CN108203879A - A kind of antibiotic finishing method of the cotton fabric based on sulfydryl-maleimide click chemistry - Google Patents
A kind of antibiotic finishing method of the cotton fabric based on sulfydryl-maleimide click chemistry Download PDFInfo
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- CN108203879A CN108203879A CN201711477193.XA CN201711477193A CN108203879A CN 108203879 A CN108203879 A CN 108203879A CN 201711477193 A CN201711477193 A CN 201711477193A CN 108203879 A CN108203879 A CN 108203879A
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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
- D06M13/322—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 nitrogen
- D06M13/402—Amides imides, sulfamic acids
- D06M13/41—Amides derived from unsaturated carboxylic acids, e.g. acrylamide
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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
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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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
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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
- D06M2101/06—Vegetal fibres cellulosic
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Abstract
The present invention relates to a kind of antibiotic finishing method of the cotton fabric based on sulfydryl maleimide click chemistry, including：Maleic anhydride is dissolved in ethyl acetate, adds in aniline, slaking reaction obtains N phenyl maleic acid monoamides；It is mixed with acetic anhydride, triethylamine, water-bath, cooling and standings, crystalline solid is precipitated, through filtering, washing, drying, obtain N phenyl maleimides；Cotton fabric after cleaning is added in, dipping is sealed in sulfhydryl modified liquid, through washing, baking, obtain sulfhydryl modified cotton fabric；Click chemistry is carried out with the antibiotic finishing solution mixing of the phenyl maleimide containing N to react, drying obtains the cotton fabric of antibiotic finish.The antibiotic finishing method of the present invention has the characteristics that process efficient is simple, reaction condition is mild, the reaction time is short compared to other antibiotic finishing methods.
Description
Technical field
The invention belongs to functional finish of cotton fabric technical fields, more particularly to a kind of to be clicked based on sulfydryl-maleimide
The antibiotic finishing method of the cotton fabric of chemistry.
Background technology
In nature, microorganism there are extremely wide, containing bacterium, virus, fungi etc. in these microorganisms, existing
Grow directly from seeds in living, people unavoidably touch the microorganisms such as all kinds of bacteriums, fungi, virus, and these microorganisms are suitable
Under the conditions of rapidly breed and spread the disease by certain approach, this to people’s lives there are strong influence, especially carefully
Bacterium, substantial amounts seriously affect the health of the mankind.Textile can provide certain moisture, temperature, nutrition to bacterium, significantly
Growth of the bacterium in textile surface is increased, cotton fabric is one kind in cellulose fibre, and cellulose is not one kind in itself
Nutriment, but many bacteriums can manufacture extracellular cellulase, be glucose by cellulose degradation, this will be into one
Step promotes the growth of bacterium and the degradation of fiber, this not only affects the beauty and wearability of textile, but also increases
Probability of the mankind by bacterium infection.
The method for sorting of common cotton fabric antibacterial can be divided into two major class：Co-blended spinning method and finishing method.Blending is spun
Silk method, which generally refers to some, does not have the fiber of reactivity side group, is to add antiseptic in fibrous polymer stage or spinning solution
Enter into fiber, carry out spinning with conventional spinning equipment, can be made and have anti-bacterial fibre.This antibiotic method not only will be anti-
Microbial inoculum is applied to the surface of fiber, but also is dispersed in fiber, and be dispersed in fiber, and antibacterial effect compares
Persistently, fabric feeling is relatively good, but requires antiseptic high temperature resistance good, and grain size is small.Finishing method refers to containing antiseptic
Solution or resin impregnate fabric, pads or coating, spray treatment, by a kind of side of antiseptic fixation on the textile
Method, so that the cotton fabric being organized has antibiotic property, this method is generally used for dyeing and finishing processing final stage and either exists
Cotton fabric is made into being handled again after finished product.Antibacterial fabric is generally divided into two kinds：Dissolution type and non-dissolving type, dissolution type
Textile refers to that antibacterial ring can be formed from diffusion inside to fiber surface, and so as to kill the bacterium in ring, such textile is resistance to
Washing property is poor, is only applicable to disposable soft goods or the fewer textile of washing times；Non-dissolving type textile is usually
Between textile and antiseptic generate chemical reaction antiseptic is grafted on fiber surface and is obtained, between antiseptic and fiber with
Covalent bond or ionic bond mode combine, antiseptic and indiffusion during effect, but can resist the killing bacteria with fiber contacts
Bacterium effect is more long.
As long as textile antimicrobial agent is divided into organic antibacterial agent, inorganic antiseptic and natural antibacterial by the difference of its constituent
Agent three classes, inorganic antiseptic heat resistance is high, easy to use, chemical stability is good, persistence is good；Organic antibacterial agent mainly has quaternary ammonium
Salt, alcohols, phenols and organic metal class, bactericidal effect is strong, and persistence is good, abundance；Natural antibacterial agent is mainly
The extract of natural plants by technology restriction, can not carry out large-scale promotion.
It is learnt by the access of document, the normal heat-proof modifier of related N-phenylmaleimide is more, though it is carried in document
To it with certain antibiotic property, but relevant research is less.
Invention content
The technical problems to be solved by the invention are to provide a kind of cotton fabric based on sulfydryl-maleimide click chemistry
Antibiotic finishing method, after overcoming the pure cotton fabric drying arranged using the antibiotic finishes such as infusion process or padding method method, hand
Feel the shortcomings that harder, clicked between the cotton fabric of the invention by N-phenylmaleimide antiseptic energy and after sulfhydryl modified
Reaction so that N-phenylmaleimide is grafted on cotton fabric, the excellent anti-microbial property of providing cotton fabric, anti-compared to other
Bacterium method for sorting, the present invention in click-reaction have the characteristics that process efficient is simple, reaction condition is mild, the reaction time is short；
And the antiseptic in the present invention is response type antiseptic, can react and firmly be combined on fiber with fabric, is sterilized
Effect is good.
A kind of antibiotic finishing method of cotton fabric based on sulfydryl-maleimide click chemistry of the present invention, including：
(1) maleic anhydride is dissolved in ethyl acetate, aniline is added dropwise, carry out slaking reaction, drying obtains
N- phenyl maleic acid monoamides；Wherein maleic anhydride, ethyl acetate, aniline amount ratio be 10~12g：30~50mL：
8.47~10.14mL；
(2) the N- phenyl maleic acids monoamides that step (1) obtains is mixed with acetic anhydride, triethylamine, water-bath, Ran Houleng
But it stands, crystalline solid is precipitated, through filtering, washing, drying, obtain N-phenylmaleimide；Wherein N- phenyl maleic acids list acyl
Amine, acetic anhydride, triethylamine amount ratio be 8~9g：17.46~18.9mL：3.2~3.46mL；
(3) it is 1 cotton fabric to be placed in bath raio：It is cleaned in 30~50 pretreatment fluid, the cotton fabric after being cleaned；It will contain
Mercaptosilane coupling agents are added in solvent, are adjusted pH=3~4 using acetic acid solution, are obtained sulfhydryl modified liquid；By the cotton after cleaning
It is 1 that fabric, which is placed in bath raio,：In 30~50 sulfhydryl modified liquid, then sealing dipping is washed, is baked, obtains sulfhydryl modified cotton
Fabric；Wherein the dosage containing mercaptosilane coupling agents is 4~6wt% of solvent；
(4) N-phenylmaleimide that step (2) obtains is dissolved in solvent, obtains antibiotic finishing solution, by step (3)
Obtained sulfhydryl modified cotton fabric is by bath raio 1：30~50 room temperature immersions add in catalyst stirring in antibiotic finishing solution, into
Row click chemistry reacts, and drying obtains the cotton fabric of antibiotic finish；Wherein the dosage of N-phenylmaleimide is the 5 of solvent
~10wt%；The dosage of catalyst is 0.5~1wt% of solvent.
The technological parameter of slaking reaction is in the step (1)：Slaking reaction temperature is 24~26 DEG C, the slaking reaction time
For 0.75~1.25h.
The technological parameter of drying is in the step (1)：Drying temperature is 40~60 DEG C, and drying time is 10~30min.
The technological parameter of water-bath is in the step (2)：Water-bath temperature is 50~60 DEG C, the water-bath time
For 0.75~1.25h.
The process conditions of cooling and standings are in the step (2)：Product is placed in the distilled water of ice and stood for 24 hours.
The process conditions washed in the step (2)：Using the distilled water flushing 2~3 times of 100~150mL.
The technological parameter of drying is in the step (2)：Drying temperature is 45~50 DEG C, and drying time is 3~3.5h.
Pretreatment fluid in the step (3) includes 12~15g/L NaOH, 5~7g/L paregal Os, surplus distilled water.
In the step (3) is gamma-mercaptopropyltriethoxysilane KH-580 containing mercaptosilane coupling agents.
Solvent in the step (3) is volume ratio 4：1 ethyl alcohol and water mixed liquid.
The technological parameter of cleaning is in the step (3)：Cleaning temperature is 60~70 DEG C, and scavenging period is 20~30min.
The time of sealing dipping is 2~3min in the step (3).
The technological parameter of baking is in the step (3)：Stoving temperature is 120~125 DEG C, and baking time is 4~6min.
Solvent in the step (4) is acetone.
Catalyst is triethylamine in the step (4).
Stirring is magnetic agitation in the step (4).
The time that chemical reaction is clicked in the step (4) is 0.5~1h.
The technological parameter of drying is in the step (4)：Drying temperature is 60~70 DEG C, and drying time is 5~10min.
The antibiotic finishing method of the present invention is raw material first with maleic anhydride, aniline, and ethyl acetate is as solvent
N- phenyl maleic acid monoamides is synthesized, with the N- phenyl maleic acids monoamides and acetic anhydride prepared under the catalytic action of triethylamine
Synthesize N- phenyl maleimides；Gamma-mercaptopropyltriethoxysilane KH-580 is recycled to carry out cotton fabric sulfhydryl modified, by cotton
Hydroxyl in fabric macromolecular is converted into sulfydryl, finally by N-phenylmaleimide with it is sulfhydryl modified after cotton fabric carry out
So as to the good antibiotic property of providing cotton fabric, traditional antibiotic finish is compensated for through the fabric that this method is handled for click-reaction
The problem of technique feel is poor has further expanded the application range of N-phenylmaleimide.
Advantageous effect
(1) silane coupling agent containing-SH is grafted to cotton fiber surface by the present invention by the method for hydrolytic condensation, obtains cotton
The precursor that mercapto is reacted as click chemistry is obtained, it finally will be previous on the basis of the click-reaction of sulfydryl-maleimide
Synthesized N-phenylmaleimide with it is sulfhydryl modified after cotton fabric react, this reaction in finishing agent pass through with wool fiber
The mode of chemical bonding combines, the excellent anti-microbial property of providing cotton fabric, and the obtained antiseptic in invention is response type antibacterial
Agent can react with fabric and firmly be combined on fiber, and bactericidal effect is good.
(2) antibiotic finishing method of the invention is compared to other antibiotic finishing methods, has that process efficient is simple, reaction item
The features such as part is mild, the reaction time is short.
(3) this invention simplifies the complexities of traditional handicraft, solve anti-using the tradition such as infusion process or padding method
After the pure cotton fabric drying that bacterium finishing technique arranges, it is harder to lead to the problem of feel.
Description of the drawings
Fig. 1 is the antibiotic finishing method schematic diagram of the cotton fabric the present invention is based on sulfydryl-maleimide click chemistry；
Fig. 2 is the infrared spectrum comparison diagram of untreated cotton fabric and the cotton fabric of antibiotic finish in the embodiment of the present invention 1；
Wherein (a) is using the infrared spectrum curve of the cotton fabric of N-phenylmaleimide antibiotic finish, and (b) is untreated cotton
The infrared spectrum curve of fabric；
Fig. 3 is untreated cotton fabric (a), sulfhydryl modified cotton fabric (b), antibiotic finish in the embodiment of the present invention 1
Cotton fabric (c) scanning electron microscope comparison diagram；
Fig. 4 is the antibacterial test figure of the cotton fabric of antibiotic finish in the present invention, and wherein cloth specimen 1 is untreated cotton fabric
Sample, cloth specimen 2,3,4 are respectively the fabric samples through antibiotic finish of the embodiment of the present invention 1~3, and Fig. 4 (a) is golden yellow Portugal
Grape coccobacillus (Gram-negative bacteria) test result, Fig. 4 (b) are Escherichia coli (gram-positive bacteria) test result.
Specific embodiment
With reference to specific embodiment, the present invention is further explained.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) it adds in 50mL ethyl acetate in the three-necked bottle of 250mL and 12g maleic anhydrides, stirring and dissolving uses dropping liquid
10.14mL aniline is slowly added dropwise in funnel, and (25 DEG C) curings 1h, 50 DEG C of dry 30min obtain N- phenyl maleic acids under room temperature
Monoamides.
(2) in the three-necked bottle of 250mL, N- phenyl maleic acids monoamides, 17.46mL that 8.0g steps (1) obtain are added in
Acetic anhydride, the mixing of 3.2mL triethylamines, 60 DEG C of water-bath 1h, in the distilled water for the ice for being subsequently poured into 20mL cooling and standings for 24 hours, analysis
Go out a large amount of yellow needles bodies, filtered, with the distillation water washing of 100mL three times, dry 3h at 50 DEG C, obtain N-
Phenyl maleimide.
(3) it is 13 × 3 cotton fabrics to be placed in bath raio：30 containing 0.45g NaOH, 0.21g paregal Os, 30mL distilled water
Pretreatment fluid in, 70 DEG C cleaning 20min, the cotton fabric after being cleaned；Gamma-mercaptopropyltriethoxysilane KH-580 is added
Enter volume ratio 1：In 4 water and alcohol mixeding liquid, pH=3~4 are adjusted with acetic acid, obtain sulfhydryl modified liquid；By the cotton after cleaning
It is 1 that fabric, which is placed in bath raio,：In 50 sulfhydryl modified liquid, then sealing dipping 3min is cleaned with deionized water, 120 DEG C of high temperature roastings
5min is dried, obtains sulfhydryl modified cotton fabric；Wherein the dosage of KH-580 is water and the 5wt% of alcohol mixeding liquid.
(4) N-phenylmaleimide that step (2) obtains is dissolved in acetone, obtains antibiotic finishing solution, by step (3)
Obtained sulfhydryl modified cotton fabric is by bath raio 1：30 room temperature immersions add in catalyst of triethylamine stirring in antibiotic finishing solution,
Click chemistry reaction 30min is carried out, the cotton fabric of antibiotic finish is obtained through 70 DEG C of drying 5min；Wherein N-phenylmaleimide
Dosage be acetone 5wt%；The dosage of triethylamine is the 0.5wt% of acetone.
Infrared spectrogram test, knot are carried out to the cotton fabric of the untreated cotton fabric in the present embodiment and antibiotic finish
As shown in Fig. 2, wherein (a) is using the infrared spectrum curve of the cotton fabric of N-phenylmaleimide antibiotic finish, (b) is fruit
The infrared spectrum curve of untreated cotton fabric, curve (a) is in 1110cm-1There is peak appearance at place, and has no this in curve (b)
Peak, this maleimide base group indicated that in N-phenylmaleimide occur chemical reaction with-SH and produce C-S keys, this
Outside, curve (a) is in 1709cm-1The stretching vibration peak for having carbonyl occurs, and also shows N-phenylmaleimide and is sent out with cotton fabric
Reaction is given birth to；895cm is found after in curve (a) and curve (b)-1The strong of carbon-carbon double bond on the imide group at place is stretched
Contracting vibration peak disappears, this just illustrates that N-phenylmaleimide takes part in reaction.
The cotton fabric of untreated cotton fabric in the present embodiment, sulfhydryl modified cotton fabric, antibiotic finish is distinguished
Electronic Speculum SEM tests are scanned, the results are shown in Figure 3, wherein the SEM that (a) is untreated cotton fabric schemes, it is seen that fiber table
Face smoother, (b) are that the SEM of sulfhydryl modified cotton fabric schemes, and too big variation, (c) are had no compared to figure (a) fiber surface
The SEM figures of cotton fabric for antibiotic finish, compared with Fig. 3 (a), (b), Fig. 3 (c) surfaces change significantly, and fiber surface has
Many fixation objects, and these substances are exactly N-phenylmaleimide.
Embodiment 2
(1) it adds in 50mL ethyl acetate in the three-necked bottle of 250mL and 12g maleic anhydrides, stirring and dissolving uses dropping liquid
10.14mL aniline is slowly added dropwise in funnel, and (25 DEG C) curings 1h, 50 DEG C of dry 30min obtain N- phenyl maleic acids under room temperature
Monoamides.
(2) in the three-necked bottle of 250mL, N- phenyl maleic acids monoamides, 17.46mL that 8.0g steps (1) obtain are added in
Acetic anhydride, the mixing of 3.2mL triethylamines, 60 DEG C of water-bath 1h, in the distilled water for the ice for being subsequently poured into 20mL cooling and standings for 24 hours, analysis
Go out a large amount of yellow needles bodies, filtered, with the distillation water washing of 100mL three times, dry 3h at 50 DEG C, obtain N-
Phenyl maleimide.
(3) it is 13 × 3 cotton fabrics to be placed in bath raio：30 containing 0.45g NaOH, 0.21g paregal Os, 30mL distilled water
Pretreatment fluid in, 70 DEG C cleaning 20min, the cotton fabric after being cleaned；Gamma-mercaptopropyltriethoxysilane KH-580 is added
Enter volume ratio 1：In 4 water and alcohol mixeding liquid, pH=3~4 are adjusted with acetic acid, obtain sulfhydryl modified liquid；By the cotton after cleaning
It is 1 that fabric, which is placed in bath raio,：In 50 sulfhydryl modified liquid, then sealing dipping 3min is cleaned with deionized water, 120 DEG C of high temperature roastings
5min is dried, obtains sulfhydryl modified cotton fabric；Wherein the dosage of KH-580 is water and the 5wt% of alcohol mixeding liquid.
(4) N-phenylmaleimide that step (2) obtains is dissolved in acetone, obtains antibiotic finishing solution, by step (3)
Obtained sulfhydryl modified cotton fabric is by bath raio 1：40 room temperature immersions add in catalyst of triethylamine stirring in antibiotic finishing solution,
Click chemistry reaction 30min is carried out, the cotton fabric of antibiotic finish is obtained through 70 DEG C of drying 5min；Wherein N-phenylmaleimide
Dosage be acetone 8wt%；The dosage of triethylamine is the 0.5wt% of acetone.
Embodiment 3
(1) it adds in 50mL ethyl acetate in the three-necked bottle of 250mL and 12g maleic anhydrides, stirring and dissolving uses dropping liquid
10.14mL aniline is slowly added dropwise in funnel, and (25 DEG C) curings 1h, 50 DEG C of dry 30min obtain N- phenyl maleic acids under room temperature
Monoamides.
(2) in the three-necked bottle of 250mL, N- phenyl maleic acids monoamides, 17.46mL that 8.0g steps (1) obtain are added in
Acetic anhydride, the mixing of 3.2mL triethylamines, 60 DEG C of water-bath 1h, in the distilled water for the ice for being subsequently poured into 20mL cooling and standings for 24 hours, analysis
Go out a large amount of yellow needles bodies, filtered, with the distillation water washing of 100mL three times, dry 3h at 50 DEG C, obtain N-
Phenyl maleimide.
(3) it is 13 × 3 cotton fabrics to be placed in bath raio：30 containing 0.45g NaOH, 0.21g paregal Os, 30mL distilled water
Pretreatment fluid in, 70 DEG C cleaning 20min, the cotton fabric after being cleaned；Gamma-mercaptopropyltriethoxysilane KH-580 is added
Enter volume ratio 1：In 4 water and alcohol mixeding liquid, pH=3~4 are adjusted with acetic acid, obtain sulfhydryl modified liquid；By the cotton after cleaning
It is 1 that fabric, which is placed in bath raio,：In 50 sulfhydryl modified liquid, then sealing dipping 3min is cleaned with deionized water, 120 DEG C of high temperature roastings
5min is dried, obtains sulfhydryl modified cotton fabric；Wherein the dosage of KH-580 is water and the 5wt% of alcohol mixeding liquid.
(4) N-phenylmaleimide that step (2) obtains is dissolved in acetone, obtains antibiotic finishing solution, by step (3)
Obtained sulfhydryl modified cotton fabric is by bath raio 1：50 room temperature immersions add in catalyst of triethylamine stirring in antibiotic finishing solution,
Click chemistry reaction 30min is carried out, the cotton fabric of antibiotic finish is obtained through 70 DEG C of drying 5min；Wherein N-phenylmaleimide
Dosage be acetone 10wt%；The dosage of triethylamine is the 0.5wt% of acetone.
Embodiment 4
Maleic anhydride, aniline, triethylamine, absolute ethyl alcohol in Examples 1 to 3 have purchased from Chinese medicines group chemical reagent
Limit company；Ethyl acetate, acetic acid are purchased from Shanghai Ling Feng chemical reagent Co., Ltd, paregal O, γ-mercapto propyl-triethoxysilicane
Alkane KH-580 is purchased from the smooth Science and Technology Ltd. of upper Haitai, and agents useful for same is the pure rank of analysis, in use need not be into one
Step purifies, and the Escherichia coli and staphylococcus aureus used in the present embodiment test are voluntarily cultivated for laboratory.
(1) cotton fabric grafting rate：
Using formula G (%)=(M1-M2)/M2× 100% (wherein M1Quality for the cotton fabric before grafting；M2For grafting
The quality of cotton fabric afterwards), the grafting rate of the cotton fabric of antibiotic finish made from calculating Examples 1 to 3, respectively 5.1%,
6.3%th, 10.8%.
(2) antibacterial test：
Antibacterial test is carried out to the cotton fabric of the antibiotic finish in the embodiment of the present invention 1~3, to antibacterial processed fabric
One carried out qualitatively analyzes, and the coating of strain is carried out first on culture medium, then cloth specimen is cut into certain shape again
Shape is affixed on culture medium and is cultivated under appropriate conditions, finally, takes out observation, and the results are shown in Figure 4, wherein
Cloth specimen 1 is untreated fabric samples, and cloth specimen 2,3,4 is respectively the antibiotic finish prepared in the embodiment of the present invention 1,2,3
Fabric samples, Fig. 4 (a) are Staphylococcus aureus bacillus (Gram-negative bacteria) test result, it is seen that are only existed on culture medium
A small number of bacteriums, but bacterium appearance is had no around the cloth specimen 2,3,4 through antibiotic finish, this just illustrates N- benzyl maleimides
Amine has staphylococcus aureus bacillus certain antibacterial ability；Fig. 4 (b) is Escherichia coli (gram-positive bacteria) test knot
Fruit, it is seen that inhibition zone occur around the cloth specimen 2,3,4 through antibiotic finish, this is with regard to apparent explanation through N- phenyl Malaysia
The cotton fabric of acid imide processing has certain antibacterial ability to Escherichia coli.
Claims (9)
1. a kind of antibiotic finishing method of the cotton fabric based on sulfydryl-maleimide click chemistry, including：
(1) maleic anhydride is dissolved in ethyl acetate, aniline is added dropwise, carry out slaking reaction, drying obtains N- benzene
Base maleic acid mono amide；Wherein maleic anhydride, ethyl acetate, aniline amount ratio be 10~12g：30~50mL：8.47
~10.14mL；
(2) the N- phenyl maleic acids monoamides that step (1) obtains is mixed with acetic anhydride, triethylamine, then water-bath cools down quiet
It puts, crystalline solid is precipitated, through filtering, washing, drying, obtain N-phenylmaleimide；Wherein N- phenyl maleic acids monoamides, second
Acid anhydride, triethylamine amount ratio be 8~9g：17.46~18.9mL：3.2~3.46mL；
(3) it is 1 cotton fabric to be placed in bath raio：It is cleaned in 30~50 pretreatment fluid, the cotton fabric after being cleaned；Sulfydryl will be contained
Silane coupling agent is added in solvent, is adjusted pH=3~4 using acetic acid solution, is obtained sulfhydryl modified liquid；By the cotton fabric after cleaning
It is 1 to be placed in bath raio：In 30~50 sulfhydryl modified liquid, then sealing dipping is washed, is baked, obtains sulfhydryl modified cotton fabric；
Wherein the dosage containing mercaptosilane coupling agents is 4~6wt% of solvent；
(4) N-phenylmaleimide that step (2) obtains is dissolved in solvent, obtains antibiotic finishing solution, step (3) is obtained
Sulfhydryl modified cotton fabric press bath raio 1：30~50 room temperature immersions add in catalyst stirring, carry out a little in antibiotic finishing solution
Chemical reaction is hit, drying obtains the cotton fabric of antibiotic finish；Wherein the dosage of N-phenylmaleimide for solvent 5~
10wt%；The dosage of catalyst is 0.5~1wt% of solvent.
2. a kind of antibiotic finish side of cotton fabric based on sulfydryl-maleimide click chemistry according to claim 1
Method, it is characterised in that：The technological parameter of slaking reaction is in the step (1)：Slaking reaction temperature is 24~26 DEG C, and curing is anti-
It is 0.75~1.25h between seasonable；The technological parameter of drying is：Drying temperature is 40~60 DEG C, and drying time is 10~30min.
3. a kind of antibiotic finish side of cotton fabric based on sulfydryl-maleimide click chemistry according to claim 1
Method, it is characterised in that：The technological parameter of water-bath is in the step (2)：Water-bath temperature is 50~60 DEG C, and water-bath is anti-
It is 0.75~1.25h between seasonable；The process conditions of cooling and standings are：Product is placed in the distilled water of ice and stood for 24 hours.
4. a kind of antibiotic finish side of cotton fabric based on sulfydryl-maleimide click chemistry according to claim 1
Method, it is characterised in that：The process conditions washed in the step (2)：Using the distilled water flushing 2~3 times of 100~150mL；It dries
Dry technological parameter is：Drying temperature is 45~50 DEG C, and drying time is 3~3.5h.
5. a kind of antibiotic finish side of cotton fabric based on sulfydryl-maleimide click chemistry according to claim 1
Method, it is characterised in that：Pretreatment fluid in the step (3) includes 12~15g/L NaOH, 5~7g/L paregal Os, surplus and steams
Distilled water.
6. a kind of antibiotic finish of cotton fabric based on sulfydryl-maleimide click chemistry according to claim 1
Method, it is characterised in that：In the step (3) is gamma-mercaptopropyltriethoxysilane KH-580 containing mercaptosilane coupling agents；
Solvent is volume ratio 4：1 ethyl alcohol and water mixed liquid.
7. a kind of antibiotic finish side of cotton fabric based on sulfydryl-maleimide click chemistry according to claim 1
Method, it is characterised in that：The technological parameter of cleaning is in the step (3)：Cleaning temperature is 60~70 DEG C, scavenging period for 20~
30min；The time of sealing dipping is 2~3min；The technological parameter of baking is：Stoving temperature is 120~125 DEG C, baking time
For 4~6min.
8. a kind of antibiotic finish side of cotton fabric based on sulfydryl-maleimide click chemistry according to claim 1
Method, it is characterised in that：Solvent in the step (4) is acetone；Catalyst is triethylamine.
9. a kind of antibiotic finish side of cotton fabric based on sulfydryl-maleimide click chemistry according to claim 1
Method, it is characterised in that：Stirring is magnetic agitation in the step (4)；The time of click chemistry reaction is 0.5~1h；Drying
Technological parameter is：Drying temperature is 60~70 DEG C, and drying time is 5~10min.
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| CN117100621A (en) * | 2023-10-24 | 2023-11-24 | 山东一飞环保材料科技有限公司 | Antibacterial nanofiber dry mask and preparation method thereof |
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| CN117100621B (en) * | 2023-10-24 | 2024-01-09 | 山东一飞环保材料科技有限公司 | Antibacterial nanofiber dry mask and preparation method thereof |
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