| With the improvement of living standards and the advancement of science and technology,people have begun to pursue a healthy and quality life,and the demand for functional materials and products has been increasing and antibacterial functional materials have received more and more attention.Textiles,such as underwear,bed sheets,and shirts,sanitary products,such as masks,food packaging materials,etc.,are prone to breed bacteria during the daily use process,which has a negative impact on product performance and human health.If these products have antibacterial properties,they can effectively inhibit the growth of bacteria,which can prevent the materials from emitting unpleasant gases and even threaten human health due to bacterial reproduction.In recent years,more and more attention has been paid to functional aromatic materials.The aromatic materials can release aromatic odor,delight the body and mind,relieve stress,and improve human sub-health.Antibacterial and aromatic composite functional materials are the development trend of multifunctional materials,but currently the preparation methods are mostly through two functional finishing,and the problem of non-persistent functions generally existed.In this paper,linalool(LAO),which has both antibacterial and aromatic properties,is selected as a functional substance.On the basis of ?-cyclodextrin(?-CD)inclusion LAO,quaternization polymerization modification of ?-CD was performed to obtain long-lasting antibacterial and aromatic properties.And use it as a functional substance,polyacrylonitrile(PAN)/LAO/quaternized ?-cyclodextrin polymer(p-CCD)micro-nanofiber were prepared by electrospinning,and their long-lasting antibacterial and aromatic properties were studied.Firstly,the LAO/?-CD inclusion complex was prepared using the saturated solution method with LAO as the core material and ?-CD as the wall material.The effects of the volume-to-mass ratio of LAO and ?-CD,the inclusion temperature and the inclusion time on the yield,oil content and oil inclusion rate of inclusion complex were investigated by a single-factor test,the optimal inclusion conditions were determined,that is,the volume-to-mass ratio of LAO and ?-CD was 1:6,the inclusion temperature was 50 °C,the inclusion time was 2 hours.At this time,the yield of inclusion complex was 74.8%,the oil content was 130.9 mg/g,and the oil inclusion rate was 64.2%.The structure of the LAO/?-CD inclusion complex was characterized by scanning electron microscope(SEM),fourier transform infrared spectroscopy(FTIR),and thermogravimetric analysis(TG).Gas chromatography-mass spectrometry was used to test the content of LAO in the inclusion complex after being left for different times.The results of the minimum inhibitory concentration showed that even the concentration of the inclusion complex reached to 25.6 mg/m L,its antibacterial property was not obvious.The content of LAO in the inclusion complex still reached to 104 mg/g after keeping 12 weeks,which has the effect of slowly release LAO and fragrance retention.Secondly,in order to enhance the antibacterial properties of the LAO/?-CD inclusion complex,?-CD was modified by quaternization polymerization.?-CD,epichlorohydrin(EP)and 2,3-epoxypropyl-trimethylammonium chloride(ETMAC)as for reactants,the quaternized ?-CD polymer was synthesized,and the reaction conditions were optimized by single-factor experiment.The effects of ?-CD and ETMAC molar ratio,?-CD and EP molar ratio,reaction temperature and reaction time on product yield and Zeta potential were discussed.The optimal reaction conditions were determined,that is,the molar ratio of ?-CD and ETMAC was 1: 5,the molar ratio of ?-CD and EP was 1:10,the reaction temperature was 60 °C,and the reaction time was 3 hours.At this reaction condition,the p-CCD yield was 4.119 g,and the Zeta potential was +12.8 m V.The SEM,1H Nuclear Magnetic Resonance Spectra(1H-NMR),FTIR,TG were used to characterize the structure of ?-CD and p-CCD,and the minimum inhibitory concentration was used to characterize the antibacterial performance.The experimental results show that the minimum inhibitory concentration of p-CCD against E.coli and S.aureus is divided into 0.8 mg/m L and 1.6 mg/m L,which significantly improves the antibacterial performance of ?-CD.Then,the LAO used as the core material and the p-CCD used as the wall material to prepare the LAO/p-CCD inclusion complex.The orthogonal test method was used to optimize the preparation conditions,that is,the volume-to-mass ratio of LAO and p-CCD was 1:6,the inclusion temperature was 50 °C and the inclusion time was 2 hours.At this time,the yield of the inclusion complex was 70.6%,the oil content was 95.2 mg/g,and the oil inclusion rate was 62.5%.The formation of the LAO/ p-CCD inclusion complex was verified by SEM,FTIR and TG analysis methods.The results antibacterial test showed that the minimum inhibitory concentration of the LAO/p-CCD inclusion complex against E.coli and S.aureus was 0.4 mg/m L,p-CCD and LAO synergistically antibacterial,which enhanced the antibacterial performance of LAO/p-CCD inclusion complex.And the content of LAO in the inclusion complex was continuously tested for 12 weeks.As a result,the release rate of LAO in the inclusion complex was only 25.9% after keeping 12 weeks,which has a long-lasting fragrance retention effect.Finally,in view of the advantages of electrospinning micro-nanofiber,such as small diameter,large specific surface area,and high porosity,as for functional carrier materials can effectively improve the stability of functional substances and regulate the release characteristics of functional substances.In this paper,PAN micro-nanofiber with different LAO/p-CCD inclusion complex mass fractions were prepared using a stepped pyramid needle-free electrospinning technology.The experimental results showed that as the LAO/p-CCD inclusion mass fraction increased,the viscosity and the electrical conductivity of the PAN solution increased,but the spinning performance was not significantly affected and the diameter of the micro-nanofiber was not significantly changed.When the LAO/p-CCD inclusion complex mass fraction increased from 0% to 10%,the antibacterial rates of micro-nanofiber against E.coli and S.aureus were changed from 11.7% to 98.2% and 9.2% to 96.6%,and the content of LAO in micro-nanofiber increased from 0 mg/g to 51.7 mg/g.The research on the long-lasting antibacterial and aromatic properties of PAN/ LAO/ p-CCD micro-nanofiber showed that the antibacterial rate of micro-nanofiber against E.coli and S.aureus respectively decreased from 98.2% and 96.6% to 94.0% and 87.5% after keeping 12 weeks.Being left for different times,the release rate of LAO in the micro-nanofiber gradually slowed down,and the fragrance retention time could reach to 12 weeks.It can be seen that PAN/LAO/ p-CCD micro-nanofiber have long-lasting antibacterial and aromatic properties. |
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