CN109537281A - A kind of manufacturing method of antibacterial fabric - Google Patents

A kind of manufacturing method of antibacterial fabric Download PDF

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Publication number
CN109537281A
CN109537281A CN201811475822.XA CN201811475822A CN109537281A CN 109537281 A CN109537281 A CN 109537281A CN 201811475822 A CN201811475822 A CN 201811475822A CN 109537281 A CN109537281 A CN 109537281A
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polylactic acid
antibacterial
organic solvent
acid polymer
polymer composite
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不公告发明人
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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
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03—Polysaccharides or derivatives thereof
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • 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
    • D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic System
    • D06M11/42—Oxides or hydroxides of copper, silver or gold
    • 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
    • D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/55—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 sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
    • D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 of the Periodic System
    • 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
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • D06M13/228—Cyclic esters, e.g. lactones
    • 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
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03—Polysaccharides or derivatives thereof
    • D06M15/05—Cellulose or derivatives thereof
    • D06M15/09—Cellulose ethers
    • 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
    • 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
    • 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
    • D06M2101/34—Polyamides

Abstract

A kind of manufacturing method of antibacterial fabric, it is characterised in that: the following steps are included: the preparation of step 1. antimicrobial fluid；The manufacture of step 2. antibacterial substrate；Step 3. filtering shaping.

Description

A kind of manufacturing method of antibacterial fabric
The application is entitled a kind of manufacturing method of anti-biotic material application No. is 201610386898X, the applying date For the divisional application of the application for a patent for invention of 2016.06.02.
Technical field
The present invention relates to a kind of manufacturing methods of antibacterial fabric.
Background technique
Anti-biotic material refers to that itself has a kind of new function material killed or inhibit microbial function.It is led in medical treatment There is extremely wide application prospect in the fields such as domain, household supplies, household electrical appliance, food packaging, in people to environmental sanitation requirement Increasing today, the application of anti-biotic material is by more extensive concern.Current antibiotic finish technology mainly has three classes 1. co-blended spinning method: first antibacterial agent being added in spinning material, anti-bacterial fibre is made, antibacterial fabric is then made.The method antibacterial Effect is lasting, and washability is good, but with high content of technology, and difficulty is big, and it is wide to be related to field, and antibacterial agent requires high；It is commonly used to production synthesis Fiber product.2. finishing method: antibacterial agent (being commonly referred to as antibacterial finishing agent) is added during fabric printing final finishing, Then various antibacterial fabrics are made.The method working process is relatively simple, and washability and durable antibacterial effect are poor.3. Antibacterial agent: being first added in spinning material and anti-bacterial fibre be made by composite finishing method, is added during fabric printing final finishing Then antibacterial fabric is made in antibacterial finishing agent, this method only uses in the specialities with high antibacterial performance requirement, Limit use scope.Current method all cannot concurrently reach the performance of air-moisture-permeable, Durable antibacterial.
Summary of the invention
In order to solve the above problem, the invention adopts the following technical scheme:
The preparation of step 1. antimicrobial fluid
The first step, the methylated cellulose aqueous solution and mass percent concentration that preparation mass percent concentration is 5-10% respectively are The copper-bath of 8-11%, it is spare；
Second step in Xiang Shangshu copper salt solution, is slowly added to chitosan, and keep micro- under microwave concussion or high-speed stirred Wave concussion or high-speed stirred 30-120min, obtain mixed solution A；Wherein, mass fraction of the chitosan in mixed solution A For 7-10%；
Third step, under ultrasonic oscillation or high-speed stirred, the ratio of 7 ︰, 4 ~ 5 ︰ 9, above-mentioned mixed solution A is delayed by volume Slowly it is added in above-mentioned methylated cellulose aqueous solution；
Then, at 40 DEG C, in the ratio for being 1 ︰ 1.2 with the molar ratio of copper ion, ascorbic acid is added and reacts 30 ~ 45min, so It is that 2-3% pectin, 5-8% sodium alginate obtain mixed liquor that mass fraction is added afterwards, then by the de-bubble of gained liquid negative pressure, stand, It is aged 36h again, obtains antimicrobial fluid；
The manufacture of step 2. antibacterial substrate
1) mass ratio is dissolved in organic solvent for 1: 1~50 polylactic acid and thermoplastic polymer and forms spinning solution；
2) polylactic acid thermoplastic polymer spinning solution is placed in electrostatic spinning machine syringe, under 8~30kV voltage, in connecing It receives and obtains polylactic acid polymer composite cellulosic membrane on electrode；
3) organic solvent is removed under 50~100 DEG C of vacuum condition, obtains polylactic acid polymer composite cellulosic membrane；
Thermoplastic polymer in preparation method step 1) provided by the invention be polyether ketone ketone, polyether-ether-ketone, polyetherimide, Polysulfones, polyether sulfone, phenolphthalein modified poly (ether-sulfone), polyphenylene sulfide, polyphenylene oxide or polyamide.
Organic solvent in preparation method step 1) provided by the invention is tetrahydrofuran, dichloroethanes, tetrachloroethanes, two Chloromethanes, chloroform, n,N-Dimethylformamide, n,N-dimethylacetamide or N, N- dimethyl pyrrolidone.
Receiving electrode in preparation method step 2) provided by the invention between emission electrode at a distance from be 8~23cm.
Polylactic acid polymer composite fibre made from electrostatic spinning machine is straight in preparation method step 2) provided by the invention Diameter is 10~50nm.
Polylactic acid polymer composite cellulosic membrane obtained with a thickness of 5~50 in preparation method step 3) provided by the invention μm, width is 5~40cm.
Step 3. filtering shaping
The antibacterial gel liquid of polylactic acid polymer composite fibre membrane filtration step 1, filtration yield every square centimeter made from step 2 For 3-9ml, bottom is filtered at room temperature using suction filtration machine, and suction filtration machine is moved back and forth with 1-2 points ms/min of speed, Filtration time is 1-2 hour, passes through 160~180 DEG C of drying tunnels after the completion of filtering, retention time 15 minutes, drying tunnel was after cooling out It is made.
Compared with the latest prior art, technical solution provided by the invention has the advantages that
1) polylactic acid polymer composite cellulosic membrane provided by the invention is conducive to when polyurethane heats because it is with porous structure in layer Between flowing, improve the uniformity of material internal structure；
2) polylactic acid polymer composite cellulosic membrane is because it with porous structure ensure that the gas permeability of material is excellent；
3) using methylcellulose as continuous phase, doping deposition nano cuprous oxide, prepare good biocompatibility, good permeability, The excellent composite antibacterial film medical material of anti-microbial property.
4) gas permeability of product, good water absorption have quick antibacterial and Durable antibacterial performance good.
5) process flow is short, technology controlling and process is easy, low production cost.
Specific embodiment
Embodiment 1
The preparation of step 1. antimicrobial fluid
The first step, the methylated cellulose aqueous solution and mass percent concentration that preparation mass percent concentration is 5% respectively are 8% Copper-bath, it is spare；
Second step in Xiang Shangshu copper salt solution, is slowly added to chitosan, and keep micro- under microwave concussion or high-speed stirred Wave concussion or high-speed stirred 30-120min, obtain mixed solution A；Wherein, mass fraction of the chitosan in mixed solution A It is 10%；
Third step, under ultrasonic oscillation or high-speed stirred, the ratio of 7 ︰ 4, above-mentioned mixed solution A is slowly added by volume Enter into above-mentioned methylated cellulose aqueous solution；
Then, at 40 DEG C, in the ratio for being 1 ︰ 1.2 with the molar ratio of copper ion, ascorbic acid is added and reacts 45min, then Addition mass fraction is 2-3% pectin, 5-8% sodium alginate obtains mixed liquor, then by the de-bubble of gained gel negative pressure, standing, then It is aged 36h, obtains antimicrobial fluid；
The preparation of step 2. antibacterial substrate
1) mass ratio is dissolved in organic solvent for 1: 1~50 polylactic acid and polyamide and forms spinning solution；
2) polylactic acid thermoplastic polymer spinning solution is placed in electrostatic spinning machine syringe, under 8~30kV voltage, in connecing It receives and obtains polylactic acid polymer composite cellulosic membrane on electrode；
3) organic solvent is removed under 50~100 DEG C of vacuum condition, obtains polylactic acid polymer composite cellulosic membrane；
Step 3. filtering shaping
The antimicrobial fluid of polylactic acid polymer composite fibre membrane filtration step 1 made from step 2, filtration yield every square centimeter are 3- 9ml, bottom are filtered using suction filtration machine, and suction filtration machine is moved back and forth with 1-2 points ms/min of speed, and filtration time is 1-2 hours, the composite cellulosic membrane of polyurethane resin is attached with after the completion of filtering by 160 DEG C of drying tunnels, retention time 15 minutes, out Drying tunnel is made after cooling.
Embodiment 2
The preparation of step 1. antimicrobial fluid
The first step, the methylated cellulose aqueous solution and mass percent concentration that preparation mass percent concentration is 10% respectively are 11% copper-bath, it is spare；
Second step in Xiang Shangshu copper salt solution, is slowly added to chitosan, and keep micro- under microwave concussion or high-speed stirred Wave concussion or high-speed stirred 120min, obtain mixed solution A；Wherein, mass fraction of the chitosan in mixed solution A is 10%；
Third step, under ultrasonic oscillation or high-speed stirred, the ratio of 7 ︰ 4, above-mentioned mixed solution A is slowly added by volume Enter into above-mentioned methylated cellulose aqueous solution；
Then, at 40 DEG C, in the ratio for being 1 ︰ 1.2 with the molar ratio of copper ion, ascorbic acid is added and reacts 45min, then Addition mass fraction is 2-3% pectin, 5-8% sodium alginate obtains mixed liquor, then by the de-bubble of gained gel negative pressure, standing, then It is aged 36h, obtains antimicrobial fluid；
The preparation of step 2. antibacterial substrate
1) mass ratio is dissolved in tetrahydrofuran for 1: 1~50 polylactic acid and polysulfones and forms spinning solution；
2) polylactic acid thermoplastic polymer spinning solution is placed in electrostatic spinning machine syringe, under 8~30kV voltage, in connecing It receives and obtains polylactic acid polymer composite cellulosic membrane on electrode；
3) organic solvent is removed under 50~100 DEG C of vacuum condition, obtains polylactic acid polymer composite cellulosic membrane；
Step 3. filtering shaping
The antimicrobial fluid of polylactic acid polymer composite fibre membrane filtration step 1 made from step 2, filtration yield every square centimeter are 3- 9ml, bottom are filtered using suction filtration machine, and suction filtration machine is moved back and forth with 1-2 points ms/min of speed, and filtration time is 1-2 hours, by 130 DEG C of drying tunnels after the completion of filtering, retention time 15 minutes, drying tunnel was made after cooling out.
Comparative example 1
Step 2 base fabric uses polyester superfine fibre film, other steps are the same as embodiment 1.
Comparative example 2
Antimicrobial fluid is by 5~9 parts of chitosan, 0.1~1 part of probenazole, 0.1~3 part of polyethylene glycol, methyl hydantoin in step 1 0.1~2 part of class compound, 2~5 parts of Peracetic acid compositions.Other steps are the same as embodiment 2.
Specific embodiment is tested for the property, using this field traditional test methods, test result is as shown in table 1, real It tests and shows that anti-biotic material of the invention can realize fast onset antibacterial effect and good in the case where keeping fine air permeability Antibacterial durability.
1 anti-biotic material permeability of table
Embodiment 1 Embodiment 2 Comparative example 1 Comparative example 2
Gas permeability (dm3/ min) 2.8 2.7 0.95 0.8
2 anti-biotic material of table does not wash antibiotic rate
Note: antibiotic rate " * * * ":>=99%, " * * ":>=90%, " * ">=50%, "-":<50%
The antibiotic rate of the anti-biotic material after 50 washings of table 3

Claims (5)

1. a kind of manufacturing method of antibacterial fabric, it is characterised in that: the following steps are included: the preparation of step 1. antimicrobial fluid；Step The manufacture of rapid 2. antibacterial substrate；Step 3. filtering shaping.
2. antibacterial fabric as described in claim 1, which is characterized in that specifically comprise the following steps:
The manufacture of antibacterial substrate
1) mass ratio is dissolved in organic solvent for 1: 1~50 polylactic acid and thermoplastic polymer and forms spinning solution；
2) polylactic acid thermoplastic polymer spinning solution is placed in electrostatic spinning machine syringe, under 8~30kV voltage, in connecing It receives and obtains polylactic acid polymer composite cellulosic membrane on electrode；
3) organic solvent is removed under 50~100 DEG C of vacuum condition, obtains polylactic acid polymer composite cellulosic membrane.
3. production method as claimed in claim 2, it is characterised in that: the manufacturing step 1 of substrate) in organic solvent be tetrahydro Furans, dichloroethanes, tetrachloroethanes, methylene chloride, chloroform, n,N-Dimethylformamide, n,N-dimethylacetamide or N, N- dimethyl pyrrolidone.
4. production method as claimed in claim 2, it is characterised in that: receiving electrode between emission electrode at a distance from for 8~ 23cm。
5. production method as claimed in claim 2, it is characterised in that: the compound fibre of polylactic acid polymer made from electrostatic spinning machine The diameter of dimension is 10~50nm.
CN201811475822.XA 2016-06-02 2016-06-02 A kind of manufacturing method of antibacterial fabric Withdrawn CN109537281A (en)

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拉马克瑞斯纳•西拉姆: "《静电纺丝与纳米纤维导论》", 30 September 2012, 东华大学出版社 *

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