CN114908566B - Virus blocking fabric and preparation method thereof - Google Patents
Virus blocking fabric and preparation method thereof Download PDFInfo
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- CN114908566B CN114908566B CN202210714606.6A CN202210714606A CN114908566B CN 114908566 B CN114908566 B CN 114908566B CN 202210714606 A CN202210714606 A CN 202210714606A CN 114908566 B CN114908566 B CN 114908566B
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- 239000004744 fabric Substances 0.000 title claims abstract description 139
- 241000700605 Viruses Species 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 230000000903 blocking effect Effects 0.000 title claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 title description 2
- 229920000742 Cotton Polymers 0.000 claims abstract description 113
- VKOUCJUTMGHNOR-UHFFFAOYSA-N Diphenolic acid Chemical compound C=1C=C(O)C=CC=1C(CCC(O)=O)(C)C1=CC=C(O)C=C1 VKOUCJUTMGHNOR-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 30
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 29
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims abstract description 28
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims abstract description 28
- 229920001046 Nanocellulose Polymers 0.000 claims abstract description 26
- 239000000835 fiber Substances 0.000 claims abstract description 17
- 230000000840 anti-viral effect Effects 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 13
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 8
- 230000000694 effects Effects 0.000 claims abstract description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 41
- 239000000243 solution Substances 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 230000006378 damage Effects 0.000 claims description 15
- 238000005096 rolling process Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 125000004185 ester group Chemical group 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 230000004584 weight gain Effects 0.000 claims description 6
- 235000019786 weight gain Nutrition 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 108090000565 Capsid Proteins Proteins 0.000 claims description 2
- 102100023321 Ceruloplasmin Human genes 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 230000003612 virological effect Effects 0.000 claims description 2
- 229920003123 carboxymethyl cellulose sodium Polymers 0.000 claims 1
- 229940063834 carboxymethylcellulose sodium Drugs 0.000 claims 1
- 238000007598 dipping method Methods 0.000 claims 1
- 238000000034 method Methods 0.000 claims 1
- 230000002147 killing effect Effects 0.000 abstract description 37
- 229920002678 cellulose Polymers 0.000 abstract description 19
- 239000001913 cellulose Substances 0.000 abstract description 19
- 239000002121 nanofiber Substances 0.000 abstract description 16
- 229910052708 sodium Inorganic materials 0.000 abstract description 4
- 239000011734 sodium Substances 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 4
- 239000000178 monomer Substances 0.000 abstract description 2
- 230000002155 anti-virotic effect Effects 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 238000007689 inspection Methods 0.000 abstract 1
- 102000004169 proteins and genes Human genes 0.000 abstract 1
- 108090000623 proteins and genes Proteins 0.000 abstract 1
- 210000000605 viral structure Anatomy 0.000 abstract 1
- 231100000263 cytotoxicity test Toxicity 0.000 description 15
- 238000002386 leaching Methods 0.000 description 15
- 231100000252 nontoxic Toxicity 0.000 description 15
- 230000003000 nontoxic effect Effects 0.000 description 15
- 230000004048 modification Effects 0.000 description 12
- 238000012986 modification Methods 0.000 description 12
- 230000002829 reductive effect Effects 0.000 description 12
- 238000010521 absorption reaction Methods 0.000 description 11
- 230000010076 replication Effects 0.000 description 10
- 238000009423 ventilation Methods 0.000 description 10
- 238000005886 esterification reaction Methods 0.000 description 7
- 230000035699 permeability Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 230000032050 esterification Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- JOOXCMJARBKPKM-UHFFFAOYSA-N 4-oxopentanoic acid Chemical compound CC(=O)CCC(O)=O JOOXCMJARBKPKM-UHFFFAOYSA-N 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 2
- 244000052769 pathogen Species 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- XKZQKPRCPNGNFR-UHFFFAOYSA-N 2-(3-hydroxyphenyl)phenol Chemical compound OC1=CC=CC(C=2C(=CC=CC=2)O)=C1 XKZQKPRCPNGNFR-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 241000711573 Coronaviridae Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 208000032370 Secondary transmission Diseases 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000531 effect on virus Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229940040102 levulinic acid Drugs 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
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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
- D06M15/05—Cellulose or derivatives thereof
-
- 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
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
-
- 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
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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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- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Engineering & Computer Science (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a virus blocking fabric and a preparation method thereof. The fabric comprises diphenolic acid, sodium carboxymethyl nanocellulose, cellulose nanofiber and cotton fabric. The preparation method of the antiviral fabric comprises the following steps: and (3) sequentially grafting sodium carboxymethyl nanocellulose, cellulose nanofibers and diphenolic acid on the surface of the cotton fabric, and washing and drying to obtain a final product. According to the invention, firstly, exposure of hydroxyl on the surface of the cotton fabric is increased through alkalization treatment, and sodium carboxymethyl cellulose is used as a connection, and nano cellulose fibers are introduced, so that the three-dimensional space on the surface of the cotton fabric has abundant hydroxyl. The anti-virus monomer is diphenolic acid, and the virus structure is destroyed by utilizing the mutual attraction between phenol groups and proteins, so that the effect of killing viruses is achieved. The invention adopts the common dipping-rolling-drying technology in industry to modify cotton fabric, prepares modified cotton fabric with excellent antiviral effect, and can pass the safety inspection.
Description
Technical Field
The invention belongs to the technical field of fabrics, and particularly relates to a virus blocking fabric and a preparation method thereof.
Background
Viruses, including coronaviruses, can survive and spread on a variety of surfaces. Because the stability of the virus varies across different surfaces and may last for several days, the inner layer may remain active for more than 4 days and the outer layer may remain active for more than 7 days in conventional surgical masks. Therefore, these pathogens must be inactivated rapidly, for example, by providing a sterile surface, by contact with the pathogen, minimizing the risk of secondary transmission. Functionalized textiles with self-disinfecting or self-cleaning properties may play a critical role in limiting the transmission of these diseases.
Diphenolic acid is a derivative produced by condensation of phenol and levulinic acid, raw materials can be obtained by decomposing biomass rich in cellulose, and the diphenol is abundant in source, biodegradable and environment-friendly. In the prior report, the diphenolic acid is mostly applied to synthetic resin, and in the prior study, the diphenolic acid has strong killing effect on bacteria, and the diphenolic acid modified antibacterial cotton fabric (patent name: a preparation method of diphenolic acid antibacterial cotton fabric, application number: 202110684232.3, publication (bulletin) number: CN 113445315A) is successfully prepared, but the application of diphenolic acid in antiviral is not found.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide the preparation method of the antiviral cotton fabric, which has the advantages of low cost, simple operation, effective disinfection and environmental friendliness. In order to achieve the aim, the invention adopts the solution that a three-dimensional network structure is constructed on the surface of cotton fabric, the content of hydroxyl is improved, antiviral monomer diphenolic acid is introduced, and the diphenolic acid is connected with cellulose through esterification reaction, so that the antiviral effect of the cotton fabric is endowed. The specific technical scheme is as follows:
a virus blocking fabric is formed by constructing an antiviral functional surface by carboxymethyl cellulose, nano cellulose fiber and diphenolic acid derivative on cotton fiber, wherein the content ranges are 1.5-2.0%, 0.3-0.5% and 1.5-2.0% respectively; the carboxymethyl cellulose molecular chain connects the nano cellulose fiber to the cotton fiber surface through the ester group, a nano cellulose network structure is formed on the cotton fiber surface, the nano cellulose surface is connected with the diphenolic acid molecule through the ester group, and the phenolic hydroxyl functional group of the nano cellulose has adsorption and damage effects on viral capsid protein, so that antiviral activity is formed.
The preparation method of the virus blocking fabric comprises the following steps:
(1) The cotton fabric is soaked in 20-25% sodium hydroxide water solution to activate the hydroxyl functional groups on the surface of the fiber;
(2) After the cotton fabric (1) is rinsed, 1.5-2% of sodium carboxymethyl cellulose aqueous solution is used for soaking treatment for 30 minutes, the weight gain is controlled to be 100-120% by rolling, heating reaction is carried out for 5 minutes at 175-185 ℃, rinsing and drying are carried out;
(3) Soaking the cotton fabric (2) in 0.3-0.5% nano cellulose fiber suspension for 30 min, rolling to control weight gain to 100-120%, heating at 175-185 ℃ for 5 min, rinsing and drying;
(4) The cotton fabric (3) is immersed for 30 minutes by ethanol solution (1.5-2.0%) of diphenolic acid, the weight gain is controlled to be 100-120% by rolling, the cotton fabric is heated and reacted for 5 minutes at 175-185 ℃, and the cotton fabric is rinsed by absolute ethanol and dried after being rinsed by deionized water.
Furthermore, the diphenolic acid is connected with cellulose molecules through ester group covalent bonds by esterification reaction, so that viruses can be effectively killed.
Further, the mass fraction of the ethanol solution of the diphenolic acid is 1.5-2.0%.
According to the preparation method of the diphenolic acid virus blocking cotton fabric, diphenolic acid is firmly connected with the cotton fabric through chemical covalent bonds, so that the preparation method of the antiviral cotton fabric with low cost and simple operation is realized, and the prepared fabric can effectively kill viruses, is comfortable to wear and is harmless to human bodies. In addition, the modification does not cause great damage to the characteristics of the cotton fabric, including moisture absorption, ventilation, softness and the like.
Having an embodiment of
The technical scheme of the invention is further described below with reference to specific examples.
Example 1
The clean cotton fabric is soaked in a sodium hydroxide solution with the mass fraction of 20% for 5 minutes, washed and dried. Then immersing in sodium carboxymethyl cellulose solution with mass fraction of 1.0% for 30 minutes, rolling to gain 100%, heating at 180 ℃ for 5 minutes, washing with deionized water, and drying.
The prepared cotton fabric is formed by cotton fibers and a very small amount of sodium carboxymethyl cellulose, and the result of ATR test is almost identical with that of the original fabric, so that the grafting rate of the sodium carboxymethyl cellulose on the surface of the cotton fibers is influenced by the too low concentration of the sodium carboxymethyl cellulose. The modified fabric has a phage killing effect of almost 0 in 30 minutes and an H1N1 virus inhibiting effect of almost 0. The modification has no influence on the physical properties of cotton fabrics, the tensile strength is about 33.24MPa, and the air permeability is about 621.04g/m 2 /d。
Example 2
The clean cotton fabric is soaked in a sodium hydroxide solution with the mass fraction of 20% for 5 minutes, washed and dried. Then immersing in 2.0% sodium carboxymethyl cellulose solution for 30 minutes, rolling to increase weight by 100%, heating at 180 ℃ for 5 minutes, washing with deionized water, and drying.
The prepared cotton fabric is formed by cotton fibers and sodium carboxymethyl cellulose, and the killing effect on phage is almost zero within 30 minutes, so that the sodium carboxymethyl cellulose has no antiviral effect. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. In addition, the modification does not cause great damage to the characteristics of the cotton fabric, including moisture absorption, ventilation, softness and the like.
Example 3
The clean cotton fabric is soaked in a sodium hydroxide solution with the mass fraction of 20% for 5 minutes, washed and dried. Then immersing in sodium carboxymethyl cellulose solution with mass fraction of 3.0% for 30 minutes, rolling to gain 100%, heating at 180 ℃ for 5 minutes, washing with deionized water, and drying.
The prepared cotton fabric is formed by cotton fibers and sodium carboxymethyl cellulose, and the killing effect on phage is almost zero within 30 minutes, so that the antiviral effect of sodium carboxymethyl nanocellulose can be further determined. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. However, because the concentration of the sodium carboxymethyl cellulose solution is too high, a layer of too thick film is formed on the surface of cotton fiber, the air permeability of the fabric is seriously affected, and the air permeability of the modified fabric is 403.77g/m after test 2 And/d, drop by more than 30%.
Example 4
The modified fabric in example 2 was immersed in a suspension of 0.1% cellulose nanofibers by mass for 30 minutes, rolled to gain 100%, heated at 180 ℃ for 5 minutes, washed with deionized water, and dried.
The prepared cotton fabric is formed by cotton fibers, sodium carboxymethyl cellulose and fewer cellulose nanofibers, and is found to be 1720cm by ATR detection -1 The ester group peak is not obvious, and the grafting amount of the nanocellulose on the surface of the fabric is proved to be small. From SEM images, it can also be seen that only a small amount of nanocellulose fibers on the cotton fiber surface did not reach the purpose of building a three-dimensional network. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. In addition, the modification does not weave cottonThe inherent properties of the article cause significant damage, including moisture absorption, breathability, softness, and the like.
Example 5
The modified fabric in example 2 was immersed in a suspension of 0.5% cellulose nanofibers by mass for 30 minutes, rolled to gain 100%, heated at 180 ℃ for 5 minutes, washed with deionized water, and dried.
The prepared cotton fabric is formed by cotton fiber, sodium carboxymethyl cellulose and cellulose nanofiber, and is found to be 1720cm by ATR detection -1 There is a distinct ester group peak. The killing effect of the fabric on phage is almost zero within 30 minutes, so that the cellulose nanofiber has no antiviral effect. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. In addition, the modification does not cause great damage to the characteristics of the cotton fabric, including moisture absorption, ventilation, softness and the like.
Example 6
The modified fabric in example 2 was immersed in a suspension of cellulose nanofibers with a mass fraction of 1.5% for 30 minutes, rolled to gain 100%, heated at 180 ℃ for 5 minutes, washed with deionized water, and dried.
The prepared cotton fabric is formed by cotton fibers, sodium carboxymethyl cellulose and excessive cellulose nanofibers, and a thick coating formed by the cellulose nanofibers is formed on the surface of the fabric, so that the air permeability of the fabric is affected, and compared with the original fabric, the air permeability of the fabric is reduced by more than 50%. The killing effect of the fabric on phage is almost zero within 30 minutes, so that the nano cellulose rice fiber is determined to have no antiviral effect. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic.
Example 7
The modified fabric in example 5 is immersed in 0.1% diphenolic acid ethanol solution for 30 minutes, rolled to gain 100%, heated for 5 minutes at 180 ℃, washed by absolute ethanol and deionized water, and dried.
The prepared cotton fabric is formed by cotton fibers, sodium carboxymethyl cellulose, cellulose nanofibers and a very small amount of diphenolic acid, and the killing effect on phage within 30 minutes is not more than 30.66%, so that the cotton fabric modified by the scheme cannot be presumed to be capable of effectively killing viruses. Further, when tested with H1N1 virus, the replication of the virus was not significantly reduced within 1 hour, and the virus killing efficiency was not more than 20.21%. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. The three-step modification does not cause great damage to the characteristics of the cotton fabric, including moisture absorption, ventilation, softness and the like.
Example 8
The modified fabric in example 5 is immersed in 0.5% diphenolic acid ethanol solution for 30 minutes, rolled to gain 100%, heated for 5 minutes at 180 ℃, washed by absolute ethanol and deionized water, and dried.
The cotton fabric is made of cotton fiber, sodium carboxymethyl cellulose, cellulose nanofiber and a very small amount of diphenolic acid. The inhibition of the fabric to phage and viruses is enhanced, and the killing effect to phage is not more than 45.20% within 30 minutes, so that the cotton fabric modified by the scheme is presumed to be capable of killing viruses. Further, when tested with H1N1 virus, the replication of the virus was not significantly reduced within 1 hour, and the virus killing efficiency was not more than 35%. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. The three-step modification can not cause great damage to the characteristics of the cotton fabric, including moisture absorption, ventilation, softness and the like.
Example 9
The modified fabric in example 5 is immersed in 1.0% diphenolic acid ethanol solution for 30 minutes, rolled to gain 100%, heated for 5 minutes at 180 ℃, washed by absolute ethanol and deionized water, and dried.
The prepared cotton fabric is formed by cotton fibers, sodium carboxymethyl cellulose, cellulose nanofibers and a small amount of diphenolic acid, and the killing effect of the cotton fabric on phage within 30 minutes is about 70.28 percent, so that the cotton fabric modified by the scheme is presumed to be capable of killing viruses. Further, when tested with H1N1 virus, replication of the virus was reduced within 1 hour, and the virus killing efficiency was about 55.33%. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. The three-step modification can not cause great damage to the characteristics of the cotton fabric, including moisture absorption, ventilation, softness and the like.
Example 10
The modified fabric in example 5 is immersed in 1.5% diphenolic acid ethanol solution for 30 minutes, rolled to gain 100%, heated for 5 minutes at 180 ℃, washed by absolute ethanol and deionized water, and dried.
The prepared cotton fabric is formed by cotton fibers, sodium carboxymethyl cellulose, cellulose nanofibers and diphenolic acid, and the killing effect of the cotton fabric on phage is about 85.56% within 30 minutes, so that the cotton fabric modified by the scheme is presumed to be capable of effectively killing viruses. Further, when tested with H1N1 virus, the replication of the virus was significantly reduced within 1 hour, and the virus killing efficiency was about 75.68%. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. The three-step modification does not cause great damage to the characteristics of the cotton fabric, including moisture absorption, ventilation, softness and the like.
Example 11
The modified fabric in example 5 is immersed in 2.0% diphenolic acid ethanol solution for 30 minutes, rolled to gain 100%, heated for 5 minutes at 180 ℃, washed by absolute ethanol and deionized water, and dried.
The prepared cotton fabric is formed by cotton fibers, sodium carboxymethyl cellulose, cellulose nanofibers and diphenolic acid, and the killing effect of the cotton fabric on phage is about 99.77% within 30 minutes, so that the cotton fabric modified by the scheme is presumed to have a certain virus killing effect. Further, when tested with H1N1 virus, the replication of the virus was significantly reduced within 1 hour, and the virus killing efficiency was about 95.98%. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. The three-step modification can not cause great damage to the characteristics of the cotton fabric, including moisture absorption, ventilation, softness and the like.
Example 12
The modified fabric in example 5 was immersed in a 2.5% by mass of diphenolic acid ethanol solution for 30 minutes, rolled to gain 100%, heated at 180 ℃ for 5 minutes, washed with absolute ethanol and deionized water, and dried.
The prepared cotton fabric is formed by cotton fibers, sodium carboxymethyl cellulose, cellulose nanofibers and a large amount of diphenolic acid, and the killing effect of the cotton fabric on phage exceeds 99.89% within 30 minutes, so that the cotton fabric modified by the scheme is presumed to be capable of effectively killing viruses. Further, when the H1N1 virus is used for testing, the replication of the virus can be obviously reduced within 1 hour, and the virus killing efficiency is about 95.43 percent. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. However, the tensile strength of the modified fabric is severely reduced by only 13.12MPa, while the original fabric exceeds 30MPa.
Example 13
The modified fabric in example 5 was immersed in a 2.0% by mass of diphenolic acid ethanol solution for 30 minutes, rolled to gain 100%, heated at 120 ℃ for 5 minutes, washed with absolute ethanol and deionized water, and dried.
The prepared cotton fabric is formed by cotton fibers, sodium carboxymethyl cellulose, nano cellulose fibers and a very small amount of diphenolic acid, after ATR detection, the ester group peak caused by diphenolic acid is not obvious, the hydroxyl is not obviously increased, and the effect of grafting diphenolic acid cannot be realized at a lower temperature. The killing effect of the fabric on phage in 30 minutes is not more than 25%, so that the cotton fabric modified by the scheme is not supposed to be capable of effectively killing viruses. Further, the test with H1N1 virus failed to reduce the replication of the virus within 1 hour, and the virus killing efficiency was lower than 20%. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. The three-step modification can not cause great damage to the characteristics of the cotton fabric, including moisture absorption, ventilation, softness and the like.
Example 14
The modified fabric in example 5 is immersed in 2.0% diphenolic acid ethanol solution for 30 minutes, rolled to gain 100%, heated for 5 minutes at 200 ℃, washed by absolute ethanol and deionized water, and dried.
The prepared cotton fabric is formed by cotton fibers, sodium carboxymethyl cellulose, nano cellulose fibers and diphenolic acid, and the killing effect of the cotton fabric on phage exceeds 99% within 30 minutes, so that the cotton fabric modified by the scheme is presumed to be capable of killing viruses. Further, when the H1N1 virus is used for testing, the replication of the virus can be reduced within 1 hour, and the virus killing efficiency is more than 95%. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. However, too high an esterification temperature has a great effect on the strength of the fabric, the tensile strength is reduced to 8.11MPa, and the original fabric exceeds 30MPa.
Example 15
The modified fabric in example 5 was immersed in a 2.0% by mass of diphenolic acid ethanol solution for 30 minutes, rolled to gain 100%, heated at 180 ℃ for 1 minute, washed with absolute ethanol and deionized water, and dried.
The prepared cotton fabric is formed by cotton fibers, sodium carboxymethyl cellulose, nano cellulose fibers and a very small amount of diphenolic acid, and the killing effect on phage within 30 minutes is not more than 10.24%, so that the cotton fabric modified by the scheme is supposed to be incapable of killing viruses, the esterification reaction is not completely carried out in too short esterification time, and the diphenolic acid content on the fabric is very low. Further, when tested with H1N1 virus, the replication reduction of the virus was not obvious within 1 hour, and the virus killing efficiency was not more than 6%. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. The modification does not cause great damage to the characteristics of the cotton fabric, including moisture absorption, ventilation, softness and the like.
Example 16
The modified fabric in example 5 was immersed in a 2.0% by mass of diphenolic acid ethanol solution for 30 minutes, rolled to gain 100%, heated at 180 ℃ for 10 minutes, washed with absolute ethanol and deionized water, and dried.
The prepared cotton fabric is formed by cotton fibers, sodium carboxymethyl cellulose, nano cellulose fibers and diphenolic acid, and the killing effect of the cotton fabric on phage exceeds 99.87% within 30 minutes, so that the cotton fabric modified by the scheme is presumed to be capable of effectively killing viruses. Further, when tested by using H1N1 virus, the replication of the virus is obviously reduced within 1 hour, and the virus killing efficiency is more than 95%. The leaching solution of the modified cotton fabric is proved to be harmless to cells after cytotoxicity test, and is safe and nontoxic. However, the high temperature conditions for a long time cause great damage to the physical properties of cotton fabrics, especially in terms of toughness, the tensile strength is reduced to 12.89MPa, whereas the original fabric exceeds 30MPa.
The following table summarises the above examples:
comparing the above 16 examples, the following conclusions are drawn: sodium carboxymethyl nanocellulose and nanocellulose fibers with proper concentrations are necessary conditions for constructing a three-dimensional network on the surface of a fabric, otherwise, the air permeability of the fabric is affected, and the wearing comfort is further affected. The esterification temperature and the concentration of the diphenolic acid can directly influence the antiviral effect, the low temperature or the low concentration of the diphenolic acid can lead the grafting rate of the surface of the fabric to be low, the effect on viruses is limited, the too high temperature, the too long esterification time or the high concentration of the diphenolic acid solution can damage the characteristics of the fabric, and the proper condition is the key for successfully preparing the modified fabric. Thus, the optimal preparation method is as follows: soaking the alkalized cotton fabric in 2% sodium carboxymethyl cellulose solution for 30 min, rolling to increase weight by 100%, heating at 180 ℃ for 5 min, rinsing with deionized water, and drying; immersing the mixture in a nano cellulose fiber suspension with the mass fraction of 0.5% for 30 minutes, heating for 5 minutes at 180 ℃ after rolling and weighting by 100%, rinsing with deionized water, and drying; finally, immersing the fabric in a diphenolic acid ethanol solution with the mass fraction of 2%, maintaining for 30 minutes, increasing the weight by 100% by rolling, heating for 5 minutes at 180 ℃, and then rinsing with absolute ethanol and deionized water in sequence and drying. Finally, the fabric with excellent virus blocking effect is obtained.
Claims (1)
1. A virus blocking fabric is formed by constructing an antiviral function surface by carboxymethylcellulose sodium, nanocellulose fibers and diphenolic acid on cotton fibers, and the preparation method of the virus blocking fabric comprises the following steps:
(1) The cotton fabric is subjected to dipping treatment by using a sodium hydroxide aqueous solution with the mass fraction of 20-25%, and hydroxyl functional groups on the surface of the fiber are activated;
(2) After the cotton fabric (1) is rinsed, soaking the cotton fabric in a sodium carboxymethyl cellulose aqueous solution with the mass fraction of 1.5-2.0% for 30 minutes, rolling to control the weight gain to be 100-120%, heating and reacting for 5 minutes at 175-185 ℃, rinsing and drying;
(3) Soaking the cotton fabric (2) in a nano cellulose fiber suspension with the mass fraction of 0.3-0.5% for 30 minutes, rolling to control the weight gain to be 100-120%, heating and reacting for 5 minutes at 175-185 ℃, rinsing and drying;
(4) Soaking the cotton fabric (3) in 1.5-2.0% diphenolic acid ethanol solution for 30 min, rolling to control weight gain to 100-120%, heating at 175-185 ℃ for 5 min, rinsing with absolute ethanol, rinsing with deionized water, and drying;
the method is characterized in that: the sodium carboxymethyl cellulose connects the nano cellulose fiber to the surface of cotton fiber through ester group, forms nano cellulose network structure on the surface of cotton fiber, connects diphenolic acid molecule through ester group on the surface of nano cellulose, and the phenolic hydroxyl functional group of the nano cellulose has adsorption and destruction effects on viral capsid protein, thus forming antiviral activity.
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| CN102877287A (en) * | 2012-10-19 | 2013-01-16 | 常州大学 | Preparation method of halamine-containing antibacterial cellulose fabric |
| JP2017057200A (en) * | 2015-09-18 | 2017-03-23 | ヤマサ醤油株式会社 | Nucleoside derivative having physiological activity such as anti-DNA virus activity |
| CN111849002A (en) * | 2020-07-20 | 2020-10-30 | 华南理工大学 | High-dimensional-stability cellulose-based transparent waterproof film and preparation method thereof |
| CN113445315A (en) * | 2021-06-21 | 2021-09-28 | 浙江理工大学 | Preparation method of diphenolic acid antibacterial cotton fabric |
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| CN102877287A (en) * | 2012-10-19 | 2013-01-16 | 常州大学 | Preparation method of halamine-containing antibacterial cellulose fabric |
| JP2017057200A (en) * | 2015-09-18 | 2017-03-23 | ヤマサ醤油株式会社 | Nucleoside derivative having physiological activity such as anti-DNA virus activity |
| CN111849002A (en) * | 2020-07-20 | 2020-10-30 | 华南理工大学 | High-dimensional-stability cellulose-based transparent waterproof film and preparation method thereof |
| CN113445315A (en) * | 2021-06-21 | 2021-09-28 | 浙江理工大学 | Preparation method of diphenolic acid antibacterial cotton fabric |
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