CN110172818A - A kind of antibacterial surface method of modifying of non-woven cloth plasma graft shell oligosaccharide derivative - Google Patents
A kind of antibacterial surface method of modifying of non-woven cloth plasma graft shell oligosaccharide derivative Download PDFInfo
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- CN110172818A CN110172818A CN201910368226.XA CN201910368226A CN110172818A CN 110172818 A CN110172818 A CN 110172818A CN 201910368226 A CN201910368226 A CN 201910368226A CN 110172818 A CN110172818 A CN 110172818A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
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- D06M2101/16—Synthetic fibres, other than mineral fibres
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Abstract
The present invention relates to the modified methods of the antibacterial surface of a kind of non-woven cloth plasma grafting chitosan oligosaccharide and its derivative, surface graft material using chitosan oligosaccharide and its derivative as non-woven fabrics, non-woven fabrics is modified by atmospheric air dielectric barrier discharge plasma surface, then with Covalent bonding together chitosan oligosaccharide and its derivative.
Description
Technical field
The invention belongs to a kind of modified methods of the antibacterial surface of non-woven cloth plasma graft shell oligosaccharide derivative, belong to
The technical field of special fibre preparation.
Background technique
Chitosan (Chitosan) is to pass through β -1,4- glucosides key connection by Glucosamine and N-acetylglucosamine
Made of, content is only second to the second largest natural biological polysaccharide of cellulose.Chitosan have biological non-toxicity, can natural degradation
Property, good biocompatibility the features such as, in addition, chitosan also presents certain antibacterial activity, having numerous studies is confirmed, shell
Glycan is able to suppress the growth and breeding of multiple-microorganism.Chitosan oligosaccharide (Chitooligosaccharide) is chitosan main chain through object
The low molecular weight basic amine group oligosaccharides that the degree of polymerization obtained after reason, chemistry or enzyme degradation fracture is 2-10.Chitosan oligosaccharide is in addition to having
Except excellent physiological property possessed by chitosan, compared with chitosan, water-soluble more preferable, function range is wider,
Bioactivity is higher.
Macromolecular fibre non-woven fabrics is widely used in many fields, can be further by modified endowing antibacterial energy
Expand its purposes.Usual anti-bacterial fibre can be prepared by antibacterial agent and high molecular polymer co-blended spinning.But antibacterial
When agent and polymer co-blended spinning, the distribution of fibre-forming condition and antibacterial agent in the fibre is relatively difficult to control.Co-blended spinning
The antibacterial agent of obtained fibrous inside cannot be contacted with bacterium, and a large amount of antibacterial agent does not have antibacterial action, the utilization of antibacterial agent
Low efficiency.In addition, the problems such as inorganic antiseptic (metals such as silver, copper, zinc) is migrated for fiber there is also antibacterial agent, on the one hand anti-
Bacterium effect is not able to maintain good persistence, and on the other hand, the dissolution of inorganic antiseptic is easy to cause secondary pollution to environment.
Summary of the invention
The invention mainly solves the technical problem of providing a kind of tables of non-woven cloth plasma graft shell oligosaccharide derivative
The antibacterial modified method in face.
Technical scheme is as follows:
(1) nonwoven is arranged on plasma device, by plasma jet to nonwoven surface under open environment, is made
Non-woven fabrics moves in plasma atmosphere, and interelectrode distance is 1~3mm, and processing power is 10~100KJ/m2, frequency 20
~50KHz, processing time are 5~30s, and it is modified to generate surface；
(2) plasma treated non-woven fabrics is delivered in chitosan oligosaccharide and its derivatives graft liquid by idler wheel, then
Non-grafted chitosan oligosaccharide and its derivative are removed by squeezing out idler wheel, extrusion pressure is arranged in 1~5bar.Then it will be grafted
Non-woven fabrics is dried under vacuum to constant weight at 40~60 DEG C.
The preparation step of the chitosan oligosaccharide derivative are as follows:
1) chlorine kojic acid synthesizes: kojic acid generates chlorine kojic acid in the case where ice bath reacts with thionyl chloride；
2) the chlorine kojic acid of 1-2mol is dissolved in the chitosan oligosaccharide aqueous solution of 1mol, is reacted while stirring at 25-35 DEG C
It is cooled to room temperature after 3-5h；
3) 20mL acetone is added and enters termination reaction in mixed solution, generates brown precipitate, is then separated by filtration product；
(4) ethyl alcohol soxhlet extraction removes extra acetone, 12h；
(5) finally, being dialysed in distilled water for 24 hours with regenerated cellulose film, the chitosan oligosaccharide-chlorine for being dried to obtain vacuum purification is bent
Acid derivative.
Plasma source in the plasma generator includes the following at least one source of selection: dielectric barrier discharge DBD
Plasma source, surface-discharge SD plasma source, plasmatorch source, arc plasma torch, sliding arc plasma pipe plasma source,
Helical resonator plasma source, microwave plasma source or atmospheric pressure plasma spray the source APPJ.
Plasma in the ion source is selected from He, Ar, Ne, Xe, air, N2、O2、H2O or CO2。
The non-woven fabrics is polyolefin, polyalkenyl halides, polysiloxanes, polyethers, polyamide, polyester, polycarbonate, poly- ammonia
Ester, epoxy resin, polyacrylonitrile, polyacrylic macromolecule, polyphenylene oxide, polyanhydride, poly- a-amino acid, polyphenylene sulfide, polyethers
The blend of one of sulfone or two or more of them；Or degradable macromolecule Poly-L-lactide, poly- (D, L)-lactic acid,
One of polyhydroxybutyrate, polycaprolactone, poly- butyrolactone, poly- valerolactone, polyester dioxane are either at least following
The copolymer of two kinds of monomers: Pfansteihl, D, Pfansteihl, hydroxyacetic acid, 3-hydroxybutyrate, 3- hydroxypentanoic acid, caprolactone, in fourth
The blended non-woven fabrics of ester, valerolactone or two or more of them.
The present invention has the advantages that compared with existing antibacterial modified technology
(1) the advantages that agent of chitosan oligosaccharide derivative antibacterial has non-volatile, and chemical stability is good, highly-safe.Chitosan oligosaccharide spreads out
The modified non-woven fabrics anti-microbial property of biological antibiotic is excellent, has in fields such as high efficiency filter material, biomedical material, protective materials
Broad application prospect.
(2) using plasma graft polymerization, short irradiation, by chitosan oligosaccharide derivative molecular with covalent bonding to nothing
The density of woven fabric fiber surface, antibacterial group is big, and the utilization efficiency of antibacterial agent is high, and anti-microbial property greatly improves, to golden grape
The fungistatic effect of coccus and Escherichia coli is up to 99%.
(3) the modified device therefor investment cost in non-woven fabrics fiber surface is low, invent at low cost, easy to operate, strong applicability,
The advantages that high treating effect, reliable in quality.It is a large amount of to shorten modification time, chemicals usage and product cost are reduced, environment is reduced
Pollution is suitable for industrialized production.
Specific embodiment:
Now in conjunction with embodiment, the invention will be further described:
The preparation step of chitosan oligosaccharide derivative are as follows:
(1) chlorine kojic acid synthesizes: kojic acid generates chlorine kojic acid in the case where ice bath reacts with thionyl chloride；
(2) the chlorine kojic acid of 1-2mol is dissolved in the chitosan oligosaccharide aqueous solution of 1mol, is reacted while stirring at 25-35 DEG C
It is cooled to room temperature after 3-5h；
(3) 20mL acetone is added and enters termination reaction in mixed solution, generates brown precipitate, is then separated by filtration product；
(4) ethyl alcohol soxhlet extraction removes extra acetone；
(5) it is dialysed in distilled water for 24 hours with regenerated cellulose film, the chitosan oligosaccharide-chlorine kojic acid for being dried to obtain vacuum purification spreads out
Biology.
Embodiment 1
(1) nonwoven is arranged on plasma treatment instrument, by plasma jet to nonwoven surface under open environment, is made
Non-woven fabrics moves in plasma atmosphere, interelectrode distance 1mm, processing power 25KJ/m2, frequency 20KHz, processing
Time is 5s, and it is modified to generate surface；
(2) chitosan oligosaccharide for the mass fraction 1.5% that plasma treated non-woven fabrics is delivered to 2g/L by idler wheel is spread out
In biology grafting aqueous solution, non-grafted chitosan oligosaccharide and its derivative then are removed by squeezing out idler wheel, extrusion pressure setting exists
2bar.Then the non-woven fabrics being grafted is dried under vacuum to constant weight at 40 DEG C.
(3) oscillation flask is carried out simultaneously with Escherichia coli (enterobacteriaceae representative), staphylococcus aureus (pyogenic baeceria representative)
Test.Print group count plate 1 × 10 is not added5CFU/mL, and sample oscillation forward backward averaging clump count difference is 4.3% (<
10%), test is effective.Remaining number of viable is counted with colony counting method, is denoted as VS, V is denoted as before processingC.According to place
The difference of front and back is managed, bacteriostasis rate (%)=(V is calculatedC-VS)/Vc × 100%.The Escherichia coli bacteriostasis rate of test group and control group
Difference is 35.3% (> 26%), and the bacteriostasis rate difference of gold-coloured staphylococci is 43.5% (> 26%), illustrates that chitosan oligosaccharide is derivative
Object modification nonwoven cloth has bacteriostasis to Escherichia coli and gold-coloured staphylococci.
Embodiment 2
(1) nonwoven is arranged on plasma device, by plasma jet to nonwoven surface under open environment, is made
Non-woven fabrics moves in plasma atmosphere, interelectrode distance 1.5mm, processing power 45KJ/m2, frequency 26KHz, place
The reason time is 10s, and it is modified to generate surface；
(2) plasma treated non-woven fabrics is delivered to the chitosan oligosaccharide and its derivatives graft liquid of 3g/L by idler wheel
In, non-grafted chitosan oligosaccharide and its derivative then are removed by squeezing out idler wheel, extrusion pressure is arranged in 3bar.It then will grafting
Good non-woven fabrics is dried under vacuum to constant weight at 50 DEG C.
(3) oscillation flask is carried out simultaneously with Escherichia coli (enterobacteriaceae representative), staphylococcus aureus (pyogenic baeceria representative)
Test.Print group count plate 1 × 10 is not added5CFU/mL, and sample oscillation forward backward averaging clump count difference is 4.3% (<
10%), test is effective.Remaining number of viable is counted with colony counting method, is denoted as VS, V is denoted as before processingC.According to place
The difference of front and back is managed, bacteriostasis rate (%)=(V is calculatedC-VS)/Vc × 100%.The Escherichia coli bacteriostasis rate of test group and control group
Difference is 45.3% (> 26%), and the bacteriostasis rate difference of gold-coloured staphylococci is 63.5% (> 26%), illustrates that chitosan oligosaccharide is derivative
Object modification nonwoven cloth has bacteriostasis to Escherichia coli and gold-coloured staphylococci.
Embodiment 3
(1) nonwoven is arranged on plasma device, by plasma jet to nonwoven surface under open environment, is made
Non-woven fabrics moves in plasma atmosphere, interelectrode distance 2mm, processing power 55KJ/m2, frequency 30KHz, processing
Time is 15s, and it is modified to generate surface；
(2) plasma treated non-woven fabrics is delivered to the chitosan oligosaccharide and its derivatives graft liquid of 3g/L by idler wheel
In, non-grafted chitosan oligosaccharide and its derivative then are removed by squeezing out idler wheel, extrusion pressure is arranged in 4bar.It then will grafting
Good non-woven fabrics is dried under vacuum to constant weight at 60 DEG C.
(3) oscillation flask is carried out simultaneously with Escherichia coli (enterobacteriaceae representative), staphylococcus aureus (pyogenic baeceria representative)
Test.Print group count plate 1 × 10 is not added5CFU/mL, and sample oscillation forward backward averaging clump count difference is 4.3% (<
10%), test is effective.Remaining number of viable is counted with colony counting method, is denoted as VS, V is denoted as before processingC.According to place
The difference of front and back is managed, bacteriostasis rate (%)=(V is calculatedC-VS)/Vc × 100%.The Escherichia coli bacteriostasis rate of test group and control group
Difference is 38.5% (> 26%), and the bacteriostasis rate difference of gold-coloured staphylococci is 51.2% (> 26%), illustrates that chitosan oligosaccharide is derivative
Object modification nonwoven cloth is significant to Escherichia coli and gold-coloured staphylococci inhibitory effect.
Claims (5)
1. a kind of non-woven cloth plasma graft shell oligosaccharide derivative antibacterial surface method of modifying, it is characterised in that steps are as follows:
Nonwoven is arranged on plasma device, by plasma jet to nonwoven surface under open environment, makes non-woven fabrics
It is moved in plasma atmosphere, interelectrode distance is 1~3mm, and processing power is 10~100KJ/m2, frequency be 20~
50KHz, processing time are 5~30s, and it is modified to generate surface；
Plasma treated non-woven fabrics is delivered in chitosan oligosaccharide derivatives graft liquid by idler wheel, then by squeezing out idler wheel
Non-grafted chitosan oligosaccharide derivative is removed, extrusion pressure is arranged in 1~5bar, then by the non-woven fabrics being grafted at 40~60 DEG C
Under be dried under vacuum to constant weight.
2. non-woven cloth plasma graft shell oligosaccharide derivative antibacterial surface method of modifying according to claim 1, feature
Be the plasma device plasma source be dielectric barrier discharge DBD plasma source, surface-discharge SD plasma source, etc.
Ion torch source, arc plasma torch, sliding arc plasma pipe plasma source, helical resonator plasma source, microwave plasma
Source or atmospheric pressure plasma spray the source APPJ.
3. the modified side of the antibacterial surface of non-woven cloth plasma grafting chitosan oligosaccharide and its derivative according to claim 2
Method, spy are that the plasma in the plasma source is selected from He, Ar, Ne, Xe, air, N2、O2、H2O or CO2。
4. non-woven cloth plasma graft shell oligosaccharide derivative antibacterial surface method of modifying according to claim 1, spy exists
In the non-woven fabrics be polyolefin, polyalkenyl halides, polysiloxanes, polyethers, polyamide, polyester, polycarbonate, polyurethane, ring
Oxygen resin, polyacrylonitrile, polyacrylic macromolecule, polyphenylene oxide, polyanhydride, poly- a-amino acid, polyphenylene sulfide, in polyether sulfone
One kind or two or more of them blend；Or degradable macromolecule Poly-L-lactide, poly- (D, L)-lactic acid, poly- hydroxyl
One of base butyric acid, polycaprolactone, poly- butyrolactone, poly- valerolactone, polyester dioxane or at least following two
The copolymer of monomer: Pfansteihl, D, Pfansteihl, hydroxyacetic acid, 3-hydroxybutyrate, 3- hydroxypentanoic acid, caprolactone, butyrolactone, penta
The blended non-woven fabrics of lactone or two or more of them.
5. non-woven cloth plasma graft shell oligosaccharide derivative antibacterial surface method of modifying according to claim 1, feature
It is the preparation step of chitosan oligosaccharide derivative are as follows:
(1) chlorine kojic acid synthesizes: kojic acid generates chlorine kojic acid in the case where ice bath reacts with thionyl chloride；
(2) the chlorine kojic acid of 1-2mol is dissolved in the chitosan oligosaccharide aqueous solution of 1mol, reacts 3-5h while stirring at 25-35 DEG C
After be cooled to room temperature；
(3) 20mL acetone is added and enters termination reaction in mixed solution, generates brown precipitate, is then separated by filtration product；
(4) ethyl alcohol soxhlet extraction removes extra acetone；
(5) it is dialysed in distilled water for 24 hours with regenerated cellulose film, is dried to obtain chitosan oligosaccharide-chlorine derivative of kojic acid of vacuum purification.
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| CN110746658A (en) * | 2019-11-05 | 2020-02-04 | 江南大学 | Chitosan/kojic acid/chlorinated kojic acid composite bacteriostatic preservative film and preparation method thereof |
| CN111826943A (en) * | 2020-06-09 | 2020-10-27 | 维达纸业(浙江)有限公司 | A antibacterial non-woven fabrics for panty-shape diapers |
| CN112552538A (en) * | 2020-12-08 | 2021-03-26 | 深圳技术大学 | Polyphenylene sulfide film resisting microbial contamination and preparation method thereof |
| CN114892400A (en) * | 2021-11-01 | 2022-08-12 | 中国电力科学研究院有限公司 | Material surface treatment device and method |
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| CN112552538A (en) * | 2020-12-08 | 2021-03-26 | 深圳技术大学 | Polyphenylene sulfide film resisting microbial contamination and preparation method thereof |
| CN112552538B (en) * | 2020-12-08 | 2022-11-04 | 深圳技术大学 | Polyphenylene sulfide film resisting microbial contamination and preparation method thereof |
| CN114892400A (en) * | 2021-11-01 | 2022-08-12 | 中国电力科学研究院有限公司 | Material surface treatment device and method |
| CN114892400B (en) * | 2021-11-01 | 2023-12-26 | 中国电力科学研究院有限公司 | Material surface treatment device and method |
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