CN102493014A - Epsilon-polylysine and polyvinyl alcohol composite biological antibacterial fiber and preparation method thereof - Google Patents
Epsilon-polylysine and polyvinyl alcohol composite biological antibacterial fiber and preparation method thereof Download PDFInfo
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- CN102493014A CN102493014A CN2011103601285A CN201110360128A CN102493014A CN 102493014 A CN102493014 A CN 102493014A CN 2011103601285 A CN2011103601285 A CN 2011103601285A CN 201110360128 A CN201110360128 A CN 201110360128A CN 102493014 A CN102493014 A CN 102493014A
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Abstract
The invention relates to a preparation method of epsilon-polylysine and polyvinyl alcohol (PVA) composite biological antibacterial fiber. During preparation, a water-DMSO system is adopted; 1-3% of NaCl is added to a mixed liquid; epsilon-polylysine is added to a well mixed spinning solvent; 8-20% of PVA is weighed, and is added to the spinning solvent under room temperature; the mixture is stirred, such that PVA sufficiently contacts the solvent; when stirring is stopped, the mixture is stood and PVA is soaked for 30-60min; the mixture is heated in a water bath; the temperature is gradually increased to 60-70 DEG C, and is maintained for 1-2h; the temperature is then increased to 95-100 DEG C, such that PVA is completely dissolved; when dissolving is finished, the temperature is maintained for 2-3h, such that spinning can be carried out; absolute methanol is adopted in a condensation bath, and a condensation time is 10-60s; antibacterial fiber in the condensation bath is fetched, and is dried under room temperature, such that primary-spun fiber is obtained. The primary-spun fiber can be drawn into an antibacterial fiber product with a diameter of 0.005-0.1mm. With the added epsilon-polylysine, the fiber is provided with good antibacterial activity, and a bacteriostasis rate is above 97%. The fiber can be used in antibacterial fabric production.
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 microbial fermentation, is formed by connecting through α-carboxyl and epsilon-amino 25～35 lysine residues.1977, Shima and Sakai found this seed amino acid polymer first in the fermentation clear liquid of Streptomyces albulus NBRC14147 bacterial strain.Epsilon-polylysine is a kind of polycation polypeptide to the human body safety non-toxic, can suppress gramnegative bacterium, gram-positive bacteria, fungi even some virus, and antimicrobial spectrum is extensive.After through the security of mouse experiment proof epsilon-polylysine, Japan, Korea S, the U.S. etc. national with it as antiseptics for natural food and extensive use.
Polyvinyl alcohol has unique powerful cementability, 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 as polymeric emulsifiers, dispersant and polyvinyl formal, acetal, butyral resin; Paper industry is as the paper product adhesive; The agricultural aspect is used for soil conditioner, agricultural chemicals adheres to synergist and vinal; Also can be used for aspects such as daily cosmetics and high-frequency quenching agent.
According to retrieval, find following pertinent literature and patent.
People such as Fei Yanna 2010 the 24th the paper delivered of volume the 8th phase " material Leader " " preparation of Tea Polyphenols/polylactic acid composite nano fibre film and anti-microbial property research " a kind of employing method of electrostatic spinning is disclosed; Tea Polyphenols is mixed the composite nano-fiber membrane that has anti-microbial property with preparation with PLA; Not only enriched the function of single polylactic acid nano fiber film; Also widened the Application Areas of Tea Polyphenols well, for a new road has been opened up in the research of antibacterial fabric.
Patent 200510024952.8 discloses activated carbon fiber-Nano Silver composite antibiotic material in medical use and preparation method thereof.Material is the Ag that is adsorbed with 200-400mg/pg on the activated carbon fiber.The preparation method adopts gasification to combine activation method to make activated carbon fiber the presoma carbon fiber-containing, makes nano-Ag particles embed fibrous inside through immersing or spray Ag-containing solution and concussion, and processing at last obtains finished product.Not 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 and obtains the regenerated silk acid solution in the acid solution; C. polyvinyl alcohol obtains poly-vinyl alcohol solution after dissolving; D. two kinds of solution blendings; E. add silver-based inorganic salt; F. carry out electrostatic spinning with silver electrode again, obtain the blended nanofibre felt; G. with the heat treatment 2～5 minutes under 100～150 ℃ temperature conditions of blended nanofibre felt, handled 3～5 hours through UV-irradiation again, obtain fibroin albumen and polyvinyl alcohol blending antibacterial nanometer fiber.
Patent CN101189971A " a kind of inorganic/application of organic nano composite antibacterial agent and fibre thereof " disclose a kind of inorganic/application of organic nano composite antibacterial agent and fibre thereof; With 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; By weight carry out processing such as moistening dispersion, grinding, high speed dispersion, stirring with reinforced order, obtain the nanoscale complex antimicrobials.This antiseptic can adopt dip method, tie-dyeing process, spraying process etc. to handle fibre.With of the present invention inorganic/the prepared clothes of organic nano composite antibacterial agent, socks, carpet, bedding, operation dress, johnny, mouth mask, hospital gauze, airstrainer etc.; Have antibiotic rate height, antibacterial action rapidly and characteristics such as anti-microbial property is lasting, wash resistant; Can be used for aspects such as life and medical treatment; Play the prevent disease generation 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 as on the compound preparation anti-bacterial fibre materials such as antiseptic and polyvinyl alcohol, activated carbon fiber, PLA; But all do not study the compound preparation anti-bacterial fibre of epsilon-polylysine and polyvinyl alcohol, have essential distinction with this patent.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method with biological composite antibacterial fibre of epsilon-polylysine polyvinyl alcohol of good antibiotic property; The present invention makes the bacteriostasis rate of the biological composite antibacterial fibre of epsilon-polylysine polyvinyl alcohol surpass 97% through adding the method for biological preservative epsilon-polylysine.
The present invention realizes that the technical scheme of purpose is: adopt water-DMSO system during preparation; The volume ratio of water and DMSO is 6: 4～2: 8; Add 1～3% NaCl in the mixed liquor, add epsilon-polylysine in the spin solvent that mixes, stirring is dissolved epsilon-polylysine fully.Take by weighing 8～20% PVA (degree of polymerization 1750 ± 50), add under the room temperature in the spinning solution, stir and make it fully to touch solvent; Leave standstill after stopping to stir and soak 30～60min, be placed in the water-bath then and heat, progressively be warming up to 60～70 ℃; Keep 1～2h; Be warming up to 95～100 ℃ then PVA is dissolved fully, dissolving finishes and is incubated 2～3h again and can sprays silk, and the absolute methanol with-20 ℃ is bathed in condensation; Condensation time 10～60s takes out drying at room temperature with anti-bacterial fibre in the condensation bath and can obtain spun.Spun can become the anti-bacterial fibre product that diameter is 0.005～0.1mm through stretching.Advantage of the present invention and good effect are: the present invention is through adding the biological preservative epsilon-polylysine in the fiber production process, the control group bacteriostasis rate that does not more add epsilon-polylysine reaches more than 97%.
The specific embodiment
Through specific embodiment the present invention is made further detailed description below, following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
Embodiment 1:
A kind of preparation method of epsilon-polylysine polyvinyl alcohol composite fiber, step is following:
Adopt water-DMSO system when preparing during preparation, the volume ratio of water and DMSO is 6: 4, adds 3% NaCl in the mixed liquor, adds 0.5% epsilon-polylysine in the spin solvent that mixes, and shakes up epsilon-polylysine is dissolved fully.Take by weighing 18% PVA (degree of polymerization 1750 ± 50), normal temperature adds down in the spin solvent, stirs and makes it fully to touch solvent; Leave standstill swelling 60min after stopping to stir, be placed in the water-bath then and heat, progressively be warming up to 70 ℃; Keep 1h, be warming up to 95～100 ℃ then PVA is dissolved fully, dissolving finishes and sprays silk after being incubated 2h again; The absolute methanol with-20 ℃, condensation time 15s are bathed in condensation.Contrast is not for adding the processing of epsilon-polylysine, and other condition is consistent with embodiment 1, and the biological composite fibre bacteriostasis rate of the epsilon-polylysine polyvinyl alcohol of embodiment 1 preparation is 97.1%.
Embodiment 2:
The preparation method of the biological composite fibre of a kind of epsilon-polylysine polyvinyl alcohol, step is following:
Adopt water-DMSO system when preparing during preparation, the volume ratio of water and DMSO is 5: 5, adds 2% NaCl in the mixed liquor, adds 1% epsilon-polylysine in the spin solvent that mixes, and shakes up epsilon-polylysine is dissolved fully.Take by weighing 15% PVA (degree of polymerization 1750 ± 50), normal temperature adds down in the spin solvent, stirs and makes it fully to touch solvent; Leave standstill after stopping to stir and soak 30min, be placed in the water-bath then and heat, progressively be warming up to 65 ℃; Keep 1h, be warming up to 95～100 ℃ then PVA is dissolved fully, dissolving finishes and is incubated 2h again and sprays silk; The absolute methanol with-20 ℃, condensation time 25s are bathed in condensation.
Contrast is not for adding the processing of epsilon-polylysine, and other condition is consistent with embodiment 2, and the biological composite fibre bacteriostasis rate of the epsilon-polylysine polyvinyl alcohol of embodiment 2 preparations is 97.6%.
Embodiment 3:
The preparation method of the biological composite fibre of a kind of epsilon-polylysine polyvinyl alcohol, step is following:
Adopt water-DMSO system when preparing during preparation, the volume ratio of water and DMSO is 4: 6, adds 1% NaCl in the mixed liquor, adds 1.2% epsilon-polylysine in the spin solvent that mixes, and shakes up epsilon-polylysine is dissolved fully.Take by weighing 10% PVA (degree of polymerization 1750 ± 50), normal temperature adds down in the spin solvent, stirs and makes it fully to touch solvent; Leave standstill after stopping to stir and soak 30min, be placed in the water-bath then and heat, progressively be warming up to 70 ℃; Keep 1h, be warming up to 95～100 ℃ then PVA is dissolved fully, dissolving finishes and is incubated 2h again and can sprays silk; The absolute methanol with-20 ℃, condensation time 60s are bathed in condensation.
Contrast is not for adding the processing of epsilon-polylysine, and other condition is consistent with embodiment 3, and the biological composite fibre bacteriostasis rate of the epsilon-polylysine polyvinyl alcohol of embodiment 3 preparations is 98.4%.
Claims (6)
1. the preparation method of an epsilon-polylysine polyvinyl alcohol (PVA) composite antibacterial fibre adopts water-DMSO system during preparation, adds 1～3% NaCl in the mixed liquor, adds epsilon-polylysine in the spin solvent that mixes, spray silk behind the adding PVA mixing.
2. the preparation method of epsilon-polylysine polyvinyl alcohol composite antibacterial fibre according to claim 1; It is characterized in that: adopt water-DMSO system during preparation; The volume ratio of water and DMSO is 6: 4～2: 8; Add 1～3% NaCl in the mixed liquor, add epsilon-polylysine in the spin solvent that mixes, stirring is dissolved epsilon-polylysine fully.
3. the preparation method of epsilon-polylysine polyvinyl alcohol composite antibacterial fibre according to claim 1 is characterized in that: take by weighing 8～20% PVA (degree of polymerization 1750 ± 50), add under the room temperature in the spinning solution; Stirring makes it fully to touch solvent, leaves standstill after stopping to stir and soaks 30～60min, is placed in the water-bath then and heats; Progressively be warming up to 60～70 ℃, keep 1～2h, be warming up to 95～100 ℃ then PVA is dissolved fully; Dissolving finishes and is incubated 2～3h again and can sprays silk; The absolute methanol with-20 ℃ is bathed in condensation, and condensation time 10～60s takes out drying at room temperature with anti-bacterial fibre in the condensation bath and can obtain spun.
4. the preparation method of epsilon-polylysine polyvinyl alcohol composite antibacterial fibre according to claim 1 is characterized in that: the antibacterial activity composition in the said spinning solution prescription is an epsilon-polylysine, and the degree of polymerization of epsilon-polylysine is 10～35.
5. the preparation method of epsilon-polylysine polyvinyl alcohol composite antibacterial fibre according to claim 1 is characterized in that: the epsilon-polylysine addition is 0.1～2%.
6. the preparation method of epsilon-polylysine polyvinyl alcohol composite antibacterial fibre according to claim 1 is characterized in that: the polyvinyl alcohol addition is 8～20%.
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| CN201110360128.5A CN102493014B (en) | 2011-11-15 | 2011-11-15 | A kind of epsilon-polylysine polyvinyl alcohol compound bio anti-bacterial fibre and preparation method thereof |
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| CN201110360128.5A CN102493014B (en) | 2011-11-15 | 2011-11-15 | A kind of epsilon-polylysine polyvinyl alcohol compound bio anti-bacterial fibre and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107059156A (en) * | 2017-04-13 | 2017-08-18 | 广州市中诚新型材料科技有限公司 | A kind of far-infrared polyester fiber |
| CN107469154A (en) * | 2017-08-10 | 2017-12-15 | 北京大清生物技术股份有限公司 | A kind of biomimetic prosthetic cartilage material with antibacterial activity and preparation method thereof |
| CN111441101A (en) * | 2020-06-10 | 2020-07-24 | 合肥工业大学 | Preparation method of P L GA/-P L antibacterial nanofiber |
| 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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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107059156A (en) * | 2017-04-13 | 2017-08-18 | 广州市中诚新型材料科技有限公司 | A kind of far-infrared polyester fiber |
| 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 |
| CN107469154A (en) * | 2017-08-10 | 2017-12-15 | 北京大清生物技术股份有限公司 | A kind of biomimetic prosthetic cartilage material with antibacterial activity and preparation method thereof |
| 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 |
| CN111441101A (en) * | 2020-06-10 | 2020-07-24 | 合肥工业大学 | Preparation method of P L GA/-P L antibacterial nanofiber |
| 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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