49
【摘要】：周圍神經(jīng)損傷以后的修復(fù)、再生和功能恢復(fù)一直是神經(jīng)科學(xué)研究的熱點(diǎn),組織工程學(xué)的出現(xiàn)為神經(jīng)損傷的修復(fù)提供了一個新的思路。目前,神經(jīng)導(dǎo)管已經(jīng)成為修復(fù)周圍神經(jīng)損傷的途徑之一。如何制備出有利于神經(jīng)再生、分化和生長的神經(jīng)導(dǎo)管支架一直是神經(jīng)組織工程學(xué)的難點(diǎn)。靜電紡絲技術(shù)所制備的電紡納米纖維支架材料具有孔隙率高、比表面積大等優(yōu)點(diǎn),能夠從納米尺度上模仿天然細(xì)胞外基質(zhì),可作為細(xì)胞生長的多孔支架,促進(jìn)細(xì)胞的遷移和增殖。 本文利用羥基丁酸-羥基戊酸共聚酯(PHBV)、聚乙二醇(PEG)、聚己內(nèi)酯(PCL)為支架材料,通過靜電紡絲、熔融紡絲、等離子體改性等技術(shù)制備三層靜電紡絲有序纖維神經(jīng)導(dǎo)管。其特征在于,由靜電紡PHBV/PEG有序亞微米纖維薄膜卷繞而成的內(nèi)層管、由熔融紡絲制備的PCL單絲編織成的中間層網(wǎng)狀導(dǎo)管和由靜電紡絲法直接噴射而成的PHBV高比表面積、高孔隙率外層管。通過掃描電鏡(SEM)、差示掃描量熱儀(DSC)、廣角X射線衍射(WAXD)、偏振紅外光譜、萬能試驗(yàn)機(jī)等手段對靜電紡絲制備的PHBV纖維的形態(tài)、纖維排列有序性、結(jié)晶性能、取向度、力學(xué)性能進(jìn)行表征；通過SEM、動態(tài)力學(xué)分析(DMA)、熱重分析(TG)、DSC、WAXD、傅里葉變換紅外光譜(FTIR)、偏光顯微鏡(PLM)等手段對PHBV/PEG纖維的形態(tài)、纖維排列有序性、相容性、結(jié)晶性能及晶體形態(tài)進(jìn)行表征；通過SEM、萬能試驗(yàn)機(jī)、接觸角儀等測試對神經(jīng)導(dǎo)管的表面微觀形態(tài)、力學(xué)性能及親水性進(jìn)行表征。主要研究結(jié)果如下： (1)PHBV可溶于氯仿(CHCl3)/DMF (10//1)混合溶劑中進(jìn)行靜電紡絲,紡絲的最佳工藝參數(shù)為：濃度6%,電壓12KV,推進(jìn)速度0.5ml/h。 (2)轉(zhuǎn)軸法制備靜電紡有序PHBV纖維過程中,隨著轉(zhuǎn)軸表面線速度的提高,纖維的排列有序度、晶區(qū)取向度及分子鏈取向度、結(jié)晶度以及力學(xué)強(qiáng)度增大,10.5m/s時達(dá)到最大值,其后又有所降低。轉(zhuǎn)軸表面線速度的提高一方面促進(jìn)纖維排列有序度的提高,另一方面也會對纖維進(jìn)行拉伸,使纖維的平均直徑減小,取向度進(jìn)一步提高,晶粒尺寸減小。電紡有序PHBV纖維在拉伸過程中經(jīng)過屈服點(diǎn)以后沒有明顯的“細(xì)頸”現(xiàn)象,而是隨著應(yīng)變的增大應(yīng)力逐漸降低直至完全斷裂。 (3)以氯仿/DMF(10/1)為溶劑,靜電紡絲制備PHBV/PEG纖維的最佳紡絲參數(shù)為：濃度8%,電壓10KV,出樣速率為0.8ml/h,接收距離18cm。當(dāng)PEG的比例小于50wt%時,PHBV/PEG共混物的可紡性都比較好,紡出的纖維表面光滑,直徑比較均勻；當(dāng)PEG增加到70wt%以后,PHBV/PEG溶液仍然能夠紡絲,但是紡出的絲斷頭很多。靜電紡絲制備PHBV/PEG有序纖維的最佳轉(zhuǎn)軸表面線速度為9.5m/s,其纖維的排列有序度較純PHBV稍差。 (4)DMA和FTIR分析證明了PHBV與PEG是不相容的。在氮?dú)鈿夥罩?PEG的加入改善了PHBV的熱穩(wěn)定性；在空氣氣氛中,當(dāng)PEG得含量超過50wt%時,共混物的熱穩(wěn)定性變差。通過DSC、XRD、POM分析表明在PHBV/PEG共混體系中隨著PEG含量的提高,PHBV熔點(diǎn)稍微降低,晶粒變小,結(jié)晶溫度顯著降低；當(dāng)PEG的含量不超過50wt%時,PHBV的結(jié)晶度基本不變,超過50wt%以后其結(jié)晶度顯著降低。 (5)在卷繞PHBV/PEG內(nèi)管過程中,卷繞層數(shù)以5層為佳,每層厚度約為8μm；中間層導(dǎo)管的最佳編織參數(shù)為：纖度為32.43tex的PCL單絲,編織錠數(shù)為8錠；神經(jīng)導(dǎo)管外層PHBV纖維膜其表面的纖維排列有序度較低,外層導(dǎo)管的孔隙率較高,為81%左右。水接觸角測試結(jié)果顯示,隨著PEG含量的增加,PHBV/PEG內(nèi)管的親水性增加；經(jīng)過等離子改性以后,PHBV外管的親水性顯著增強(qiáng)。
[Abstract]:The repair, regeneration and functional recovery of peripheral nerve injury have been the focus of neuroscience research. The appearance of tissue engineering provides a new idea for the repair of nerve injury. At present, the nerve conduit has become one of the ways to repair the peripheral nerve injury. Transcatheter stent is a difficult problem in neural tissue engineering. Electrospun electrospun nanofiber scaffold has the advantages of high porosity and large surface area. It can mimic natural extracellular matrix from nanoscale, which can be used as a porous scaffold for cell growth and promote cell migration and proliferation.
In this paper, three layers of electrospun fibers were prepared by using hydroxybutyrate Hydroxyvalerate copolyester (PHBV), polyethylene glycol (PEG) and polyhexyl ester (PCL) as scaffolds, which were prepared by electrostatic spinning, melt spinning, and plasma modification. It was characterized by an inner tube rolled by a electrostatic spinning PHBV/PEG ordered submicron fiber film. The PHBV high specific surface area, high porosity surface area, and high porosity outer tube formed by PCL monofilament made by melt spinning and direct injection by electrostatic spinning method, and by means of scanning electron microscopy (SEM), differential scanning calorimeter (DSC), wide-angle X ray diffraction (WAXD), partial vibration infrared spectroscopy, universal testing machine and so on, the PHBV prepared by electrostatic spinning The morphology, ordering, crystallization, orientation, and mechanical properties of fibers are characterized by SEM, dynamic mechanical analysis (DMA), thermogravimetric analysis (TG), DSC, WAXD, Fourier transform infrared (FTIR), polarization microscope (PLM) and other means for the morphology, ordering, compatibility, crystallization and crystal morphology of PHBV/ PEG fibers The surface micromorphology, mechanical properties and hydrophilicity of the nerve conduits were characterized by SEM, universal testing machine and contact angle meter. The main results were as follows:
(1) PHBV can be electrospun in mixed solvents of chloroform (CHCl3) /DMF (10//1). The best spinning parameters are: concentration 6%, voltage 12KV, advancing speed 0.5ml/h.
(2) in the process of preparing the ordered PHBV fiber by the rotating shaft method, the order degree of the fiber, the orientation degree of the crystal area, the degree of molecular chain orientation, the crystallinity and the mechanical strength increase with the increase of the surface line speed of the rotating shaft, and the maximum value is reached at the time of 10.5m/s. The increase of the speed of the axis of the rotating shaft promotes the arrangement of the fibers on the one hand. On the other hand, the fiber will be stretched, the average diameter of the fiber is reduced, the orientation degree is further improved, and the grain size decreases. After the yield point of the electrospun ordered PHBV fiber, there is no obvious "fine neck" phenomenon after the yield point, but the stress gradually decreases to the complete fracture with the increase of strain.
(3) with chloroform /DMF (10/1) as solvent, the optimum spinning parameters for the preparation of PHBV/PEG fibers by electrostatic spinning are as follows: the concentration is 8%, the voltage 10KV, the sample rate is 0.8ml/h, the receiving distance 18cm. when the proportion of PEG is less than 50wt%, the spinnability of the PHBV/PEG blends is better, the fiber surface is smooth and the diameter is more uniform; PEG increases to 70wt%, The PHBV/PEG solution can still spin, but the spun yarn has a lot of broken ends. The optimal axis speed of the electrostatic spinning PHBV/PEG ordered fiber is 9.5m/s, and the order degree of the fiber is slightly worse than that of the pure PHBV.
(4) DMA and FTIR analysis showed that PHBV was incompatible with PEG. In the nitrogen atmosphere, the addition of PEG improved the thermal stability of PHBV. In the air atmosphere, when the content of PEG exceeded 50wt%, the thermal stability of the blends became worse. The analysis of DSC, XRD, POM analysis showed that the melting point decreased slightly in the PHBV/PEG co mixing system with the increase of the content. Grain size decreased and crystallization temperature decreased significantly. When the content of PEG was not more than 50wt%, the crystallinity of PHBV remained almost unchanged, and its crystallinity decreased significantly after 50wt%.
(5) in the process of winding PHBV/PEG inner tube, the number of winding layers is good with 5 layers, and the thickness of each layer is about 8 mu m; the best weaving parameters of the middle layer catheter are PCL monofilament with the size of 32.43tex, the number of weave ingot is 8, the fiber arrangement of the PHBV fiber membrane on the outer layer of the nerve conduit is lower, the porosity of the outer tube is higher, and is about 81%. The contact angle test results show that the hydrophilicity of the PHBV/PEG inner tube increases with the increase of the PEG content, and the hydrophilicity of the PHBV tube is significantly enhanced after the plasma modification.
【學(xué)位授予單位】：東華大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2011
【分類號】：R318.08
本文編號：2143731
[Abstract]:The repair, regeneration and functional recovery of peripheral nerve injury have been the focus of neuroscience research. The appearance of tissue engineering provides a new idea for the repair of nerve injury. At present, the nerve conduit has become one of the ways to repair the peripheral nerve injury. Transcatheter stent is a difficult problem in neural tissue engineering. Electrospun electrospun nanofiber scaffold has the advantages of high porosity and large surface area. It can mimic natural extracellular matrix from nanoscale, which can be used as a porous scaffold for cell growth and promote cell migration and proliferation.
In this paper, three layers of electrospun fibers were prepared by using hydroxybutyrate Hydroxyvalerate copolyester (PHBV), polyethylene glycol (PEG) and polyhexyl ester (PCL) as scaffolds, which were prepared by electrostatic spinning, melt spinning, and plasma modification. It was characterized by an inner tube rolled by a electrostatic spinning PHBV/PEG ordered submicron fiber film. The PHBV high specific surface area, high porosity surface area, and high porosity outer tube formed by PCL monofilament made by melt spinning and direct injection by electrostatic spinning method, and by means of scanning electron microscopy (SEM), differential scanning calorimeter (DSC), wide-angle X ray diffraction (WAXD), partial vibration infrared spectroscopy, universal testing machine and so on, the PHBV prepared by electrostatic spinning The morphology, ordering, crystallization, orientation, and mechanical properties of fibers are characterized by SEM, dynamic mechanical analysis (DMA), thermogravimetric analysis (TG), DSC, WAXD, Fourier transform infrared (FTIR), polarization microscope (PLM) and other means for the morphology, ordering, compatibility, crystallization and crystal morphology of PHBV/ PEG fibers The surface micromorphology, mechanical properties and hydrophilicity of the nerve conduits were characterized by SEM, universal testing machine and contact angle meter. The main results were as follows:
(1) PHBV can be electrospun in mixed solvents of chloroform (CHCl3) /DMF (10//1). The best spinning parameters are: concentration 6%, voltage 12KV, advancing speed 0.5ml/h.
(2) in the process of preparing the ordered PHBV fiber by the rotating shaft method, the order degree of the fiber, the orientation degree of the crystal area, the degree of molecular chain orientation, the crystallinity and the mechanical strength increase with the increase of the surface line speed of the rotating shaft, and the maximum value is reached at the time of 10.5m/s. The increase of the speed of the axis of the rotating shaft promotes the arrangement of the fibers on the one hand. On the other hand, the fiber will be stretched, the average diameter of the fiber is reduced, the orientation degree is further improved, and the grain size decreases. After the yield point of the electrospun ordered PHBV fiber, there is no obvious "fine neck" phenomenon after the yield point, but the stress gradually decreases to the complete fracture with the increase of strain.
(3) with chloroform /DMF (10/1) as solvent, the optimum spinning parameters for the preparation of PHBV/PEG fibers by electrostatic spinning are as follows: the concentration is 8%, the voltage 10KV, the sample rate is 0.8ml/h, the receiving distance 18cm. when the proportion of PEG is less than 50wt%, the spinnability of the PHBV/PEG blends is better, the fiber surface is smooth and the diameter is more uniform; PEG increases to 70wt%, The PHBV/PEG solution can still spin, but the spun yarn has a lot of broken ends. The optimal axis speed of the electrostatic spinning PHBV/PEG ordered fiber is 9.5m/s, and the order degree of the fiber is slightly worse than that of the pure PHBV.
(4) DMA and FTIR analysis showed that PHBV was incompatible with PEG. In the nitrogen atmosphere, the addition of PEG improved the thermal stability of PHBV. In the air atmosphere, when the content of PEG exceeded 50wt%, the thermal stability of the blends became worse. The analysis of DSC, XRD, POM analysis showed that the melting point decreased slightly in the PHBV/PEG co mixing system with the increase of the content. Grain size decreased and crystallization temperature decreased significantly. When the content of PEG was not more than 50wt%, the crystallinity of PHBV remained almost unchanged, and its crystallinity decreased significantly after 50wt%.
(5) in the process of winding PHBV/PEG inner tube, the number of winding layers is good with 5 layers, and the thickness of each layer is about 8 mu m; the best weaving parameters of the middle layer catheter are PCL monofilament with the size of 32.43tex, the number of weave ingot is 8, the fiber arrangement of the PHBV fiber membrane on the outer layer of the nerve conduit is lower, the porosity of the outer tube is higher, and is about 81%. The contact angle test results show that the hydrophilicity of the PHBV/PEG inner tube increases with the increase of the PEG content, and the hydrophilicity of the PHBV tube is significantly enhanced after the plasma modification.
【學(xué)位授予單位】：東華大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2011
【分類號】：R318.08
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