CN102493014B - A kind of epsilon-polylysine polyvinyl alcohol compound bio anti-bacterial fibre and preparation method thereof - Google Patents
A kind of epsilon-polylysine polyvinyl alcohol compound bio anti-bacterial fibre and preparation method thereof Download PDFInfo
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- CN102493014B CN102493014B CN201110360128.5A CN201110360128A CN102493014B CN 102493014 B CN102493014 B CN 102493014B CN 201110360128 A CN201110360128 A CN 201110360128A CN 102493014 B CN102493014 B CN 102493014B
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Abstract
The present invention relates to a kind of production method of epsilon-polylysine polyvinyl alcohol (PVA) composite antibacterial fibre, during preparation, adopt water-DMSO system, add the NaCl of 1 ~ 3% in mixed liquor, in the spin solvent mixed, add epsilon-polylysine.Take the PVA of 8 ~ 20%, add under room temperature in spinning solution, stir and make it fully to touch solvent, stop stirring rear standing immersion 30 ~ 60min, then be placed in water-bath and heat, progressively be warming up to 60 ~ 70 DEG C, keep 1 ~ 2h, be then warming up to 95 ~ 100 DEG C and PVA is dissolved completely, dissolve the complete 2 ~ 3h that is incubated again and can carry out spray silk, the condensation bath absolute methanol of-20 DEG C, condensation time 10 ~ 60s, in condensation being bathed, anti-bacterial fibre takes out drying at room temperature and can obtain spun.Spun becomes by stretching the anti-bacterial fibre product that diameter is 0.005 ~ 0.1mm.Adding of epsilon-polylysine makes fiber be provided with good bacteriostatic activity, and bacteriostasis rate reaches more than 97%, can be used for antibiotic fabric and produces.
Description
Technical field
The invention belongs to biological chemical field, relate to a kind of preparation method of epsilon-polylysine polyvinyl alcohol compound bio anti-bacterial fibre.
Background technology
Epsilon-polylysine (epsilon-polylysine) is a kind of lysine homopolymer of being produced by fermentable, is formed by connecting by α-carboxyl and epsilon-amino by 25 ~ 35 lysine residues.1977, Shima and Sakai found this amino acid polymer first in the fermentation clear liquid of StreptomycesalbulusNBRC14147 bacterial strain.Epsilon-polylysine is a kind of polycationic polypeptides nontoxic to human-body safety, and can suppress gramnegative bacterium, gram-positive bacteria, fungi even some virus, antimicrobial spectrum is extensive.After proving epsilon-polylysine security by mouse experiment, the countries such as Japan, Korea S, the U.S. it can be used as antiseptics for natural food and extensive use.
Polyvinyl alcohol has unique strong adherence, epithelium pliability, flatness, and its aqueous solution has good cementability and film forming, is mainly used in textile industry warp size, fabric finishing agent, vinylon fiber raw material; Building decoration industry 107 glue, coating for internal and external wall, adhesive; Chemical industry is used as polymeric emulsifiers, dispersant and polyvinyl formal, acetal, butyral resin; Paper industry is used as paper product adhesive; Agricultural aspect is used for soil conditioner, agricultural chemicals adheres to synergist and vinal; Also can be used for the aspect such as daily cosmetics and high-frequency quenching agent.
According to the retrieval, following pertinent literature and patent is found.
The paper " preparation of Tea Polyphenols/polylactic acid composite nano fibre film and anti-microbial property research " that the people such as Fei Yanna delivered the 24th volume the 8th phase " material Leader " in 2010 discloses a kind of employing method of electrostatic spinning, Tea Polyphenols is mixed to prepare the composite nano-fiber membrane with anti-microbial property with PLA, not only enrich the function of single polylactic acid nano fiber film, also widened the Application Areas of Tea Polyphenols well, the research for antibacterial fabric opens a new road.
Patent 200510024952.8 discloses activated carbon fiber-Nano Silver composite antibiotic material in medical use and preparation method thereof.Material is Ag activated carbon fiber being adsorbed with 200-400mg/pg.Presoma carbon fiber-containing adopts gasification to obtain activated carbon fiber in conjunction with activation method by preparation method, and make nano-Ag particles embed fibrous inside by immersing or spray Ag-containing solution and shaking, finally processing obtains finished product.Not with an organic solvent, cost is low, and security performance is high, is easy to large-scale production.
Patent CN101187089 " fibroin albumen and polyvinyl alcohol blending antibacterial nanometer fiber and preparation method thereof " discloses a kind of nanofiber and preparation method thereof, and its component is fibroin albumen, Ag simple substance particle and polyvinyl alcohol; Its preparation method is: a. natural silk obtains regenerated silk fibroin after coming unstuck, dissolve, purify, drying; B. again fibroin albumen is dissolved in acid solution and obtains regenerated silk acid solution; C. polyvinyl alcohol obtains poly-vinyl alcohol solution after dissolving; D. two kinds of solution blendings; E. silver-based inorganic salt is added; F. carry out electrostatic spinning with silver electrode again, obtain blended nanofibre felt; G. by the heat treatment 2 ~ 5 minutes under the temperature conditions of 100 ~ 150 DEG C of blended nanofibre felt, then through UV-irradiation process 3 ~ 5 hours, fibroin albumen and polyvinyl alcohol blending antibacterial nanometer fiber is obtained.
Patent CN101189971A " application of a kind of inorganic/organic nano composite antibacterial and fibre thereof " discloses the application of a kind of inorganic/organic nano composite antibacterial and fibre thereof, by inorganic antiseptic: 0.01 ~ 20 part, organic antibacterial agent: 0.01 ~ 35 part, the compatible finishing agent of inorganic/organic antibacterial agent: 0.0001-0.4 part, polymer binder: 0.05 ~ 40 part, the stabilizing agent of anti-inorganic antiseptic variable color: 0.0001-0.4 part, efficient emulsifying agent: 0.1-30 part, distilled water: 100 parts, moistening dispersion is carried out by weight with reinforced order, grinding, high speed dispersion, the processing such as stirring, obtain nanoscale complex antimicrobials.This antiseptic can adopt the process fibres such as dip method, tie-dyeing process, spraying process.With clothes, socks, carpet, bedding, operation dress, johnny, mouth mask, hospital gauze, airstrainer etc. obtained by inorganic/organic nano composite antibacterial of the present invention; have that antibiotic rate is high, antibacterial action rapidly and the characteristics such as anti-microbial property is lasting, wash resistant; can be used for the aspect such as life and medical treatment; play prevent disease occur and propagate; protection human health, the effect of improving the quality of living.
Above-mentioned patent document mainly concentrates on and adopts inorganic Ag, Cu particle or organic antibacterial agent dodecyl benzyl dimethyl ammonium chloride, cetyl pyridinium ammonium chloride etc. are prepared on antibacterial fiber material as compounds such as antiseptic and polyvinyl alcohol, activated carbon fiber, PLAs, but all do not study epsilon-polylysine and polyvinyl alcohol compound prepares anti-bacterial fibre, there is essential distinction with this patent.
Summary of the invention
The object of this invention is to provide a kind of preparation method with the epsilon-polylysine polyvinyl alcohol biological composite antibacterial fiber of good antibiotic property, the present invention, by adding the method for biological preservative epsilon-polylysine, makes the bacteriostasis rate of epsilon-polylysine polyvinyl alcohol biological composite antibacterial fiber more than 97%.
The technical scheme that the present invention realizes object is: adopt water-DMSO system during preparation, the volume ratio of water and DMSO is 6: 4 ~ 2: 8, add the NaCl of 1 ~ 3% in mixed liquor, in the spin solvent mixed, add epsilon-polylysine, stir and epsilon-polylysine is dissolved completely.Take the PVA (degree of polymerization 1750 ± 50) of 8 ~ 20%, add under room temperature in spinning solution, stirring makes it fully to touch solvent, stop stirring rear standing immersion 30 ~ 60min, then be placed in water-bath and heat, progressively be warming up to 60 ~ 70 DEG C, keep 1 ~ 2h, then being warming up to 95 ~ 100 DEG C makes PVA dissolve completely, dissolve the complete 2 ~ 3h that is incubated again and can carry out spray silk, the condensation bath absolute methanol of-20 DEG C, condensation time 10 ~ 60s, in condensation being bathed, anti-bacterial fibre takes out drying at room temperature and can obtain spun.Spun becomes by stretching the anti-bacterial fibre product that diameter is 0.005 ~ 0.1mm.Advantage of the present invention and good effect are: the present invention by adding biological preservative epsilon-polylysine in fiber manufacturing process, and the control group bacteriostasis rate more not adding epsilon-polylysine reaches more than 97%.
Detailed description of the invention
Below by specific embodiment, the invention will be further described, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
Embodiment 1:
A preparation method for epsilon-polylysine polyvinyl alcohol composite fiber, step is as follows:
Adopt water-DMSO system when preparing during preparation, the volume ratio of water and DMSO is 6: 4, adds the NaCl of 3% in mixed liquor, adds the epsilon-polylysine of 0.5%, shake up and epsilon-polylysine is dissolved completely in the spin solvent mixed.Take the PVA (degree of polymerization 1750 ± 50) of 18%, add under normal temperature in spin solvent, stirring makes it fully to touch solvent, stops stirring rear standing swelling 60min, is then placed in water-bath and heats, progressively be warming up to 70 DEG C, keep 1h, be then warming up to 95 ~ 100 DEG C and PVA dissolved completely, dissolve complete be incubated 2h again after carry out spray silk, the condensation bath absolute methanol of-20 DEG C, condensation time 15s.Contrast is not for adding the process of epsilon-polylysine, and other condition is consistent with embodiment 1, and the biological composite fibre bacteriostasis rate of epsilon-polylysine polyvinyl alcohol prepared by embodiment 1 is 97.1%.
Embodiment 2:
A preparation method for the biological composite fibre of epsilon-polylysine polyvinyl alcohol, step is as follows:
Adopt water-DMSO system when preparing during preparation, the volume ratio of water and DMSO is 5: 5, adds the NaCl of 2% in mixed liquor, adds the epsilon-polylysine of 1%, shake up and epsilon-polylysine is dissolved completely in the spin solvent mixed.Take the PVA (degree of polymerization 1750 ± 50) of 15%, add under normal temperature in spin solvent, stirring makes it fully to touch solvent, stops stirring rear leaving standstill and soaks 30min, be then placed in water-bath and heat, progressively be warming up to 65 DEG C, keep 1h, be then warming up to 95 ~ 100 DEG C and PVA is dissolved completely, dissolve the complete 2h that is incubated again and carry out spray silk, the condensation bath absolute methanol of-20 DEG C, condensation time 25s.
Contrast is not for adding the process of epsilon-polylysine, and other condition is consistent with embodiment 2, and the biological composite fibre bacteriostasis rate of epsilon-polylysine polyvinyl alcohol prepared by embodiment 2 is 97.6%.
Embodiment 3:
A preparation method for the biological composite fibre of epsilon-polylysine polyvinyl alcohol, step is as follows:
Adopt water-DMSO system when preparing during preparation, the volume ratio of water and DMSO is 4: 6, adds the NaCl of 1% in mixed liquor, adds the epsilon-polylysine of 1.2%, shake up and epsilon-polylysine is dissolved completely in the spin solvent mixed.Take the PVA (degree of polymerization 1750 ± 50) of 10%, add under normal temperature in spin solvent, stirring makes it fully to touch solvent, stops stirring rear leaving standstill and soaks 30min, be then placed in water-bath and heat, progressively be warming up to 70 DEG C, keep 1h, be then warming up to 95 ~ 100 DEG C and PVA is dissolved completely, dissolving the complete 2h that is incubated again can carry out spray silk, the condensation bath absolute methanol of-20 DEG C, condensation time 60s.
Contrast is not for adding the process of epsilon-polylysine, and other condition is consistent with embodiment 3, and the biological composite fibre bacteriostasis rate of epsilon-polylysine polyvinyl alcohol prepared by embodiment 3 is 98.4%.
Claims (1)
1. the preparation method of epsilon-polylysine polyvinyl alcohol (PVA) composite antibacterial fibre, water-DMSO system is adopted during preparation, the volume ratio of water and DMSO is 6: 4 ~ 2: 8, the NaCl of 1 ~ 3% is added in mixed liquor, adding 0.1 ~ 2% degree of polymerization in the spin solvent mixed is the epsilon-polylysine of 10 ~ 35, stirs and epsilon-polylysine is dissolved completely; Take the PVA that 8 ~ 20% degree of polymerization are 1750 ± 50, add under room temperature in spinning solution, stirring makes it fully to touch solvent, stop stirring rear standing immersion 30 ~ 60min, then be placed in water-bath and heat, be progressively warming up to 60 ~ 70 DEG C, keep 1 ~ 2h, then being warming up to 95 ~ 100 DEG C makes PVA dissolve completely, and dissolving the complete 2 ~ 3h that is incubated again can carry out spray silk; The condensation bath absolute methanol of-20 DEG C, condensation time 10 ~ 60s, in condensation being bathed, anti-bacterial fibre takes out drying at room temperature and can obtain spun.
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| CN105332093A (en) * | 2015-01-03 | 2016-02-17 | 浙江理工大学 | Bionic composite micro-nanofiber with filter and absorption dual functions and preparation method of bionic composite micro-nanofiber |
| CN105771421A (en) * | 2016-03-09 | 2016-07-20 | 仙桃永利医疗用品有限公司 | Non-woven composite material for filter respirator |
| CN107059156B (en) * | 2017-04-13 | 2018-06-05 | 广州市中诚新型材料科技有限公司 | A kind of far-infrared polyester fiber |
| CN107469154B (en) * | 2017-08-10 | 2020-07-17 | 北京大清生物技术股份有限公司 | Bionic artificial cartilage material with antibacterial activity and preparation method thereof |
| CN111441101B (en) * | 2020-06-10 | 2023-04-07 | 合肥工业大学 | Preparation method of PLGA/epsilon-PL antibacterial nano fiber |
| CN111691008A (en) * | 2020-07-14 | 2020-09-22 | 福建恒安集团有限公司 | Preparation method of antibacterial and antiviral protective material |
| CN112848439A (en) * | 2021-01-04 | 2021-05-28 | 许胜强 | Production process of antibacterial medical gloves |
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| JPH1136136A (en) * | 1997-07-11 | 1999-02-09 | Kuraray Co Ltd | Antibacterial polyvinyl alcohol fiber, its production and construction |
| CN1403641A (en) * | 2002-10-14 | 2003-03-19 | 中国石油化工集团公司 | Water soluble polyvinyl alcohol fiber and its prepn and use |
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