CN108823977A - A kind of preparation method of antibacterial PLA non-woven cloth - Google Patents
A kind of preparation method of antibacterial PLA non-woven cloth Download PDFInfo
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- CN108823977A CN108823977A CN201810777703.3A CN201810777703A CN108823977A CN 108823977 A CN108823977 A CN 108823977A CN 201810777703 A CN201810777703 A CN 201810777703A CN 108823977 A CN108823977 A CN 108823977A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M10/02—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 ultrasonic or sonic; Corona discharge
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
Abstract
The present invention provides a kind of preparation methods of antibacterial PLA non-woven cloth, and using a step method of formation in situ, method is simple, easily operated, require reaction condition low.Amine-terminated hyperbranced compound plays the role of reactant, dispersing agent and adhesive, not additional substance.Amino existing for hyperbranched surface can carry out graft reaction with the active group of the PLA fiber surface after plasma treatment.The durability of nano silver PLA nonwoven product obtained is good, high reliablity, non-environmental-pollution, and this antibacterial PLA non-woven cloth can be widely used in medical and health industry.
Description
Technical field
The invention belongs to non-woven processing technique fields, are related to a kind of preparation method of antibacterial PLA non-woven cloth.
Background technique
Acid fiber be using the amyloid agricultural product such as corn, wheat, beet as raw material, after fermented generation lactic acid, then
It is that a kind of raw material can be planted, easily be planted that acid fiber by polylactic, which is made, through polycondensation and melt spinning, and waste in nature can be natural
The synthetic fibers of degradation.The alternative conventional polypropylene melt-blow nonwoven of polylactic acid non-weaving cloth, in terms of health care
Operating coat, operation drape, mask, baby' diaper, sanltary towel, adult incontinence products, isolation clothes, disposable breathing mask,
Gloves etc., it is also possible to make diaper, amenities and other physiological hygiene articles etc..Acid fiber by polylactic has natural antibacterial, but
Antibiotic property is generally poor.
Since polylactic acid fiber surface lacks active group, surface is modified more difficult.
Summary of the invention
Simple the purpose of the invention is to provide a kind of preparation method, at low cost, safety and stability has excellent antibacterial
The preparation method of the PLA non-woven cloth of energy.
To solve the above problems, the technical solution adopted in the present invention is as follows：
A kind of preparation method of antibacterial PLA non-woven cloth, which is characterized in that include the following steps：
PLA non-woven cloth is pre-processed, the first spare PLA non-woven cloth is obtained；
Media processes are carried out to the described first spare PLA non-woven cloth, obtain the second spare PLA non-woven cloth；
Prepare cationic nano-silver solution；
Described second spare PLA non-woven cloth is put into the cationic nano-silver solution and is handled, third is obtained
Spare PLA non-woven cloth；
PLA nano silver non-woven cloth is obtained according to the spare PLA of the third.
Preferably, in the methods described above, PLA non-woven cloth is pre-processed, it is non-woven obtains the first spare PLA
Cloth, including：At the first time with soaked in absolute ethyl alcohol by the PLA non-woven cloth, ultrasound the second time of washing, then it is anti-with ionized water
Multiple cleaning, removes surface impurity, the described first spare PLA non-woven cloth is obtained after drying.
Preferably, in the methods described above, the first time includes：Between 0.5 hour to 2 hours；When described second
Between include：Between 0.2 hour to 1 hour.
Preferably, in the methods described above, media processes are carried out to the described first spare PLA non-woven cloth, obtains second
Spare PLA non-woven cloth, including：
Described first spare PLA non-woven cloth is placed between the electrode plate of atmospheric plasma mixed processing equipment, is applied
Making alive is handled by medium of argon gas；
The power of the apparatus for processing plasma includes 20w~50w, and the processing time is 30 seconds~70 seconds.
Preferably, in the methods described above, the preparation process of the cationic nano-silver solution is as follows：It will be amine-terminated hyperbranced
Fluidized polymer is dissolved in chloroform, obtains the first solution that mass concentration is 20~200g/L；Polyepichlorohydrin-dimethylamine
It is added in first solution, Hyperbranched Polymer with Terminal Amido and polyepichlorohydrin-dimethylamine are according to 3:1~5:1 is opened
Ring reaction, obtains cation-modified Hyperbranched Polymer with Terminal Amido after 50~60 DEG C of vacuum drying；
The modified ultra-branching solution of 2g-10g/L is prepared according to the cation-modified Hyperbranched Polymer with Terminal Amido；
The silver nitrate and sodium borohydride solution that the first concentration is added into the modified ultra-branching solution, it is molten to obtain second
Liquid, so that the content of silver ion is 50-400mg/L in second solution.
Preferably, in the methods described above, the described second spare PLA non-woven cloth is put into cationic nano-silver solution
It is handled, obtains the spare PLA non-woven cloth of third, including：
Described second spare PLA non-woven cloth is put into the cationic nano-silver solution, bain-marie heating, heating temperature
Degree is set as 65-90 DEG C, grafting time 10-60min, obtains the spare PLA non-woven cloth of third.
Preferably, in the methods described above, antibacterial PLA non-woven cloth is obtained according to the spare PLA of the third, including：
The spare PLA non-woven cloth of the third is washed, dried or dried, the antibacterial PLA non-woven cloth is obtained.
Compared with prior art, the beneficial effects of the present invention are：
In the preparation method of antibacterial PLA non-woven cloth provided by the invention, using a step method of formation in situ, method letter
It is single, it is easily operated, reaction condition is required low.Amine-terminated hyperbranced compound plays the role of reactant, dispersing agent and adhesive,
Not additional substance.Amino existing for hyperbranched surface can be with the active group of the PLA fiber surface after plasma treatment
Carry out graft reaction.The durability of nano silver PLA nonwoven product obtained is good, high reliablity, non-environmental-pollution, this anti-
Bacterium PLA non-woven cloth can be widely used in medical and health industry.
Detailed description of the invention
The flow diagram of the preparation method of antibacterial PLA non-woven cloth in Fig. 1 embodiment of the present invention；
Fig. 2 is the nano-Ag particles of antibacterial PLA nonwoven fabric surface growth in the embodiment of the present invention.
Specific embodiment
Invention is further described in detail With reference to embodiment.
The present invention provides a kind of preparation methods of antibacterial PLA non-woven cloth, and as shown in FIG. 1, FIG. 1 is the embodiment of the present invention
The flow diagram of the preparation method of middle antibacterial PLA non-woven cloth.Specifically, shown method includes：Step S101 is non-to PLA
Woven cloths are pre-processed, and the first spare PLA non-woven cloth is obtained；Step S103, to the described first spare PLA non-woven cloth into
Row media processes obtain the second spare PLA non-woven cloth；Step S105 prepares cationic nano-silver solution；Step S107, will
The second spare PLA non-woven cloth, which is put into the cationic nano-silver solution, to be handled, and obtains that the spare PLA of third is non-knits
Make cloth；And step S109, PLA nano silver non-woven cloth is obtained according to the spare PLA of the third.
In above-mentioned steps S101, PLA non-woven cloth is pre-processed, obtains the first spare PLA non-woven cloth, packet
It includes：At the first time with soaked in absolute ethyl alcohol by the PLA non-woven cloth, ultrasound the second time of washing, then it is repeatedly clear with ionized water
It washes, removes surface impurity, the described first spare PLA non-woven cloth is obtained after drying.
Specifically, the first time includes：Between 0.5 hour to 2 hours；Second time includes：It arrives within 0.2 hour
Between 1 hour.
In above-mentioned steps 103, media processes are carried out to the described first spare PLA non-woven cloth, obtain the second spare PLA
Non-woven cloth, including：
Described first spare PLA non-woven cloth is placed between the electrode plate of atmospheric plasma mixed processing equipment, is applied
Making alive is handled by medium of argon gas；
The power of the apparatus for processing plasma includes 20w~50w, and the processing time is 30 seconds~70 seconds.
In above-mentioned steps S105, cationic nano-silver solution is prepared.
Specifically preparation process includes：
Hyperbranched Polymer with Terminal Amido is dissolved in chloroform, the first solution that mass concentration is 20~200g/L is obtained；
Polyepichlorohydrin-dimethylamine is added in first solution, Hyperbranched Polymer with Terminal Amido and Hydrin-diformazan
Amine is according to 3:1~5:1 carries out ring-opening reaction, and cation-modified amine-terminated hyperbrancedization polymerization is obtained after 50~60 DEG C of vacuum drying
Object；
The modified ultra-branching solution of 2g-10g/L is prepared according to the cation-modified Hyperbranched Polymer with Terminal Amido；
The silver nitrate and sodium borohydride solution that the first concentration is added into the modified ultra-branching solution, it is molten to obtain second
Liquid, so that the content of silver ion is 50-400mg/L in second solution.
In above-mentioned steps S107, the described second spare PLA non-woven cloth is put into the cationic nano-silver solution
It is handled, obtains the spare PLA non-woven cloth of third.
Specifically, the described second spare PLA non-woven cloth is put into the cationic nano-silver solution, bain-marie adds
Heat, heating temperature are set as 65-90 DEG C, grafting time 10-60min, obtain the spare PLA non-woven cloth of third.
In above-mentioned steps S109, PLA nano silver non-woven cloth is obtained according to the spare PLA of the third, including：
The spare PLA non-woven cloth of the third is washed, dried or dried, the antibacterial PLA non-woven cloth is obtained.
Next, being illustrated with two specific embodiments.
Embodiment 1
The PLA non-woven cloth (30g/m2) to be processed for having cut out 20 × 10cm of 6g non-woven cloth is placed in dehydrated alcohol
10min is impregnated, ultrasonic washing is then used, to remove the greasy dirt and processing impurity of material surface.It is placed in after washing completely
In clean container, it is placed in baking oven and is dried under the conditions of 65 DEG C.
Corona treatment is carried out to hot wind non-woven material using atmospheric plasma DY-D1K plasma processing.
Equipment uses argon gas for carrier gas, the configuration of capacitance coupling type electrode plate.There are 50s in 50 watts of the power used, processing time.
Hyperbranched Polymer with Terminal Amido is dissolved in chloroform, the solution A that mass concentration is 100g/L is obtained；Polycyclic oxygen
In chloropropane-dimethylamine solution A, Hyperbranched Polymer with Terminal Amido and polyepichlorohydrin-dimethylamine 5:1 carries out ring-opening reaction,
A kind of cation-modified Hyperbranched Polymer with Terminal Amido is obtained after 50 DEG C of vacuum drying.Prepare the modified ultra-branching solution of 4g/L
120ml, the silver nitrate solution and a small amount of reducing agent (not needing reducing agent under high temperature), the content of silver ion that 0.1mol/L is added are
200mg/L。
By step 2, by treated, PLA non-woven cloth is put into cationic nano-silver solution, bain-marie heating, heating temperature
Degree is set as 65 DEG C, grafting time 60min；PLA non-woven cloth after reaction is washed with clear water, it is remaining hydrophilic small to remove
Molecule.Nano silver pla non-woven cloth is obtained after drying.
Embodiment 2
By PLA non-woven cloth after plasma grafting is handled, the modified PLA non-woven cloth in surface is obtained.
Hyperbranched Polymer with Terminal Amido is dissolved in chloroform, the solution A that mass concentration is 100g/L is obtained；Polycyclic oxygen
In chloropropane-dimethylamine solution A, Hyperbranched Polymer with Terminal Amido and polyepichlorohydrin-dimethylamine 4:1 carries out ring-opening reaction,
A kind of cation-modified Hyperbranched Polymer with Terminal Amido is obtained after 60 DEG C of vacuum drying.
The modified PLA non-woven cloth in surface is impregnated into amine-terminated hyperbrancedization solution, bath raio 1:20, temperature is 60 DEG C, when
Between be 30min, obtained after drying amino grafting PAL non-woven cloth.
Amino grafting is non-woven to be immersed in (0.001mol/L) silver nitrate solution, bath raio 1:30, dip time is
20min.Non-woven cloth after silver nitrate dipping passes through 100 DEG C of steam treatment 10min, obtains nano silver PLA non-woven cloth.
The antibacterial uvioresistant cotton fabric that Examples 1 and 2 obtain is tested, anti-microbial property test is referring to FZ/T73023-
The bacteriostasis rate of plant after 2006 concussion flask method test antibiotic finishes, test strain is Gram-negative bacteria Escherichia coli
(E.coli) and gram-positive bacteria staphylococcus aureus (S.aureus).Bacteriostasis rate can achieve 99% or more.
In the preparation method of antibacterial PLA non-woven cloth provided in an embodiment of the present invention, using a step method of formation in situ, side
Method is simple, easily operated, requires reaction condition low.Amine-terminated hyperbranced compound plays reactant, dispersing agent and adhesive
Effect, not additional substance.Amino existing for hyperbranched surface can be with the activity of the PLA fiber surface after plasma treatment
Group carries out graft reaction.The durability of nano silver PLA nonwoven product obtained is good, high reliablity, non-environmental-pollution, this
Kind antibacterial PLA non-woven cloth can be widely used in medical and health industry.
It will be apparent to those skilled in the art that can make various other according to the above description of the technical scheme and ideas
Corresponding change and deformation, and all these changes and deformation all should belong to the protection scope of the claims in the present invention
Within.
Claims (7)
1. a kind of preparation method of antibacterial PLA non-woven cloth, which is characterized in that include the following steps：
PLA non-woven cloth is pre-processed, the first spare PLA non-woven cloth is obtained；
Media processes are carried out to the described first spare PLA non-woven cloth, obtain the second spare PLA non-woven cloth；
Prepare cationic nano-silver solution；
Described second spare PLA non-woven cloth is put into the cationic nano-silver solution and is handled, it is spare to obtain third
PLA non-woven cloth；
PLA nano silver non-woven cloth is obtained according to the spare PLA non-woven cloth of the third.
2. the method as described in claim 1, which is characterized in that pre-processed to PLA non-woven cloth, it is spare to obtain first
PLA non-woven cloth, including：At the first time with soaked in absolute ethyl alcohol by the PLA non-woven cloth, ultrasound the second time of washing, then
It is cleaned repeatedly with ionized water, removes surface impurity, the described first spare PLA non-woven cloth is obtained after drying.
3. method according to claim 2, which is characterized in that the first time includes：Between 0.5 hour to 2 hours；Institute
Stating for the second time includes：Between 0.2 hour to 1 hour.
4. the method as described in claim 1, which is characterized in that media processes are carried out to the described first spare PLA non-woven cloth,
The second spare PLA non-woven cloth is obtained, including：
Described first spare PLA non-woven cloth is placed between the electrode plate of atmospheric plasma mixed processing equipment, electricity is applied
Pressure, is handled by medium of argon gas；
The power of the apparatus for processing plasma includes 20w~50w, and the processing time is 30 seconds~70 seconds.
5. the method according to claim 1, wherein the preparation process of the cationic nano-silver solution is as follows：
Hyperbranched Polymer with Terminal Amido is dissolved in chloroform, the first solution that mass concentration is 20~200g/L is obtained；Polycyclic oxygen
Chloropropane-dimethylamine is added in first solution, and Hyperbranched Polymer with Terminal Amido and polyepichlorohydrin-dimethylamine are according to 3:
1~5:1 carries out ring-opening reaction, obtains cation-modified Hyperbranched Polymer with Terminal Amido after 50~60 DEG C of vacuum drying；
The modified ultra-branching solution of 2g-10g/L is prepared according to the cation-modified Hyperbranched Polymer with Terminal Amido；
The silver nitrate and sodium borohydride solution that the first concentration is added into the modified ultra-branching solution, obtain the second solution, make
The content for obtaining silver ion in second solution is 50-400mg/L.
6. the method as described in claim 1, which is characterized in that the described second spare PLA non-woven cloth is put into cation and is received
It is handled in the silver-colored solution of rice, obtains the spare PLA non-woven cloth of third, including：
Described second spare PLA non-woven cloth is put into the cationic nano-silver solution, bain-marie heating, heating temperature is set
It is set to 65-90 DEG C, grafting time 10-60min, obtains the spare PLA non-woven cloth of third.
7. the method as described in claim 1, which is characterized in that it is non-woven to obtain antibacterial PLA according to the spare PLA of the third
Cloth, including：
The spare PLA non-woven cloth of the third is washed, dried or dried, the antibacterial PLA non-woven cloth is obtained.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111996794A (en) * | 2020-08-28 | 2020-11-27 | 南通大学 | Preparation method of antibacterial polylactic acid non-woven material |
| WO2022188513A1 (en) * | 2021-03-09 | 2022-09-15 | 深圳安吉尔饮水产业集团有限公司 | Antimicrobial polylactic acid material and preparation method therefor |
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| CN111996794A (en) * | 2020-08-28 | 2020-11-27 | 南通大学 | Preparation method of antibacterial polylactic acid non-woven material |
| WO2022188513A1 (en) * | 2021-03-09 | 2022-09-15 | 深圳安吉尔饮水产业集团有限公司 | Antimicrobial polylactic acid material and preparation method therefor |
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