CN105603740B - A kind of antibiotic ultraviolet-resistant bafta and its preparation technology - Google Patents
A kind of antibiotic ultraviolet-resistant bafta and its preparation technology Download PDFInfo
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- CN105603740B CN105603740B CN201610106042.2A CN201610106042A CN105603740B CN 105603740 B CN105603740 B CN 105603740B CN 201610106042 A CN201610106042 A CN 201610106042A CN 105603740 B CN105603740 B CN 105603740B
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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
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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
- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
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Abstract
A kind of antibiotic ultraviolet-resistant bafta and its preparation technology, it is related to antibacterial cotton fabric field, in the preparation technology, the carboxymethyl chitosan of molecular weight≤500,000 is prepared first, then carboxymethyl chitosan solution is prepared using carboxymethyl chitosan, and dipping pretreatment is carried out to raw cotton fabric using carboxymethyl chitosan solution, obtain carboxymethyl chitosan modified cotton fabric；Silver ion absorbing and reducing processing finally is carried out to carboxymethyl chitosan modified cotton fabric using silver ion solution and reducing agent.The present invention adsorbs silver ion using the carboxymethyl chitosan original position of molecular weight≤500,000, and reduces silver ion in surface of cotton fabric, Nano Silver bafta is made, the antibiotic ultraviolet-resistant performance of the Nano Silver bafta is good, and water-wash resistance is good.
Description
Technical field
The present invention relates to antibacterial cotton fabric field, in particular to a kind of antibiotic ultraviolet-resistant bafta and its preparation
Technique.
Background technology
In life, various harmful bacterias are flooded with, various diseases are brought.With carrying for living standards of the people
Height, health and health are increasingly taken seriously, and anti-biotic material and its product increasingly cause the concern of people.
Wherein, silver-colored antibacterial ability is very strong, and the bactericidal effect with wide spectrum, will not produce murder by poisoning in human body accumulation again,
Antibacterial activity material is being used as a long time ago.But silver ion has light sensitivity, it is easy to redox, occur deposition of silver,
Reduction antibacterial activity simultaneously becomes brown or black, influences the outward appearance of product.And nano level metallic silver corpuscle have it is very strong anti-
Bacterium activity, and without light sensitivity, so that antibacterial stability is greatly improved.But nanometer silver granuel is prepared at present
The method of son will typically use the surfactants such as the polymer such as polyvinylpyrrolidone or enuatrol as protective agent,
The organic substance of these non-biocompatibles is difficult to remove, and is easy to be also attached on product when carrying out antimicrobial treatment to product,
Potential toxicity can be caused to human body.
Chitosan is the natural polymer extracted by organism, with good Bc and certain antibacterial effect
Really, and silver ion can be complexed.Zhang Yufei exists《The stability of chitosan nano silver solution and answering on antibiotic finish of the fabric
With》In, chitosan and Nano Silver are compounded to form the Polymer Solution of Nano Silver, then be made into Nano Silver fabric, this side
The stability of Nano Silver prepared by method influences whether the bafta after the Durability of antimicrobial effect of fabric, and general Nano Silver processing not
With anti-ultraviolet property.Bafta after being handled with Nano Silver is by multiple washing, and the silver particles of fabric face adhesion can flow
Lose, so as to reduce the antibacterial effect of fabric.
The content of the invention
It is an object of the invention to provide a kind of antibiotic ultraviolet-resistant bafta and its preparation technology, the technology utilization molecule
The carboxymethyl chitosan original position absorption silver ion of amount≤50 ten thousand, and silver ion is reduced in surface of cotton fabric, Nano Silver cotton is made and knits
Thing, the antibiotic ultraviolet-resistant performance of the Nano Silver bafta is good, and water-wash resistance is good.
The present invention is solved its technical problem and realized using following technical scheme.
The present invention proposes a kind of preparation technology of antibiotic ultraviolet-resistant bafta, and it includes：
Prepare carboxymethyl chitosan, molecular weight≤500,000 of carboxymethyl chitosan；
Carboxymethyl chitosan solution is prepared using carboxymethyl chitosan, and using carboxymethyl chitosan solution to raw cotton fabric
Dipping pretreatment is carried out, carboxymethyl chitosan modified cotton fabric is obtained；And
Carboxymethyl chitosan modified cotton fabric is carried out at silver ion absorbing and reducing using silver ion solution and reducing agent
Reason.
Further, the above-mentioned carboxymethyl chitosan for preparing includes：
By water and isopropanol in mass ratio 1:Chitosan, NaOH, solvent, with solvent is made, are mixed to get mixed liquor by 4, in
Stirring alkalization 1.5h~2.5h, obtains the first solution at 45 DEG C~55 DEG C；
Instill dissolved with chloroacetic aqueous isopropanol, in reacting more than 7h at 45 DEG C~55 DEG C, obtain in the first solution
Second solution；
The molten colloid substance for being located at lower floor in the second solution is collected, deionized water is added in molten colloid substance, is fully stirred
Dissolving is mixed, pH is to neutrality for regulation, obtains the 3rd solution；And
Methanol is added in the 3rd solution, is staticly settled, suction filtration obtains filter residue, filter residue is rinsed with absolute ethyl alcohol, takes out again
Filter, the filter residue that suction filtration again is obtained grinds in being dried in vacuo 1.5h~2.5h at 55 DEG C~65 DEG C and obtains carboxymethyl chitosan.
Further, above-mentioned in the step of the first solution is made, chitosan and NaOH mass ratio are 1：1~1.5, mix
The concentration for closing chitosan in liquid is 0.08g/ml~0.12g/ml.
Further, it is above-mentioned in the step of the second solution is made, dissolved with the monoxone in chloroacetic aqueous isopropanol
Concentration be 0.5g/ml~1g/ml；Volume ratio dissolved with chloroacetic aqueous isopropanol and solvent is 1:4~6.
Further, above-mentioned in the step of three solution is made, the volume ratio of deionized water and solvent is 2~3:1.
Further, it is above-mentioned the step of methanol is added in the 3rd solution in, the volume ratio of methanol and solvent is 4~6:1.
Further, it is above-mentioned that the progress pretreatment of raw cotton fabric is included using carboxymethyl chitosan：Carboxylic is dissolved with distilled water
Methyl chitosan, prepares the carboxymethyl chitosan solution that mass concentration is 0.5%~1.5%；Raw cotton fabric is put into carboxymethyl
In chitosan solution, 0.5h~1.5h is vibrated at room temperature.
Further, above-mentioned silver ion solution is AgNO3Solution, reducing agent is sodium borohydride.
Further, it is above-mentioned using silver ion solution and reducing agent carboxymethyl chitosan modified cotton fabric is carried out silver from
Sub- absorbing and reducing processing includes：
Under the conditions of lucifuge, the AgNO for being 350ppm~450ppm with distilled water configuration concentration3Solution, by carboxymethyl chitosan
Sugared modified cotton fabric is put into AgNO3In solution, 0.5h~1.5h is vibrated at room temperature, silver ion bafta is obtained；
Sodium borohydride is dissolved with distilled water, the reductant solution that concentration is 750ppm~850ppm is made, by silver ion cotton
Fabric is placed in reductant solution, and 20min~30min is vibrated at room temperature, Nano Silver bafta is obtained；And
Nano Silver bafta is taken out and washed, 20min~30min is dried at 75 DEG C~85 DEG C.
The present invention proposes a kind of antibiotic ultraviolet-resistant bafta, is made using above-mentioned preparation technology.
The beneficial effect of the compound of the embodiment of the present invention and the manufacture craft of compound is：
1st, preparation technology of the present invention prepares the carboxymethyl chitosan of molecular weight≤50 first, then prepares carboxymethyl chitosan
Solution, and carboxymethyl chitosan modification is carried out to raw cotton fabric；Finally using silver ion solution and reducing agent to modification
Bafta afterwards carries out silver ion absorbing and reducing processing, obtains antibiotic ultraviolet-resistant bafta.The technology utilization carboxymethyl chitosan
Glycan molecule original position absorption silver ion, and silver ion is reduced in surface of cotton fabric, Nano Silver bafta is made, the Nano Silver bafta
Antibiotic ultraviolet-resistant performance it is good, and water-wash resistance is good.
2nd, preparation technology of the present invention adsorbs silver ion using low molecule amount carboxymethyl chitosan glycan molecule original position, and in bafta
Surface reduction silver ion, the in-situ synthesis of this silver particles is to prepare one of new method of composite, have reduction material into
This, the advantage of process simplification；Bafta is as matrix, with matrix without interfacial reaction in the preparation process of composite,
Matrix surface is pollution-free, and the silver particles size of generation is small, is nanometer-level silver.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional production that can be obtained by commercially available purchase
Product.
The antibiotic ultraviolet-resistant bafta and its preparation technology of the embodiment of the present invention are specifically described below.
The present invention proposes a kind of preparation technology of antibiotic ultraviolet-resistant bafta, and it includes：
The carboxymethyl chitosan of molecular weight≤500,000 is prepared, the viscosity of the carboxymethyl chitosan of molecular weight≤500,000 is smaller；
Carboxymethyl chitosan solution is prepared using carboxymethyl chitosan, and using carboxymethyl chitosan solution to raw cotton fabric
Dipping pretreatment is carried out, carboxymethyl chitosan modified cotton fabric is obtained；And
Carboxymethyl chitosan modified cotton fabric is carried out at silver ion absorbing and reducing using silver ion solution and reducing agent
Reason.Silver ion solution is preferably AgNO3Solution, reducing agent is preferably sodium borohydride.
The present invention reaction principle be：
Bafta is prepared by the less carboxymethyl chitosan of viscosity (carboxymethyl chitosans of molecular weight≤500,000)
After solution dipping, hydroxy functional group present on bafta passes through hydrogen bond and the amino in carboxymethyl chitosan glycan molecule, hydroxyl phase
Interaction, so that by carboxymethyl chitosan solution absorption in surface of cotton fabric.Because carboxymethyl chitosan both carries amino, and band
There is carboxyl, therefore in neutral conditions, the carboxymethyl chitosan of surface of cotton fabric absorption is negatively charged, so that the fibre of bafta
Dimension is negatively charged, the silver ion in absorption silver ion solution, makes silver ion absorption in surface of cotton fabric, then by the reduction of reducing agent
Effect, makes the silver ion reduction of surface of cotton fabric into silver particles, and the silver ion particle of generation is small.And due to carboxymethyl chitosan
The suction-operated of sugar, makes silver particles adsorbed close on bafta.
In the present embodiment, preparing carboxymethyl chitosan includes：
By water and isopropanol in mass ratio 1:Chitosan, NaOH, solvent, with solvent is made, are mixed to get mixed liquor by 4, in
Stirring alkalization 1.5h~2.5h, obtains the first solution at 45 DEG C~55 DEG C；Wherein, chitosan and NaOH mass ratio are 1：1~
1.5, the concentration of chitosan is 0.08g/ml~0.12g/ml in mixed liquor.Chitosan and NaOH mass ratio are preferably 1:
1.35, the concentration of chitosan is preferably 0.1g/ml in mixed liquor.
Instill dissolved with chloroacetic aqueous isopropanol, in reacting more than 7h at 45 DEG C~55 DEG C, obtain in the first solution
Second solution；Wherein, it is 0.5g/ml~1g/ml dissolved with the chloroacetic concentration in chloroacetic aqueous isopropanol；Dissolved with chloroethene
The aqueous isopropanol of acid and the volume ratio of solvent are 1:4~6.It is excellent dissolved with the chloroacetic concentration in chloroacetic aqueous isopropanol
Elect 0.75g/ml as；Volume ratio dissolved with chloroacetic aqueous isopropanol and solvent is preferably 1:5.
The molten colloid substance for being located at lower floor in the second solution is collected, deionized water is added in molten colloid substance, is fully stirred
Dissolving is mixed, pH is to neutrality for regulation, obtains the 3rd solution；Wherein, deionized water and the volume ratio of solvent are 2~3:1, deionized water
Volume ratio with solvent is preferably 2.5:1.
Methanol is added in the 3rd solution, is staticly settled, suction filtration obtains filter residue, filter residue is rinsed with absolute ethyl alcohol, takes out again
Filter, the filter residue that suction filtration again is obtained grinds in being dried in vacuo 1.5h~2.5h at 55 DEG C~65 DEG C and obtains carboxymethyl chitosan.
Wherein, the volume ratio of methanol and solvent is 4~6:1, the volume ratio of methanol and solvent is preferably 5:1.
In the present embodiment, carrying out pretreatment to raw cotton fabric using carboxymethyl chitosan includes：Carboxylic first is dissolved with distilled water
Base enclosure glycan, prepares the carboxymethyl chitosan solution that mass concentration is 0.5%~1.5%；Raw cotton fabric is put into carboxymethyl shell
In glycan solution, 0.5h~1.5h is vibrated at room temperature.
In the present embodiment, silver ion is carried out to carboxymethyl chitosan modified cotton fabric using silver ion solution and reducing agent
Absorbing and reducing processing includes：
Under the conditions of lucifuge, the AgNO for being 350ppm~450ppm with distilled water configuration concentration3Solution, by carboxymethyl chitosan
Sugared modified cotton fabric is put into AgNO3In solution, 0.5h~1.5h is vibrated at room temperature, silver ion bafta is obtained；
Sodium borohydride is dissolved with distilled water, the reductant solution that concentration is 750ppm~850ppm is made, by silver ion cotton
Fabric is placed in reductant solution, and 20min~30min is vibrated at room temperature, Nano Silver bafta is obtained；And
Nano Silver bafta is taken out and washed, 20min~30min is dried at 75 DEG C~85 DEG C.
The present invention also proposes a kind of antibiotic ultraviolet-resistant bafta, is made using above-mentioned preparation technology.
The feature and performance to the present invention are described in further detail with reference to embodiments.
Embodiment 1
Embodiment 1 provides a kind of antibiotic ultraviolet-resistant bafta, and its preparation process is as follows：
Prepare the less carboxymethyl chitosan of viscosity：
10g chitosans are weighed to be added in 500mL four-hole boiling flasks, add 13.5gNaOH, add 100ml solvents (water with
Isopropanol presses 1:4 prepare), instilled in after stirring alkalization 2h at 50 DEG C dissolved with the chloroacetic aqueous isopropanol 20ml of 15g, in 0.5h
Drip, in reaction more than 7h at 50 DEG C.Reaction pours out supernatant liquor after terminating, and is added in lower floor's collosol state material
250ml deionized waters, are sufficiently stirred for dissolving, add 10% salt acid for adjusting pH to neutrality, add 500ml methanol, staticly settle,
Suction filtration, and filter residue is rinsed with a large amount of absolute ethyl alcohols, suction filtration, will be dried in vacuo 2h by filtered filter residue at 60 DEG C again again,
Grind and obtain white solid and yellow solid, as carboxymethyl chitosan, after testing, carboxymethyl chitosan made from the present embodiment
The molecular weight of sugar is between 100,000~200,000, and viscosity is small.
Raw cotton fabric is pre-processed using carboxymethyl chitosan：
Take 1g carboxymethyl chitosans to be placed in 250ml conical flask, pour into the dissolving of 100ml distilled water, it is 1% that concentration, which is made,
Carboxymethyl chitosan solution.Then the raw cotton cloth for taking size to be 77cm is placed in above-mentioned conical flask vibrates 1h at room temperature.
Prepare Nano Silver bafta：
Take 0.04gAgNO3It is placed on outside to be surrounded by black packaging and opaque conical flask, pours into 100ml distillations water-soluble
Solution, is made the solution that concentration is 400ppm.The above-mentioned cotton for being soaked with carboxymethyl chitosan is put into and fills AgNO3Solution in,
1h is vibrated at room temperature.Take 0.08g sodium borohydrides to be placed in 250ml conical flask, pour into the dissolving of 100ml distilled water, be made dense
The solution for 800ppm is spent, above-mentioned cotton is placed in sodium borohydride solution, 25min is vibrated at room temperature.Take out cotton water
Wash, 25min is dried at 80 DEG C, Nano Silver bafta is obtained, by it marked as d.
Embodiment 2
Embodiment 2 provides a kind of antibiotic ultraviolet-resistant bafta, and its preparation process is as follows：
Prepare the less carboxymethyl chitosan of viscosity：
10g chitosans are weighed to be added in 500mL four-hole boiling flasks, add 10gNaOH, add 125ml solvents (water with it is different
Propyl alcohol presses 1:4 prepare), instilled in after stirring alkalization 1.5h at 45 DEG C dissolved with the chloroacetic aqueous isopropanols of 15.625g
Dripped in 31.25ml, 0.5h, in reaction more than 7h at 45 DEG C.Reaction pours out supernatant liquor after terminating, in lower floor's collosol state
250ml deionized waters are added in material, dissolving is sufficiently stirred for, adds 10% salt acid for adjusting pH to neutrality.Add 500ml first
Alcohol, is staticly settled, suction filtration, and rinses filter residue with a large amount of absolute ethyl alcohols, again suction filtration, will again filtered filter residue at 55 DEG C
1.5h is dried in vacuo, grinding obtains white solid and yellow solid, as carboxymethyl chitosan.
Raw cotton fabric is pre-processed using carboxymethyl chitosan：
Take 0.5g carboxymethyl chitosans to be placed in 250ml conical flask, pour into the dissolving of 100ml distilled water, concentration, which is made, is
0.5% carboxymethyl chitosan solution.Then the raw cotton cloth for taking size to be 77cm is placed in above-mentioned conical flask to be vibrated at room temperature
0.5h。
Prepare Nano Silver bafta：
Take 0.035gAgNO3It is placed on outside to be surrounded by black packaging and opaque conical flask, pours into 100ml distilled water
Dissolving, is made the solution that concentration is 350ppm.The above-mentioned cotton for being soaked with carboxymethyl chitosan is put into and fills AgNO3Solution
In, 0.5h is vibrated at room temperature.0.075g sodium borohydrides are taken to be placed in 250ml conical flask, the distillation for pouring into 100ml is water-soluble
Solution, is made the solution that concentration is 750ppm, above-mentioned cotton is placed in sodium borohydride solution, 20min is vibrated at room temperature.Take
Go out cotton washing, dry 20min at 75 DEG C, Nano Silver bafta is obtained, by it marked as e.
Embodiment 3
Embodiment 3 provides a kind of antibiotic ultraviolet-resistant bafta, and its preparation process is as follows：
Prepare the less carboxymethyl chitosan of viscosity：
10g chitosans are weighed to be added in 500mL four-hole boiling flasks, add 15gNaOH, add 85ml solvents (water with it is different
Propyl alcohol presses 1:4 prepare), instilled in after stirring alkalization 2.5h at 55 DEG C dissolved with the chloroacetic aqueous isopropanol 14ml of 14g, in 0.5h
Drip, in reaction more than 7h at 55 DEG C.Reaction pours out supernatant liquor after terminating, and 250ml is added in the molten colloid substance of lower floor
Deionized water, is sufficiently stirred for dissolving, adds 10% salt acid for adjusting pH to neutrality.500ml methanol is added, is staticly settled, suction filtration,
And filter residue is rinsed with a large amount of absolute ethyl alcohols, suction filtration, will be dried in vacuo 2.5h by filtered filter residue at 65 DEG C again again, grinding
Obtain white solid and yellow solid, as carboxymethyl chitosan.
Raw cotton fabric is pre-processed using carboxymethyl chitosan：
Take 1.5g carboxymethyl chitosans to be placed in 250ml conical flask, pour into the dissolving of 100ml distilled water, concentration, which is made, is
1.5% carboxymethyl chitosan solution.Then the raw cotton cloth for taking size to be 77cm is placed in above-mentioned conical flask to be vibrated at room temperature
1.5h。
Prepare Nano Silver bafta：
Take 0.045gAgNO3It is placed on outside to be surrounded by black packaging and opaque conical flask, pours into 100ml distilled water
Dissolving, is made the solution that concentration is 450ppm.The above-mentioned cotton for being soaked with carboxymethyl chitosan is put into and fills AgNO3Solution
In, 1.5h is vibrated at room temperature.0.085g sodium borohydrides are taken to be placed in 250ml conical flask, the distillation for pouring into 100ml is water-soluble
Solution, is made the solution that concentration is 850ppm, above-mentioned cotton is placed in sodium borohydride solution, 30min is vibrated at room temperature.Take
Go out cotton washing, dry 30min at 85 DEG C, Nano Silver bafta is obtained, by it marked as f.
Embodiment 4
Embodiment 4 provides a kind of antibiotic ultraviolet-resistant bafta, the basic phase of preparation process of its preparation process and embodiment 1
Together, difference is as follows：Carboxymethyl chitosan solution when being pre-processed using carboxymethyl chitosan to raw cotton fabric
Concentration is 2%, Nano Silver bafta is finally made, by it marked as g.
Comparative example 1
Comparative example 1 provides a kind of bafta, and its preparation process is as follows：
The viscosity of the carboxymethyl chitosan of molecular weight >=1,000,000 is larger, uses the carboxymethyl chitosan of molecular weight >=1,000,000
Raw cotton fabric is pre-processed：
Take 1.5g carboxymethyl chitosans to be placed in 250ml conical flask, pour into the dissolving of 100ml distilled water, concentration, which is made, is
1.5% carboxymethyl chitosan solution.Then the raw cotton cloth for taking size to be 77cm is placed in above-mentioned conical flask to be vibrated at room temperature
1.5h。
Take 0.045gAgNO3It is placed on outside to be surrounded by black packaging and opaque conical flask, pours into 100ml distilled water
Dissolving, is made the solution that concentration is 450ppm.The above-mentioned cotton for being soaked with carboxymethyl chitosan is put into and fills AgNO3Solution
In, 1.5h is vibrated at room temperature.0.085g sodium borohydrides are taken to be placed in 250ml conical flask, the distillation for pouring into 100ml is water-soluble
Solution, is made the solution that concentration is 850ppm, above-mentioned cotton is placed in sodium borohydride solution, 30min is vibrated at room temperature.Take
Go out cotton washing, dry 30min at 85 DEG C, obtain bafta, by it marked as c.
Comparative example 2
Comparative example 2 provides a kind of bafta, and its preparation process is as follows：
Take 0.045gAgNO3It is placed on outside to be surrounded by black packaging and opaque conical flask, pours into 100ml distilled water
Dissolving, is made the solution that concentration is 450ppm.Size is put into for 77cm raw cotton cloth and fills AgNO3Solution in, in room temperature
Lower vibration 1.5h.Take 0.085g sodium borohydrides to be placed in 250ml conical flask, pour into 100ml distilled water dissolving, concentration is made
For 850ppm solution, above-mentioned cotton is placed in sodium borohydride solution, 30min is vibrated at room temperature.Cotton washing is taken out,
30min is dried at 85 DEG C, bafta is obtained, by it marked as b.
Comparative example 3
Comparative example 3 provides a kind of bafta, and its preparation process is as follows：
10g chitosans are weighed to be added in 500mL four-hole boiling flasks, add 13.5gNaOH, add 100ml solvents (water with
Isopropanol presses 1:4 prepare), instilled in after stirring alkalization 2h at 50 DEG C dissolved with the chloroacetic aqueous isopropanol 20ml of 15g, in 0.5h
Drip, in reaction more than 7h at 50 DEG C.Reaction pours out supernatant liquor after terminating, and is added in lower floor's collosol state material
250ml deionized waters, are sufficiently stirred for dissolving, add 10% salt acid for adjusting pH to neutrality, add 500ml methanol, staticly settle,
Suction filtration, and filter residue is rinsed with a large amount of absolute ethyl alcohols, suction filtration, will be dried in vacuo 2h by filtered filter residue at 60 DEG C again again,
Grinding obtains white solid and yellow solid, the as less carboxymethyl chitosan of viscosity.
Take 1g carboxymethyl chitosans to be placed in 250ml conical flask, pour into the dissolving of 100ml distilled water, it is 1% that concentration, which is made,
Carboxymethyl chitosan solution.Then the raw cotton cloth for taking size to be 77cm is placed in above-mentioned conical flask vibrates 1h at room temperature,
Bafta is obtained, by it marked as h.
Below by way of the performance of experimental test Nano Silver bafta of the present invention.
1st, influence of the different carboxymethyl chitosans to Pretreatment on Cotton fabric uvioresistant
Bafta a, b, c, d are chosen, wherein a is the raw cotton fabric without any processing；B is without at carboxymethyl chitosan
Reason, the bafta directly handled using silver nitrate and sodium borohydride；C is to be prepared through the less carboxymethyl chitosan pretreatment of viscosity
Nano Silver bafta；The Nano Silver bafta that d prepares for the present invention through the larger carboxymethyl chitosan pretreatment of viscosity,
A, b, c, d uvioresistant value are tested, test result is as shown in the table：
The uvioresistant value of the bafta of the different carboxymethyl chitosan processing of table 1
UPF UPF, Ultraviolet Protection Factor, represent bafta protectiving ultraviolet
Ability, its numerical value shows that more greatly its anti-ultraviolet effect is better.As can be seen from the above table, raw cotton fabric a ultraviolet-resistent property
It is poor, substantially without protection effect.Bafta b without carboxymethyl chitosan processing, its UPF numerical value has one compared with a
Fixed raising, with preferable ultraviolet radiation protective effect.Through molecular weight >=1,000,000 carboxymethyl chitosan (the larger carboxylic of viscosity
Methyl chitosan) pretreatment bafta c ultraviolet-resistent property it is suitable with b ultraviolet-resistent property.Through molecular weight≤500,000 carboxymethyl
The bafta d of chitosan (the less carboxymethyl chitosan of viscosity) pretreatment is compared with former three, and its ultraviolet-resistent property has bright
Aobvious raising, according to the testing standard about bafta resistance to ultraviolet radiation energy, d UPF numerical value has reached 50+, has
There is very excellent protection effect, it can thus be seen that Nano Silver bafta of the present invention belongs to uvioresistant product.
2nd, influence of the carboxymethyl chitosan solution concentration to Nano Silver bafta ultraviolet-resistent property
B is, without carboxymethyl chitosan processing (concentration of carboxymethyl chitosan solution is 0), directly to use silver nitrate and boron
The bafta of sodium hydride processing；E is nanometer prepared by the less carboxymethyl chitosan solution pretreatment of viscosity through concentration 0.5%
Silver-colored bafta；D is Nano Silver bafta prepared by the less carboxymethyl chitosan solution pretreatment of viscosity through concentration 1%；F is
Nano Silver bafta prepared by the less carboxymethyl chitosan solution pretreatment of viscosity through concentration 1.5%；G is through concentration 2%
The Nano Silver bafta for preparing of viscosity less carboxymethyl chitosan solution pretreatment, test b, e, d, f, g uvioresistant
Value, test result is as shown in the table：
Influence of the different carboxymethyl chitosan solution concentration of table 2 to bafta uvioresistant
As can be seen from the above table, with the increase of the carboxymethyl chitosan solution concentration for pretreatment, on bafta
UPF values are also increased as, and when carboxymethyl chitosan solution concentration is 1%, UPF values can reach maximum, continue to increase carboxymethyl
Chitosan solution concentration, UPF values have dropped on the contrary, but their anti-ultraviolet UPF values all reach 50+, illustrate using viscous
Spending the less obtained bafta of carboxymethyl chitosan solution pretreatment all has very excellent ultraviolet radiation protective effect, i.e., originally
The anti-ultraviolet property of invention Nano Silver bafta is excellent, especially with the less carboxymethyl chitosan of viscosity that concentration is 1%
The uvioresistant performance of the obtained Nano Silver bafta of sugar juice pretreatment is optimal.
3rd, the water-wash resistance of Nano Silver bafta
By Nano Silver bafta d by multiple washing, and test the anti-of after the washing of different number of times Nano Silver bafta d
Ultraviolet value, test result is as shown in the table：
Ultraviolet-resistent property of the Nano Silver bafta of table 3 after the washing of different number of times
As can be seen from the above table, Nano Silver bafta is not after washing 5 times compared with before washing, and UPF values have declined, still
It is still the uvioresistant product with excellent protection effect.After washing 10 times compared with washing 5 times, UPF values do not change substantially,
But after washing 20 times, compared with washing 10 times, UPF values rise on the contrary.It was found from the result that Nano Silver bafta is washed, nanometer
Silver-colored bafta is after 20 times are washed, although specific UPF values have declined, still all in 50+, illustrates that the present invention prepares work
The uvioresistant performance of Nano Silver bafta made from skill is fine, and water-wash resistance is fine.
4th, the antibiotic property of Nano Silver bafta
Bafta a, h, d, i are chosen, wherein a is the raw cotton fabric without any processing；H is merely through the less carboxylic of viscosity
The bafta of methyl chitosan immersion treatment；D is the Nano Silver prepared through the less carboxymethyl chitosan pretreatment of viscosity
Bafta, i is the Nano Silver bafta that Nano Silver bafta d is obtained after 20 times.
By strain experimental test a, h, d, i antibiotic property, the test strain used in experiment is：Staphylococcus aureus
Bacterium (Staphylococcus aureus), ATCC 6538, gram-positive bacteria；Escherichia coli (Escherichia coli),
ATCC 25922, Gram-negative bacteria.Staphylococcus aureus (S.aureus) is a kind of gram-positive bacteria, Escherichia coli
(E.coli) it is a kind of Gram-negative bacteria, they are typical pathogenic bacteria, in order to which the Nano Silver cotton prepared in test experience is knitted
The anti-microbial property of thing, is to examine strain according to AATCC147-2004 using staphylococcus aureus and Escherichia coli《Bafta it is anti-
Bacterium property：Parallel streak method》The antibacterial sector width and anti-microbial property of standard testing difference bafta.As a result it is as shown in the table：
Table 4 is inoculated with width of the Escherichia coli to the antibacterial area of different baftas
Table 5 is inoculated with width of the staphylococcus aureus to the antibacterial area of different baftas
Antibacterial width of the Nano Silver bafta i after washing 20 times to Escherichia coli is can be seen that from above-mentioned two table
It is suitable with Nano Silver bafta d antibacterial width, the antibacterial width of staphylococcus aureus has been declined, has illustrated present invention system
The antibacterial effect of Nano Silver bafta has preferable water-wash resistance made from standby technique.
In addition in strain experiment, raw cotton fabric a does not have antibiotic property, and bacterium is overgrowed with around it；Merely through carboxymethyl
Bafta h after chitosan processing overgrows with bacterium in the intersection that bafta is contacted with bacterium, and bafta h does not have antibacterial substantially
Property, reason is：Chitosan has free amine group, in acid condition generation-NH3 +And with antibiotic property, and carboxymethyl chitosan exists
More substitution is there occurs on amino, the content of free amine group is reduced, the antibiotic property of carboxymethyl chitosan is also reduced, so
Through molecular weight≤bafta of 500,000 carboxymethyl chitosan (the less carboxymethyl chitosan of viscosity) processing do not have antibacterial effect,
The water-soluble carboxymethyl chitosan that experimental result and Li little Fang et al. have found almost does not have to staphylococcus aureus and Escherichia coli
There is the result of inhibitory action consistent.Obvious yellowish-brown is presented in Nano Silver bafta d surface, and Nano Silver bafta d has obvious
Antibacterial effect, all without bacterial growth around bafta, have obvious antibacterial area, it was confirmed that preparation technology system of the present invention
The Nano Silver bafta obtained has bacteriostasis property, because Nano Silver particle diameter is small, specific surface area is big, it is easier to be attached to cell membrane
On, cell membrane is destroyed, makes bacterium loss of function.Bafta i has declined in the color of the bafta after 20 times are washed, still
Still there is obvious anti-microbial property, bafta i is better than staphylococcus aureus to the antibiotic property of Escherichia coli.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (8)
1. a kind of preparation technology of antibiotic ultraviolet-resistant bafta, it is characterised in that it includes：
Prepare carboxymethyl chitosan, molecular weight≤500,000 of the carboxymethyl chitosan；
Carboxymethyl chitosan solution is prepared using the carboxymethyl chitosan, and using the carboxymethyl chitosan solution to raw cotton
Fabric carries out dipping pretreatment, obtains carboxymethyl chitosan modified cotton fabric；And
The carboxymethyl chitosan modified cotton fabric is carried out at silver ion absorbing and reducing using silver ion solution and reducing agent
Reason；
The silver ion solution is AgNO3Solution, the reducing agent is sodium borohydride, utilizes the silver ion solution and institute
State reducing agent includes to the carboxymethyl chitosan modified cotton fabric progress silver ion absorbing and reducing processing：
Under the conditions of lucifuge, the AgNO for being 350ppm~450ppm with distilled water configuration concentration3Solution, by the carboxymethyl chitosan
Sugared modified cotton fabric is put into the AgNO3In solution, 0.5h~1.5h is vibrated at room temperature, silver ion bafta is obtained；
With distilled water dissolve sodium borohydride, be made concentration be 750ppm~850ppm the reductant solution, by it is described silver from
Unginned cotton's fabric is placed in the reductant solution, and 20min~30min is vibrated at room temperature, Nano Silver bafta is obtained；And
The Nano Silver bafta is taken out and washed, 20min~30min is dried at 75 DEG C~85 DEG C.
2. the preparation technology of antibiotic ultraviolet-resistant bafta according to claim 1, it is characterised in that prepare the carboxylic first
Base enclosure glycan includes：
By water and isopropanol in mass ratio 1:Chitosan, NaOH, the solvent, with solvent is made, are mixed to get mixed liquor by 4, in
Stirring alkalization 1.5h~2.5h, obtains the first solution at 45 DEG C~55 DEG C；
Instill dissolved with chloroacetic aqueous isopropanol, in reacting more than 7h at 45 DEG C~55 DEG C, obtain in first solution
Second solution；
The molten colloid substance for being located at lower floor in second solution is collected, deionized water is added in the molten colloid substance, fills
Divide stirring and dissolving, pH is to neutrality for regulation, obtains the 3rd solution；And
Methanol is added in the 3rd solution, is staticly settled, suction filtration obtains filter residue, the filter residue is rinsed with absolute ethyl alcohol, then
Secondary suction filtration, the filter residue that suction filtration again is obtained grinds in being dried in vacuo 1.5h~2.5h at 55 DEG C~65 DEG C and obtains the carboxylic first
Base enclosure glycan.
3. the preparation technology of antibiotic ultraviolet-resistant bafta according to claim 2, it is characterised in that be made described the
In the step of one solution, the chitosan and the NaOH mass ratio are 1：1~1.5, chitosan described in the mixed liquor
Concentration be 0.08g/ml~0.12g/ml.
4. the preparation technology of antibiotic ultraviolet-resistant bafta according to claim 2, it is characterised in that be made described the
In the step of two solution, the chloroacetic concentration dissolved with chloroacetic aqueous isopropanol is 0.5g/ml~1g/ml；Institute
The volume ratio stated dissolved with chloroacetic aqueous isopropanol and the solvent is 1:4~6.
5. the preparation technology of antibiotic ultraviolet-resistant bafta according to claim 2, it is characterised in that be made described the
In the step of three solution, the volume ratio of the deionized water and the solvent is 2~3:1.
6. the preparation technology of antibiotic ultraviolet-resistant bafta according to claim 2, it is characterised in that molten the described 3rd
In the step of methanol is added in liquid, the volume ratio of the methanol and the solvent is 4~6:1.
7. the preparation technology of antibiotic ultraviolet-resistant bafta according to claim 1, it is characterised in that utilize the carboxylic first
Base enclosure glycan carries out pretreatment to raw cotton fabric to be included：The carboxymethyl chitosan is dissolved with distilled water, preparing mass concentration is
0.5%~1.5% carboxymethyl chitosan solution；The raw cotton fabric is put into the carboxymethyl chitosan solution,
0.5h~1.5h is vibrated at room temperature.
8. a kind of antibiotic ultraviolet-resistant bafta, it is characterised in that be made using any one of claim 1 to 7 preparation technology.
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| CN107030818B (en) * | 2016-09-28 | 2019-05-21 | 北京林业大学 | A kind of preparation method of mildew-proof flame retarded composite wood modifying agent and improved wood |
| CN106758216B (en) * | 2016-12-02 | 2018-09-14 | 辽东学院 | A kind of antibacterial, the processing method of uvioresistant cotton fabric |
| CN109576980B (en) * | 2017-03-30 | 2021-03-30 | 南通大学 | Ecological environment-friendly antibacterial crease-resistant finishing method for polyester-cotton blended fabric |
| CN107022247B (en) * | 2017-05-08 | 2019-08-06 | 奇瑞汽车股份有限公司 | A kind of preparation method and applications of antibacterial composite coating |
| CN107354738A (en) * | 2017-09-04 | 2017-11-17 | 西南大学 | Chitosan/cotton antibacterial composite fabric is prepared with NMMO |
| CN107503141A (en) * | 2017-09-14 | 2017-12-22 | 苏州经贸职业技术学院 | A kind of antibacterial decontamination dual function fabrics auxiliary agent and preparation method thereof |
| CN110373899B (en) * | 2019-06-27 | 2021-12-07 | 浙江理工大学 | Washable antibacterial cotton fabric and preparation method thereof |
| CN110644231A (en) * | 2019-09-29 | 2020-01-03 | 东华大学 | Antibacterial socks and preparation method thereof |
| CN112813527A (en) * | 2020-12-28 | 2021-05-18 | 江苏品创纺织科技有限公司 | Chitin fiber blended mildew-proof fabric |
| CN113150508B (en) * | 2021-03-31 | 2022-10-14 | 上海久升吸塑有限公司 | Medical tray and preparation method thereof |
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| CN101223887B (en) * | 2008-01-31 | 2011-09-14 | 吴继贤 | Nano silver antimicrobial solution and preparing method thereof |
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