CN111411509A - Nano chitosan modified cotton fiber and preparation method thereof - Google Patents
Nano chitosan modified cotton fiber and preparation method thereof Download PDFInfo
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- CN111411509A CN111411509A CN202010381557.XA CN202010381557A CN111411509A CN 111411509 A CN111411509 A CN 111411509A CN 202010381557 A CN202010381557 A CN 202010381557A CN 111411509 A CN111411509 A CN 111411509A
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 136
- 229920000742 Cotton Polymers 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 69
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 51
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 claims abstract description 32
- 229920002678 cellulose Polymers 0.000 claims abstract description 27
- 239000001913 cellulose Substances 0.000 claims abstract description 27
- 239000002270 dispersing agent Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 24
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000002791 soaking Methods 0.000 claims abstract description 13
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 9
- 239000004744 fabric Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 230000036541 health Effects 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims 2
- IEKHISJGRIEHRE-UHFFFAOYSA-N 16-methylheptadecanoic acid;propan-2-ol;titanium Chemical compound [Ti].CC(C)O.CC(C)CCCCCCCCCCCCCCC(O)=O.CC(C)CCCCCCCCCCCCCCC(O)=O.CC(C)CCCCCCCCCCCCCCC(O)=O IEKHISJGRIEHRE-UHFFFAOYSA-N 0.000 claims 1
- 230000006750 UV protection Effects 0.000 abstract description 8
- 238000004321 preservation Methods 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 22
- 238000000498 ball milling Methods 0.000 description 20
- 239000008367 deionised water Substances 0.000 description 20
- 229910021641 deionized water Inorganic materials 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 20
- 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 description 12
- 239000001768 carboxy methyl cellulose Substances 0.000 description 12
- 230000008569 process Effects 0.000 description 12
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 12
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 12
- 239000006229 carbon black Substances 0.000 description 11
- 239000006185 dispersion Substances 0.000 description 10
- 238000006467 substitution reaction Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- 239000000835 fiber Substances 0.000 description 7
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 239000005543 nano-size silicon particle Substances 0.000 description 4
- 230000003385 bacteriostatic effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 241000222122 Candida albicans Species 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229940095731 candida albicans Drugs 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 1
- 241000238424 Crustacea Species 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 241000237852 Mollusca Species 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000002538 fungal effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000009759 skin aging Effects 0.000 description 1
- 230000037380 skin damage Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/08—Organic compounds
- D06M10/10—Macromolecular compounds
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- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/06—Inorganic compounds or elements
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- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
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- 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
- D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
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Abstract
The invention discloses a nano chitosan modified cotton fiber. The invention discloses a preparation method of the nano chitosan modified cotton fiber, which comprises the following steps: putting the cotton fiber into a sodium hydroxide solution, stirring, washing, drying, putting into a sodium periodate solution, and stirring in a dark place to obtain activated cotton fiber; uniformly mixing nano chitosan, a cellulose dispersant and acetic acid, adding triisostearoyl isopropyl titanate, stirring, adding tetraethoxysilane under a stirring state, continuously stirring, and defoaming in vacuum to obtain a pretreated nano chitosan solution; and soaking the activated cotton fiber in the pretreated nano chitosan solution, performing pulse microwave treatment, filtering, and airing at room temperature to obtain the nano chitosan modified cotton fiber. The invention adopts the nano chitosan to modify the cotton fiber, so that the cotton fiber has better heat preservation foundation, excellent antibacterial and ultraviolet resistance, environment-friendly method and application in the fields of medical treatment, sanitation and antibacterial fabrics.
Description
Technical Field
The invention relates to the technical field of cotton fiber modification, in particular to a nano chitosan modified cotton fiber and preparation and application thereof.
Background
The cotton fiber is popular with consumers due to excellent moisture absorption, ventilation, comfort, softness, heat preservation, reproducibility, degradability and the like. However, cotton fibers still have insufficient functionality compared to synthetic fibers. The cotton fiber has the characteristics of large specific surface area, strong moisture absorption capacity and the like, so that microorganisms are easy to attach, reproduce and transmit in the process of taking, thereby causing the strength reduction of the cotton fiber, the generation of stains, discoloration and odor, even the transmission of diseases and influencing the health of human bodies.
Meanwhile, excessive ultraviolet irradiation can cause skin damage, aging and even canceration. Therefore, in order to fully exploit the potential functions of the cotton fibers and improve the technical content and the product added value of the cotton fibers, the functional modification of the cotton fibers becomes an important research direction.
The nano material is a material with the size of 1-100nm, has the advantages of uniform particle size, multiple functions and the like, and has wide research and application in the fields of biology, medicine, textile, printing and dyeing and the like. Among various types of nano materials, nano chitosan is a natural biological polymer obtained by deacetylation of chitin, and widely exists in shells of natural crustaceans, skins of insects and the like, skeletons of mollusks and cell walls of fungal algae plants, and the natural polymer is widely concerned by various industries due to excellent performances such as biocompatibility, safety, microbial degradability and the like. However, at present, the nano chitosan and the cotton fiber lack firm acting force combination, and the washing fastness is weak, so that the antibacterial and ultraviolet resistance of the cotton fiber is continuously poor.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a nano chitosan modified cotton fiber and a preparation method and application thereof.
A preparation method of nano chitosan modified cotton fiber comprises the following steps:
s1, putting the cotton fiber into a sodium hydroxide solution, stirring at 70-80 ℃, washing, drying, putting into a sodium periodate solution, and stirring in the dark to obtain activated cotton fiber;
s2, uniformly mixing the nano chitosan, the cellulose dispersant and acetic acid, adding triisostearoyl isopropyl titanate, stirring at 40-50 ℃, adding tetraethoxysilane under a stirring state, continuously stirring, and carrying out vacuum defoaming to obtain a pretreated nano chitosan solution;
s3, soaking the activated cotton fiber in the pretreated nano chitosan solution, performing pulse microwave treatment for 5-15min, pausing for 5-15S every 1min of microwave treatment reaction, wherein the microwave power is 400-500W, filtering, and drying at room temperature to obtain the nano chitosan modified cotton fiber.
Preferably, in S1, the concentration of the sodium hydroxide solution is 0.5-0.8 mol/L.
Preferably, in S1, the mass fraction of the sodium periodate solution is 2.13-4.32%.
Preferably, in S1, the mass ratio of the cotton fiber to the sodium hydroxide solution to the sodium periodate solution is 10-20: 80-120: 80-120.
Preferably, in S2, the mass ratio of the nano chitosan, the cellulose dispersant, the acetic acid, the triisostearoyl isopropyl titanate and the tetraethoxysilane is 2-4: 0.1-0.5: 20-40: 1-2: 10-20.
The cellulose dispersant is prepared by the following process: dissolving sodium carboxymethylcellulose with a substitution degree of 0.2-0.4 in deionized water, wherein the weight ratio of the sodium carboxymethylcellulose to the deionized water is 1: 3-5, adding white carbon black in the stirring process, wherein the adding amount of the white carbon black is 0.2-0.4 time of that of the sodium carboxymethyl cellulose, and performing ball milling dispersion for 10-30min at the ball milling rotation speed of 800-1000r/min to obtain the cellulose dispersing agent.
The cellulose dispersant has a particle size of 0.1-0.15 μm, a viscosity of 10-14mPa.s, and a centrifugal stability of 88-90%.
The cellulose dispersing agent has good dispersibility, small particle size and high stability, can promote the nano chitosan to be uniformly dispersed in an acetic acid solution, and can activate the nano chitosan to enhance the bonding strength with the nano silicon dioxide.
Preferably, in S2, the nano chitosan has a particle size of 10-80 nm.
Preferably, in the nano chitosan of S2, the mass percentage of chitosan with a particle size of 10nm or more and less than 30nm is 30-50%, the mass percentage of chitosan with a particle size of 30nm or more and less than 50nm is 40-60%, and the balance is chitosan with a particle size of 50nm or more and 80nm or less.
Preferably, in S3, the pulse microwave treatment is carried out for 8-12min, the reaction is suspended for 8-12S every 1min of microwave treatment, and the microwave power is 430-470W.
A nano chitosan modified cotton fiber is prepared by the preparation method of the nano chitosan modified cotton fiber.
The nano chitosan modified cotton fiber is applied to the fields of antibacterial fabrics or medical treatment and health.
The technical effects of the invention are as follows:
(1) because the surface of the nano chitosan contains a large amount of cations, and the tetraethoxysilane is hydrolyzed into silicon dioxide with negative charges in an acetic acid solution, the nano silicon dioxide obtained by hydrolysis is tightly adsorbed on the surface of the nano chitosan by utilizing the interaction of the nano chitosan and the tetraethoxysilane, and the triisostearoyl isopropyl titanate promotes the chemical bonding between the nano silicon dioxide and the chitosan, so that the nano chitosan has excellent anti-aging and chemical resistance; meanwhile, the method can effectively avoid the agglomeration phenomenon of the nano silicon dioxide, and the nano chitosan is uniformly grafted on the surface;
(2) the invention grafts the pretreated nano chitosan on the surface of the activated cotton fiber, and can form a protective film on the surface of the activated cotton fiber, so that the product has good antibacterial and ultraviolet resistance performances, good mechanical property and difficult shedding in the washing process, thereby having lasting antibacterial and ultraviolet resistance performances;
(3) the fiber obtained by the invention has a large amount of nano-scale gaps, obtains excellent heat preservation effect, enables the heat preservation effect of the product to be controllable by controlling the addition amount of nano-silica, has a heat conductivity coefficient of 0.01-0.014W/(m.K) at normal temperature, and has more stable thermodynamic performance compared with other materials.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
The cotton fibers used in the examples and comparative examples were fine staple cotton planted in the plain of Jianghuai, Anhui, China.
Example 1
A preparation method of nano chitosan modified cotton fiber comprises the following steps:
s1, putting 10kg of cotton fibers into 120kg of sodium hydroxide solution with the concentration of 0.5 mol/L, stirring for 40min at 80 ℃, washing with deionized water, drying, putting into 120kg of sodium periodate solution with the mass fraction of 2.13%, and stirring for 20min in a dark place to obtain activated cotton fibers;
s2, dissolving 1kg of sodium carboxymethylcellulose with the substitution degree of 0.2 in 5kg of deionized water, adding 0.2kg of white carbon black in the stirring process, and performing ball milling and dispersion for 30min at the ball milling rotation speed of 800r/min to obtain a cellulose dispersing agent with the particle size of 0.15 mu m, the viscosity of 10mPa.s and the centrifugal stability of 90%;
uniformly mixing 4kg of nano chitosan, 0.1kg of cellulose dispersant and 40kg of acetic acid, adding 1kg of triisostearoyl isopropyl titanate, stirring for 20min at 50 ℃, adding 20kg of tetraethoxysilane under the stirring state, continuously stirring for 2h, and carrying out vacuum defoaming to obtain a pretreated nano chitosan solution;
in the nano chitosan, the chitosan with the grain diameter of more than or equal to 10nm and less than 30nm accounts for 30 percent by mass, the chitosan with the grain diameter of more than or equal to 30nm and less than 50nm accounts for 60 percent by mass, and the balance is the chitosan with the grain diameter of more than or equal to 50nm and less than or equal to 80 nm;
and S3, soaking the activated cotton fiber in the pretreated nano chitosan solution, performing pulse microwave treatment for 5min, pausing for 15S every 1min of microwave treatment reaction, wherein the microwave power is 400W, filtering, and airing at room temperature to obtain the nano chitosan modified cotton fiber.
Example 2
A preparation method of nano chitosan modified cotton fiber comprises the following steps:
s1, feeding 20kg of cotton fibers into 80kg of sodium hydroxide solution with the concentration of 0.8 mol/L, stirring for 60min at 70 ℃, washing with deionized water, drying, feeding 80kg of sodium periodate solution with the mass fraction of 4.32%, and stirring for 50min in a dark place to obtain activated cotton fibers;
s2, dissolving 1kg of sodium carboxymethylcellulose with the degree of substitution of 0.4 in 3kg of deionized water, adding 0.4kg of white carbon black in the stirring process, and performing ball milling and dispersion for 10min at the ball milling rotating speed of 1000r/min to obtain a cellulose dispersing agent with the particle size of 0.1 mu m, the viscosity of 14mPa.s and the centrifugal stability of 88%;
uniformly mixing 2kg of nano chitosan, 0.5kg of cellulose dispersant and 20kg of acetic acid, adding 2kg of triisostearoyl isopropyl titanate, stirring for 40min at 40 ℃, adding 10kg of tetraethoxysilane under a stirring state, continuously stirring for 4h, and carrying out vacuum defoaming to obtain a pretreated nano chitosan solution;
in the nano chitosan, the chitosan with the grain diameter of more than or equal to 10nm and less than 30nm accounts for 50 percent by mass, the chitosan with the grain diameter of more than or equal to 30nm and less than 50nm accounts for 40 percent by mass, and the balance is the chitosan with the grain diameter of more than or equal to 50nm and less than or equal to 80 nm;
and S3, soaking the activated cotton fiber in the pretreated nano chitosan solution, performing pulse microwave treatment for 15min, pausing for 5S every 1min of microwave treatment reaction, wherein the microwave power is 500W, filtering, and airing at room temperature to obtain the nano chitosan modified cotton fiber.
Example 3
A preparation method of nano chitosan modified cotton fiber comprises the following steps:
s1, putting 12kg of cotton fibers into 110kg of sodium hydroxide solution with the concentration of 0.6 mol/L, stirring for 45min at 77 ℃, washing with deionized water, drying, putting into 110kg of sodium periodate solution with the mass fraction of 2.46%, and stirring for 30min in a dark place to obtain activated cotton fibers;
s2, dissolving 1kg of sodium carboxymethylcellulose with the degree of substitution of 0.25 in 4.5kg of deionized water, adding 0.25kg of white carbon black in the stirring process, and carrying out ball milling dispersion for 25min at the ball milling rotating speed of 850r/min to obtain a cellulose dispersing agent with the particle size of 0.14 mu m, the viscosity of 11mPa.s and the centrifugal stability of 89.5%;
uniformly mixing 3.5kg of nano chitosan, 0.2kg of cellulose dispersant and 35kg of acetic acid, adding 1.3kg of triisostearoyl isopropyl titanate, stirring for 25min at 48 ℃, adding 17kg of tetraethoxysilane under the stirring state, continuously stirring for 2.5h, and defoaming in vacuum to obtain a pretreated nano chitosan solution;
in the nano chitosan, the chitosan with the grain diameter of more than or equal to 10nm and less than 30nm accounts for 35 percent by mass, the chitosan with the grain diameter of more than or equal to 30nm and less than 50nm accounts for 55 percent by mass, and the balance is the chitosan with the grain diameter of more than or equal to 50nm and less than or equal to 80 nm;
and S3, soaking the activated cotton fiber in the pretreated nano chitosan solution, performing pulse microwave treatment for 8min, pausing for 12S every 1min of microwave treatment reaction, wherein the microwave power is 430W, filtering, and airing at room temperature to obtain the nano chitosan modified cotton fiber.
Example 4
A preparation method of nano chitosan modified cotton fiber comprises the following steps:
s1, putting 18kg of cotton fibers into 90kg of sodium hydroxide solution with the concentration of 0.7 mol/L, stirring for 55min at 73 ℃, washing with deionized water, drying, putting into 90kg of sodium periodate solution with the mass fraction of 3.87%, and stirring for 40min in a dark place to obtain activated cotton fibers;
s2, dissolving 1kg of sodium carboxymethylcellulose with the degree of substitution of 0.35 in 3.5kg of deionized water, adding 0.35kg of white carbon black in the stirring process, and carrying out ball milling dispersion for 15min at the ball milling rotating speed of 950r/min to obtain a cellulose dispersing agent with the particle size of 0.12 mu m, the viscosity of 13mPa.s and the centrifugal stability of 88.5%;
uniformly mixing 2.5kg of nano chitosan, 0.4kg of cellulose dispersant and 25kg of acetic acid, adding 1.7kg of triisostearoyl isopropyl titanate, stirring at 42 ℃ for 35min, adding 13kg of tetraethoxysilane under the stirring state, continuously stirring for 3.5h, and defoaming in vacuum to obtain a pretreated nano chitosan solution;
in the nano chitosan, the mass percent of chitosan with the particle size of more than or equal to 10nm and less than 30nm is 45 percent, the mass percent of chitosan with the particle size of more than or equal to 30nm and less than 50nm is 45 percent, and the balance is chitosan with the particle size of more than or equal to 50nm and less than or equal to 80 nm;
and S3, soaking the activated cotton fiber in the pretreated nano chitosan solution, performing pulse microwave treatment for 12min, pausing for 8S every 1min of microwave treatment reaction, wherein the microwave power is 470W, filtering, and airing at room temperature to obtain the nano chitosan modified cotton fiber.
Example 5
A preparation method of nano chitosan modified cotton fiber comprises the following steps:
s1, putting 15kg of cotton fibers into 100kg of 0.65 mol/L sodium hydroxide solution, stirring for 50min at 75 ℃, washing with deionized water, drying, putting 100kg of sodium periodate solution with the mass fraction of 3.22%, and stirring for 35min in a dark place to obtain activated cotton fibers;
s2, dissolving 1kg of sodium carboxymethylcellulose with the degree of substitution of 0.3 in 4kg of deionized water, adding 0.3kg of white carbon black in the stirring process, and performing ball milling and dispersion for 20min at the ball milling rotating speed of 900r/min to obtain a cellulose dispersing agent with the particle size of 0.13 mu m, the viscosity of 12mPa.s and the centrifugal stability of 89%;
uniformly mixing 3kg of nano chitosan, 0.3kg of cellulose dispersant and 30kg of acetic acid, adding 1.5kg of triisostearoyl isopropyl titanate, stirring for 30min at 45 ℃, adding 15kg of tetraethoxysilane under a stirring state, continuously stirring for 3h, and carrying out vacuum defoaming to obtain a pretreated nano chitosan solution;
in the nano chitosan, the chitosan with the grain diameter of more than or equal to 10nm and less than 30nm accounts for 40 percent by mass, the chitosan with the grain diameter of more than or equal to 30nm and less than 50nm accounts for 50 percent by mass, and the balance is the chitosan with the grain diameter of more than or equal to 50nm and less than or equal to 80 nm;
s3, soaking the activated cotton fiber in the pretreated nano chitosan solution, performing pulse microwave treatment for 10min, pausing for 10S every 1min of microwave treatment reaction, wherein the microwave power is 450W, filtering, and airing at room temperature to obtain the nano chitosan modified cotton fiber.
Comparative example 1
A preparation method of modified cotton fiber comprises the following steps:
s1, dissolving 1kg of sodium carboxymethylcellulose with the degree of substitution of 0.3 in 4kg of deionized water, adding 0.3kg of white carbon black in the stirring process, and performing ball milling and dispersion for 20min at the ball milling rotating speed of 900r/min to obtain a cellulose dispersing agent with the particle size of 0.13 mu m, the viscosity of 12mPa.s and the centrifugal stability of 89%;
uniformly mixing 3kg of nano chitosan, 0.3kg of cellulose dispersant and 30kg of acetic acid, adding 1.5kg of triisostearoyl isopropyl titanate, stirring for 30min at 45 ℃, adding 15kg of tetraethoxysilane under a stirring state, continuously stirring for 3h, and carrying out vacuum defoaming to obtain a pretreated nano chitosan solution;
in the nano chitosan, the chitosan with the grain diameter of more than or equal to 10nm and less than 30nm accounts for 40 percent by mass, the chitosan with the grain diameter of more than or equal to 30nm and less than 50nm accounts for 50 percent by mass, and the balance is the chitosan with the grain diameter of more than or equal to 50nm and less than or equal to 80 nm;
s2, soaking the cotton fibers in the pretreated nano chitosan solution, performing pulse microwave treatment for 10min, pausing for 10S every 1min of microwave treatment reaction, wherein the microwave power is 450W, filtering, and airing at room temperature to obtain the modified cotton fibers.
Comparative example 2
A preparation method of modified cotton fiber comprises the following steps:
s1, putting 15kg of cotton fibers into 100kg of 0.65 mol/L sodium hydroxide solution, stirring for 50min at 75 ℃, washing with deionized water, drying, putting 100kg of sodium periodate solution with the mass fraction of 3.22%, and stirring for 35min in a dark place to obtain activated cotton fibers;
s2, uniformly mixing 3kg of nano chitosan and 30kg of acetic acid to obtain a nano chitosan solution;
in the nano chitosan, the chitosan with the grain diameter of more than or equal to 10nm and less than 30nm accounts for 40 percent by mass, the chitosan with the grain diameter of more than or equal to 30nm and less than 50nm accounts for 50 percent by mass, and the balance is the chitosan with the grain diameter of more than or equal to 50nm and less than or equal to 80 nm;
s3, soaking the activated cotton fiber in the pretreated nano chitosan solution, performing pulse microwave treatment for 10min, pausing for 10S every 1min of microwave treatment reaction, wherein the microwave power is 450W, filtering, and airing at room temperature to obtain the modified cotton fiber.
Comparative example 3
A preparation method of modified cotton fiber comprises the following steps:
s1, putting 15kg of cotton fibers into 100kg of 0.65 mol/L sodium hydroxide solution, stirring for 50min at 75 ℃, washing with deionized water, drying, putting 100kg of sodium periodate solution with the mass fraction of 3.22%, and stirring for 35min in a dark place to obtain activated cotton fibers;
s2, dissolving 1kg of sodium carboxymethylcellulose with the degree of substitution of 0.3 in 4kg of deionized water, adding 0.3kg of white carbon black in the stirring process, and performing ball milling and dispersion for 20min at the ball milling rotating speed of 900r/min to obtain a cellulose dispersing agent with the particle size of 0.13 mu m, the viscosity of 12mPa.s and the centrifugal stability of 89%;
uniformly mixing 3kg of nano chitosan, 0.3kg of cellulose dispersant and 30kg of acetic acid, adding 15kg of tetraethoxysilane under the stirring state, continuously stirring for 3 hours, and carrying out vacuum defoaming to obtain a pretreated nano chitosan solution;
in the nano chitosan, the chitosan with the grain diameter of more than or equal to 10nm and less than 30nm accounts for 40 percent by mass, the chitosan with the grain diameter of more than or equal to 30nm and less than 50nm accounts for 50 percent by mass, and the balance is the chitosan with the grain diameter of more than or equal to 50nm and less than or equal to 80 nm;
s3, soaking the activated cotton fiber in the pretreated nano chitosan solution, performing pulse microwave treatment for 10min, pausing for 10S every 1min of microwave treatment reaction, wherein the microwave power is 450W, filtering, and airing at room temperature to obtain the modified cotton fiber.
Comparative example 4
A preparation method of modified cotton fiber comprises the following steps:
s1, putting 15kg of cotton fibers into 100kg of 0.65 mol/L sodium hydroxide solution, stirring for 50min at 75 ℃, washing with deionized water, drying, putting 100kg of sodium periodate solution with the mass fraction of 3.22%, and stirring for 35min in a dark place to obtain activated cotton fibers;
s2, dissolving 1kg of sodium carboxymethylcellulose with the degree of substitution of 0.3 in 4kg of deionized water, adding 0.3kg of white carbon black in the stirring process, and performing ball milling and dispersion for 20min at the ball milling rotating speed of 900r/min to obtain a cellulose dispersing agent with the particle size of 0.13 mu m, the viscosity of 12mPa.s and the centrifugal stability of 89%;
uniformly mixing 3kg of nano chitosan, 0.3kg of cellulose dispersant and 30kg of acetic acid, adding 1.5kg of triisostearoyl isopropyl titanate, stirring for 30min at 45 ℃, adding 15kg of nano titanium dioxide under a stirring state, continuously stirring for 3h, and defoaming in vacuum to obtain a pretreated nano chitosan solution;
in the nano chitosan, the chitosan with the grain diameter of more than or equal to 10nm and less than 30nm accounts for 40 percent by mass, the chitosan with the grain diameter of more than or equal to 30nm and less than 50nm accounts for 50 percent by mass, and the balance is the chitosan with the grain diameter of more than or equal to 50nm and less than or equal to 80 nm;
s3, soaking the activated cotton fiber in the pretreated nano chitosan solution, performing pulse microwave treatment for 10min, pausing for 10S every 1min of microwave treatment reaction, wherein the microwave power is 450W, filtering, and airing at room temperature to obtain the modified cotton fiber.
Comparative example 5
A preparation method of modified cotton fiber comprises the following steps:
s1, putting 15kg of cotton fibers into 100kg of 0.65 mol/L sodium hydroxide solution, stirring for 50min at 75 ℃, washing with deionized water, drying, putting 100kg of sodium periodate solution with the mass fraction of 3.22%, and stirring for 35min in a dark place to obtain activated cotton fibers;
s2, dissolving 1kg of sodium carboxymethylcellulose with the degree of substitution of 0.3 in 4kg of deionized water, adding 0.3kg of white carbon black in the stirring process, and performing ball milling and dispersion for 20min at the ball milling rotating speed of 900r/min to obtain a cellulose dispersing agent with the particle size of 0.13 mu m, the viscosity of 12mPa.s and the centrifugal stability of 89%;
uniformly mixing 3kg of nano chitosan, 0.3kg of cellulose dispersant and 30kg of acetic acid, adding 1.5kg of triisostearoyl isopropyl titanate, stirring for 30min at 45 ℃, adding 15kg of tetraethoxysilane under a stirring state, continuously stirring for 3h, and carrying out vacuum defoaming to obtain a pretreated nano chitosan solution;
in the nano chitosan, the chitosan with the grain diameter of more than or equal to 10nm and less than 30nm accounts for 40 percent by mass, the chitosan with the grain diameter of more than or equal to 30nm and less than 50nm accounts for 50 percent by mass, and the balance is the chitosan with the grain diameter of more than or equal to 50nm and less than or equal to 80 nm;
s3, soaking the activated cotton fiber in the pretreated nano chitosan solution, heating to 60-80 ℃, preserving the temperature for 10min, filtering, and airing at room temperature to obtain the modified cotton fiber.
The nano chitosan modified cotton fiber obtained in example 5 and the modified cotton fibers obtained in comparative examples 1-5 were compared, specifically as follows:
1. the mechanical properties of the resulting fibers from each group were tested:
| specific strength, cN/tex | Elongation at break,% | |
| Example 5 | 31.8 | 7.56 |
| Comparative example 1 | 29.0 | 7.03 |
| Comparative example 2 | 29.7 | 7.27 |
| Comparative example 3 | 27.8 | 6.41 |
| Comparative example 4 | 26.3 | 6.89 |
| Comparative example 5 | 25.7 | 7.45 |
| Cotton fiber | 24.9 | 6.25 |
2. The antibacterial performance of the obtained fibers of each group is tested:
escherichia coli, staphylococcus aureus and candida albicans are selected as test strains, an improved oscillating flask method is adopted for testing, and the bacteriostasis rate results are as follows:
wherein the test result is expressed by the bacteriostatic rate,
Y＝(Xa-Xb)/Xa×100％
y is the bacteriostatic rate,%; xaThe number of colonies before sample oscillation; xbThe number of colonies after the sample oscillation is taken as the number of colonies;
| escherichia coli | Staphylococcus aureus | Candida albicans | |
| Example 5 | 98.6％ | 95.7％ | 97.3％ |
| Comparative example 1 | 98.3％ | 94.9％ | 98.0％ |
| Comparative example 2 | 88.8％ | 84.1％ | 87.5％ |
| Comparative example 3 | 91.7％ | 89.3％ | 92.5％ |
| Comparative example 4 | 99.2％ | 98.5％ | 99.8％ |
| Comparative example 5 | 97.5％ | 94.0％ | 92.6％ |
| Cotton fiber | 60.8％ | 44.7％ | 53.5％ |
After 20 times of washing, the bacteriostatic rate results are as follows:
3. and (3) testing the heat insulation performance of the obtained fibers of each group, wherein the test method specifically comprises the following steps:
tightly winding the obtained fibers of each group on a hard board with a certain size, and preparing a sample to be tested (a sheet material with the length and the width not less than 30 mm) after drawing out the hard board; before testing, placing each group of samples in a constant temperature and humidity chamber for balancing for 24 hours, wherein the temperature is 20 +/-2 ℃, and the relative humidity is 65 +/-5%; the test is carried out by a hot wire method solid thermal conductivity coefficient instrument, and the result is as follows:
| thermal conductivity, W/(m. K) | |
| Example 5 | 0.011 |
| Comparative example 1 | 0.017 |
| Comparative example 2 | 0.023 |
| Comparative example 3 | 0.020 |
| Comparative example 4 | 0.025 |
| Comparative example 5 | 0.030 |
| Cotton fiber | 0.071 |
4. And (3) carrying out ultraviolet resistance test on the obtained fibers of each group, wherein the ultraviolet resistance test comprises the following specific steps:
the fibers obtained from each group were processed into a plain weave fabric and subjected to an ultraviolet resistance test according to the method specified in GB/T17032-1997 (wherein the UVA band is 320-420nm and the UVB band is 275-320nm) with the following results:
the results of the above four tables show that: the modified cotton fiber has a good heat preservation foundation and excellent antibacterial and ultraviolet resistance.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A preparation method of nano chitosan modified cotton fiber is characterized by comprising the following steps:
s1, putting the cotton fiber into a sodium hydroxide solution, stirring at 70-80 ℃, washing, drying, putting into a sodium periodate solution, and stirring in the dark to obtain activated cotton fiber;
s2, uniformly mixing the nano chitosan, the cellulose dispersant and acetic acid, adding triisostearoyl isopropyl titanate, stirring at 40-50 ℃, adding tetraethoxysilane under a stirring state, continuously stirring, and carrying out vacuum defoaming to obtain a pretreated nano chitosan solution;
s3, soaking the activated cotton fiber in the pretreated nano chitosan solution, performing pulse microwave treatment for 5-15min, pausing for 5-15S every 1min of microwave treatment reaction, wherein the microwave power is 400-500W, filtering, and drying at room temperature to obtain the nano chitosan modified cotton fiber.
2. The method for preparing nano chitosan modified cotton fiber as claimed in claim 1, wherein the concentration of sodium hydroxide solution in S1 is 0.5-0.8 mol/L.
3. The method for preparing nano chitosan modified cotton fiber according to claim 1, wherein in S1, the mass fraction of the sodium periodate solution is 2.13-4.32%.
4. The method for preparing the nano chitosan modified cotton fiber according to claim 2 or 3, wherein in S1, the mass ratio of the cotton fiber to the sodium hydroxide solution to the sodium periodate solution is 10-20: 80-120: 80-120.
5. The method for preparing the nano chitosan modified cotton fiber of claim 1, wherein in S2, the mass ratio of the nano chitosan, the cellulose dispersant, acetic acid, isopropyl triisostearoyl titanate and ethyl orthosilicate is 2-4: 0.1-0.5: 20-40: 1-2: 10-20.
6. The method for preparing the nano chitosan modified cotton fiber according to claim 1, wherein in S2, the nano chitosan has a particle size of 10-80 nm.
7. The method for preparing the chitosan-modified cotton fiber of claim 6, wherein in the nano chitosan of S2, the mass percentage of chitosan with the particle size of more than or equal to 10nm and less than 30nm is 30-50%, the mass percentage of chitosan with the particle size of more than or equal to 30nm and less than 50nm is 40-60%, and the balance is chitosan with the particle size of more than or equal to 50nm and less than or equal to 80 nm.
8. The method as claimed in claim 1, wherein in S3, the pulse microwave treatment is performed for 8-12min, the reaction time is 1min and the reaction time is 8-12S, and the microwave power is 430-470W.
9. A nano chitosan modified cotton fiber, which is characterized by being prepared by the preparation method of the nano chitosan modified cotton fiber of any one of claims 1 to 8.
10. The nano chitosan modified cotton fiber as claimed in claim 9, which is applied to the fields of antibacterial fabrics or medical health.
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