CN108978191B - Antibacterial far infrared health acrylic fiber and preparation method and application thereof - Google Patents
Antibacterial far infrared health acrylic fiber and preparation method and application thereof Download PDFInfo
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- CN108978191B CN108978191B CN201810664282.3A CN201810664282A CN108978191B CN 108978191 B CN108978191 B CN 108978191B CN 201810664282 A CN201810664282 A CN 201810664282A CN 108978191 B CN108978191 B CN 108978191B
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- 239000004575 stone Substances 0.000 claims abstract description 93
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- FYZFRYWTMMVDLR-UHFFFAOYSA-M trimethyl(3-trimethoxysilylpropyl)azanium;chloride Chemical compound [Cl-].CO[Si](OC)(OC)CCC[N+](C)(C)C FYZFRYWTMMVDLR-UHFFFAOYSA-M 0.000 claims abstract description 16
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- 238000003756 stirring Methods 0.000 claims description 10
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- 238000000746 purification Methods 0.000 claims description 7
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 239000012467 final product Substances 0.000 claims description 5
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical group CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 3
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- 230000037072 sun protection Effects 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 3
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- 239000000835 fiber Substances 0.000 abstract description 20
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- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 6
- 241000588724 Escherichia coli Species 0.000 description 5
- 150000002825 nitriles Chemical class 0.000 description 5
- 241000222122 Candida albicans Species 0.000 description 4
- 239000002553 antibacterial enhancer Substances 0.000 description 4
- 229940095731 candida albicans Drugs 0.000 description 4
- 125000002091 cationic group Chemical group 0.000 description 4
- 230000004089 microcirculation Effects 0.000 description 4
- 229920000728 polyester Polymers 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 4
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
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- 230000008569 process Effects 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 241000191940 Staphylococcus Species 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000002318 adhesion promoter Substances 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 239000012496 blank sample Substances 0.000 description 2
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- 238000011056 performance test Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910021654 trace metal Inorganic materials 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
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- 239000008280 blood Substances 0.000 description 1
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- 230000017531 blood circulation Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
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- 238000005338 heat storage Methods 0.000 description 1
- 210000005260 human cell Anatomy 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000010355 oscillation Effects 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
- 239000002245 particle Substances 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
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- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—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 silicon or compounds thereof
- D06M11/79—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 silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
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- D—TEXTILES; PAPER
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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
- 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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- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
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Abstract
The invention relates to an antibacterial far infrared health acrylic fiber and a preparation method and application thereof, wherein in the method, firstly, inorganic dispersant and antibacterial reinforcing agent trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride are used for carrying out surface antibacterial reinforcing modification on taiji stone nano powder, then the modified taiji stone nano powder, amino coupling agent and deionized water are used for forming a dispersion solution, the acrylic fiber is soaked in the dispersion solution for reaction under certain bath ratio and reaction conditions, after the reaction is finished, a large amount of organic solvent and deionized water are used for washing and washing, and finally, the acrylic fiber is dried in the air under natural conditions, so that the antibacterial far infrared health acrylic fiber is obtained. The fiber can be applied to underwear, underpants, socks, sportswear, swimwear, sun-proof clothes and home textile fabrics, and has remarkable and lasting antibacterial and far infrared effects, the far infrared emissivity reaches more than 93 percent, and the total antibacterial property reaches more than 94.2 percent.
Description
Technical Field
The invention belongs to the field of fiber processing, and particularly relates to an antibacterial far infrared health acrylic fiber, and a preparation method and application thereof.
Background
Taiji stone is a natural ore whose main component is silicon dioxide, but also a small amount of titanium dioxide, and various trace metal mineral elements. Its high-frequency resonance frequency is very close to the resonance frequency of human cell molecule, and can promote human body to absorb and gather positive energy, and possesses several excellent functions of far infrared radiation property, UV-resisting property and certain antibacterial property.
According to research and research, the underwear containing taiji stone can obviously promote blood microcirculation of human bodies and promote metabolism. With the discovery of the natural health-care function of the tai chi stone, a plurality of textile functional products related to the tai chi stone are sequentially seen in the market. The products include fiber, yarn and fabric, but in most of the products, regarding the application of the taiji stone, the taiji stone and the spinning solution are blended in the spinning process to process the spinning solution into the fiber, or the fiber is spun into the yarn, or finally the yarn containing the taiji stone is woven into the fabric.
For example, chinese patent application (CN104153031A) discloses a health-care fiber capable of promoting human microcirculation and a manufacturing method thereof, which comprises mixing ultrafine tayata stone micropowder with a fiber base material, drying, adding a polymer spinning aid, granulating to obtain tayata stone masterbatch, and mixing the tayata stone masterbatch with homogeneous fiber slices to finally obtain the health-care fiber; chinese patent application (CN103726125A) discloses an anti-mite and antibacterial polyester staple fiber and a preparation method thereof, wherein the anti-mite and antibacterial polyester staple fiber is prepared by preparing micron-sized heat-storage anti-mite ceramic powder containing taiji stone and silver-loaded nano titanium dioxide composite antibacterial powder in an esterification polymerization spinning mode, or preparing the powder into master batches, mixing the master batches with polyester chips, and then spinning to obtain the anti-mite and antibacterial polyester staple fiber which has strong antibacterial effect on staphylococcus aureus and escherichia coli; although the health-care fibers related to the two Chinese patents contain the tai chi stone raw material, the tai chi stone nano powder is added into the spinning solution, the addition amount of the tai chi stone nano powder is particularly limited by adding the tai chi stone nano powder into the spinning solution, in order to ensure the spinnability and the spinning uniformity, the addition amount is generally not more than 5 wt%, and the function and the efficacy of the tai chi stone are difficult to be well exerted; chinese patent (CN104153098A) discloses a health-care fabric capable of promoting human microcirculation, which adopts taiji stone polyacrylonitrile fiber (acrylic fiber), but the fiber is produced by adding taiji stone ultrafine micro-nano powder which has the function of promoting human microcirculation and is rich in various trace metal mineral elements and far infrared functions into the fabric during spinning, mixing the taiji stone ultrafine micro-nano powder with homogeneous fiber slices uniformly, and spinning to obtain taiji stone fiber.
Disclosure of Invention
The invention provides an antibacterial far infrared health acrylic fiber which combines taiji stone with the surface of an acrylic fiber by a post-finishing mode and enables a fiber product to maximally exert the function and the effect of the taiji stone, a preparation method and application thereof, aiming at solving the problems that the amount of the taiji stone nano powder added into the existing spinning solution is limited, and the taiji stone fiber/silk thread cannot well exert the far infrared and antibacterial effects of the taiji stone. The technical scheme provided by the invention is as follows:
a preparation method of antibacterial far infrared health care acrylic fiber comprises the following steps:
(1) taiji stone surface antibacterial enhancement modification
Dispersing a certain amount of the tai chi stone nano powder into deionized water, enabling the proportion of the tai chi stone nano powder to be 10-20 g/100mL, adding an inorganic dispersing agent accounting for 1-5 wt% of the tai chi stone nano powder, stirring to enable the tai chi stone nano powder to be fully dispersed to form a uniform dispersion liquid, then dropwise adding an antibacterial reinforcing agent trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride into the dispersion liquid while stirring, enabling the proportion of the antibacterial reinforcing agent to be 0.5-1.2 g/100mL, adjusting the pH value to be 4-7, continuously reacting for 12-24 hours at the temperature of 60-80 ℃, centrifugally purifying by using a precipitating agent after the reaction is finished, and drying a final product in a vacuum drying oven at a high temperature after centrifugal purification to obtain the antibacterial reinforced modified tai chi stone nano powder;
(2) preparation of antibacterial far infrared health acrylic fiber
Mixing the antibacterial enhanced modified tai chi stone nano powder obtained in the step (1) with an amino coupling agent in a proportion of 5: 1-5: 2 in a mass ratio of 50 to 80mL/g, and then, mixing acrylic fibers in a bath ratio of 1:20 to 1:50, adding the mixture into the dispersion, reacting at 40-100 ℃ for 8-12 h, washing with a large amount of organic solvent after the reaction is finished, washing with a large amount of deionized water, and drying in the air under natural conditions to obtain the antibacterial far infrared health acrylic fiber.
Preferably, in the step (1), the inorganic dispersant is sodium tripolyphosphate, sodium hexametaphosphate or sodium pyrophosphate.
Preferably, in step (1), the pH is adjusted by adding dilute nitric acid, acetic acid or phosphoric acid.
Preferably, in the step (1), the precipitant is absolute ethyl alcohol, and the addition amount of the precipitant is 1/5-1/3 of the volume of the solution after the reaction.
Preferably, in the step (2), the amino coupling agent is aminopropyltrimethoxysilane or 3-aminopropyltriethoxysilane or gamma-aminoethylaminopropyltrimethoxysilane.
Preferably, in the step (2), the organic solvent is a mixture of tetrahydrofuran and deionized water, ethanol and deionized water, or ethyl acetate and deionized water.
Preferably, in the step (1), the tai chi stone nano powder is fully dried to remove surface moisture before being dispersed in deionized water.
In addition, the invention also provides the antibacterial far infrared health care acrylic fiber prepared by the preparation method of the antibacterial far infrared health care acrylic fiber.
In addition, the invention also provides the application of the antibacterial far infrared health care acrylic fiber, which is characterized by being applied to underwear, underpants, socks, sportswear, swimwear, sun protection clothes and home textile fabrics.
The beneficial technical effects obtained by the invention are as follows:
1. the invention breaks through the conventional method for preparing the raw material fibril containing the tai chi stone by adding the tai chi stone nano powder into the spinning solution, and the tai chi stone is chemically combined with the surface of the acrylic fiber in a post-finishing mode, so that the fiber product can permanently and maximally exert the antibacterial and far infrared effects of the tai chi stone;
2. according to the invention, firstly, the surface antibacterial enhancement modification is carried out on the tai chi stone nano powder through an inorganic dispersant and an antibacterial enhancer trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, wherein the trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride contains a cationic antibacterial group, the antibacterial performance is stable, a silicon-oxygen bond in a molecule is easy to hydrolyze in water and reacts with a hydroxyl on the surface of an inorganic substance to form silanol, and a small amount of trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride reacts with a part of hydroxyl on the surface of the tai chi stone to form a covalent bond, so that the tai chi stone has better antibacterial performance; after the surface antibacterial enhancement modification of the tai chi stone nano powder, an amino coupling agent and deionized water form a dispersion solution, and acrylic fibers are soaked in the dispersion solution for reaction at a certain bath ratio and under certain reaction conditions; the amino silane coupling agent has a silicon-oxygen-carbon bond, can react with residual hydroxyl on the surface of the taiji stone on one hand, and has amino on the other hand as a bonding promoter of a nitrile polymer, so that the antibacterial reinforced taiji stone and acrylic fiber are tightly combined together, the antibacterial and far infrared effects of the taiji stone are more obvious, and the antibacterial and far infrared effects of the taiji stone are hardly weakened after multiple times of water washing;
3. the post-finishing treatment method is simple, has high cost performance, mild treatment process conditions and small damage to the performance of the acrylic fiber, and optimizes post-finishing process parameters through multiple tests, thereby endowing the taiji stone acrylic fiber product with lasting, remarkable antibacterial and far infrared health-care effects; the far infrared emissivity reaches more than 93 percent; the antibacterial property to staphylococcus aureus, escherichia coli and candida albicans reaches more than 97.8%, 94.2% and 96.5% respectively.
Drawings
FIG. 1 is a microscope image of the surface morphology of antibacterial far infrared health acrylic fiber in the representative example (example 2) of the present invention;
FIG. 2 is a graph showing the results of an antibacterial test control of antibacterial far infrared health acrylic fibers in an exemplary embodiment (example 2) of the present invention, in which
A is a golden yellow staphylococcus blank sample agar plate picture; b is a golden yellow staphylococcus test sample agar plate picture; c is a diagram of an agar plate of a blank sample of the escherichia coli ball; d is an agar plate picture of an escherichia coli test sample; e is a Candida albicans blank agar plate picture; f is the picture of an agar plate of a candida albicans test sample.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It is to be understood that these examples are for purposes of illustration only and are not intended to limit the scope of the present invention, which is to be construed as merely preferred or presently preferred embodiments of the invention; further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the technical contents of the present invention, and those equivalents also fall within the scope of the present invention defined by the appended claims.
Example 1
A preparation method of antibacterial far infrared health care acrylic fiber comprises the following steps:
(1) the surface of the Taiji stone is antibacterial, enhanced and modified. Dispersing 10g of commercially available tai chi stone nano powder into 100mL of deionized water, adding sodium tripolyphosphate accounting for 1 wt% of the tai chi stone nano powder, stirring to fully disperse the tai chi stone nano powder to form a uniform dispersion liquid, then dropwise adding 0.5g of trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride serving as an antibacterial enhancer into the dispersion liquid while stirring, dropwise adding dilute nitric acid or acetic acid or phosphoric acid, adjusting the pH to be 4, and continuously reacting for 12 hours at 60 ℃, wherein the trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride contains a cationic antibacterial group and has stable antibacterial performance, a silicon-oxygen carbon bond in a molecule is easy to hydrolyze in water and reacts with hydroxyl on the surface of an inorganic substance to form silanol, and a small amount of trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride reacts with partial hydroxyl on the surface of the tai stone to ensure that the tai stone has better antibacterial performance, and after the reaction is finished, carrying out centrifugal purification by adopting absolute ethyl alcohol accounting for 1/5 volume of the solution after the reaction, and drying the final product in a vacuum drying oven at room temperature after the centrifugal purification to obtain the antibacterial enhanced modified taiji stone nano powder.
(2) Preparing antibacterial far infrared health acrylic fiber. Mixing the antibacterial enhanced modified tai chi stone nano powder obtained in the step (1) with aminopropyl trimethoxy silane in a ratio of 5: 1 is fully dispersed in deionized water to form dispersion liquid, the proportion of the deionized water to the antibacterial reinforced modified tai chi stone nano powder is 50mL/g, then acrylic fibers are added into the dispersion liquid in a bath ratio of 1:20, the mixture reacts for 8 hours at 40 ℃, an aminosilane coupling agent has a silica-carbon bond, on one hand, the aminosilane coupling agent can react with residual hydroxyl on the surface of the tai chi stone, on the other hand, amino groups are arranged as an adhesion promoter of a nitrile polymer, the antibacterial reinforced tai chi stone and the acrylic fibers are tightly combined together, after the reaction is finished, the mixture is washed by a large amount of mixed solvent of tetrahydrofuran and deionized water in a volume ratio of 7:3, then the mixture is washed by a large amount of deionized water, and finally the mixture is dried in the air under natural condition, so that the antibacterial far infrared health care acrylic fibers.
Example 2
A preparation method of antibacterial far infrared health care acrylic fiber comprises the following steps:
(1) the surface of the Taiji stone is antibacterial, enhanced and modified. Fully drying 15g of commercial tai chi stone nano powder to remove surface moisture, dispersing the tai chi stone nano powder in 100mL of deionized water, fully drying the tai chi stone nano powder to facilitate the tai chi stone nano powder to be rapidly and uniformly dispersed in an aqueous solution with a dispersing agent, adding sodium hexametaphosphate accounting for 3 wt% of the tai chi stone nano powder, stirring the mixture to fully disperse the mixture to form a uniform dispersion liquid, then dropwise adding 0.8g of antibacterial enhancer trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride into the dispersion liquid while stirring the mixture, dropwise adding dilute nitric acid or acetic acid or phosphoric acid into the mixture to adjust the pH to be 6, continuously reacting the mixture for 16 hours at the condition of 75 ℃, wherein the trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride contains a cationic antibacterial group and has stable antibacterial performance, and silicon oxygen bonds in molecules of the silicon oxygen are easily hydrolyzed in water and react with hydroxyl on the surface of inorganic matters to form silanol, and (2) reacting a small amount of trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride with partial hydroxyl on the surface of the tai chi stone to ensure that the tai chi stone has better antibacterial performance, centrifugally purifying by using anhydrous ethanol accounting for 1/4 of the volume of the solution after reaction, and drying the final product in a vacuum drying oven at room temperature after centrifugal purification to obtain the antibacterial enhanced modified tai chi stone nano powder.
(2) Preparing antibacterial far infrared health acrylic fiber. Mixing the antibacterial enhanced modified tai chi stone nano powder obtained in the step (1) with 3-aminopropyl triethoxysilane by the following ratio of 10: 3, fully dispersing the deionized water in the deionized water to form a dispersion liquid, enabling the proportion of the deionized water to the antibacterial reinforced modified tai chi stone nano powder to be 65mL/g, then adding acrylic fibers into the dispersion liquid in a bath ratio of 1:35, then reacting for 10 hours at 70 ℃, wherein an aminosilane coupling agent has a silica-carbon bond, can react with residual hydroxyl on the surface of the tai chi stone on one hand, and has amino on the other hand as a bonding promoter of a nitrile polymer, so that the antibacterial reinforced tai chi stone and the acrylic fibers are tightly combined together, after the reaction is finished, washing by a large amount of mixed solvent of ethanol and deionized water in a volume ratio of 7:3, then washing by a large amount of deionized water, and finally airing under natural conditions to obtain the antibacterial far infrared health-care acrylic fibers. In this embodiment, as a representative example, the inventor of the present application uses the sample of this embodiment as an observation object, and performs scanning electron microscope observation on the antibacterial far infrared health acrylic fiber prepared from the sample, wherein the acrylic fiber surface is clearly distributed with denser antibacterial enhanced modified tayaite nano powder particles, and an electron microscope image thereof is shown in fig. 1.
Example 3
A preparation method of antibacterial far infrared health care acrylic fiber comprises the following steps:
(1) the surface of the Taiji stone is antibacterial, enhanced and modified. Fully drying 20g of commercially available tai chi stone nano powder to remove surface moisture, dispersing the tai chi stone nano powder in 100mL of deionized water, adding sodium pyrophosphate accounting for 5 wt% of the tai chi stone nano powder, stirring to fully disperse the tai chi stone nano powder to form uniform dispersion, then dropwise adding 1.2g of trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride serving as an antibacterial enhancer into the dispersion while stirring, dropwise adding dilute nitric acid or acetic acid or phosphoric acid, adjusting the pH to be 7, continuously reacting for 24 hours at 80 ℃, wherein trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride contains cationic antibacterial groups, the antibacterial property is stable, silicon-oxygen bonds in molecules are easily hydrolyzed in water and react with hydroxyl on the surface of an inorganic substance to form silanol, and a small amount of trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride reacts with partial hydroxyl on the surface of the tai stone to enable the tai chi stone to have better antibacterial property, and after the reaction is finished, carrying out centrifugal purification by adopting absolute ethyl alcohol accounting for 1/3 volume of the solution after the reaction, and drying the final product in a vacuum drying oven at room temperature after the centrifugal purification to obtain the antibacterial enhanced modified taiji stone nano powder.
(2) Preparing antibacterial far infrared health acrylic fiber. Mixing the antibacterial reinforced modified tai chi stone nano powder obtained in the step (1) with gamma-aminoethyl aminopropyl trimethoxysilane by the weight ratio of 5: 2, fully dispersing the deionized water in the deionized water to form a dispersion liquid, enabling the ratio of the deionized water to the antibacterial enhanced modified tai chi stone nano powder to be 80mL/g, then adding acrylic fibers into the dispersion liquid in a bath ratio of 1:50, then reacting for 12 hours at 100 ℃, wherein an aminosilane coupling agent has a silica-carbon bond, can react with residual hydroxyl on the surface of the tai chi stone on one hand, and has amino on the other hand as a bonding promoter of a nitrile polymer, so that the antibacterial enhanced tai chi stone and the acrylic fibers are tightly combined together, after the reaction is finished, washing by a large amount of mixed solvent of ethyl acetate and deionized water in a volume ratio of 7:3, then washing by a large amount of deionized water, and finally airing under natural conditions to obtain the antibacterial far infrared health-care acrylic fibers.
The antibacterial far infrared health care acrylic fiber prepared by the embodiments 1 to 3 of the invention has good antibacterial property and far infrared property, and the acrylic fiber is especially suitable for being applied to underwear, underpants, socks, sportswear, swimwear, sun protection clothes and home textile fabrics.
Examples 1-3 Performance testing of post-finished acrylic fibers
1. The far infrared performance test of the acrylic fiber prepared in examples 1 to 3 of the present invention was carried out in accordance with GB/T30127-2013 for detecting and evaluating far infrared performance of textile, and the test results are shown in Table 1.
Table 1 examples 1-3 test results of far infrared performance of antibacterial far infrared health acrylic fiber
| Source of test sample | Far infrared emissivity | Far infrared wavelength range | Far infrared radiation temperature rise value |
| Example 1 | 93％ | 10～15μm | 1.7℃ |
| Example 2 | 95％ | 10～15μm | 1.7℃ |
| Example 3 | 95％ | 10～15μm | 1.7℃ |
According to the test result, the antibacterial far infrared health acrylic fiber produced by the production method has the far infrared emissivity of over 93 percent, the far infrared radiation temperature rise value of 1.7 ℃, the far infrared emissivity exceeds the technical requirements of textile materials on far infrared performance test, namely the far infrared emissivity is more than or equal to 88 percent, the far infrared radiation temperature rise value is more than or equal to 1.4 ℃, the far infrared wavelength range of the antibacterial far infrared health acrylic fiber is close to the wavelength of a human body, and the emitted far infrared is absorbed by the human body, so that the antibacterial far infrared health acrylic fiber can promote the blood circulation and metabolism of the human body, improve the immunity of the human body.
2. According to GB/T20944.3-2008, evaluation of antibacterial performance of textiles part 3: oscillation method, antibacterial effect tests of staphylococcus aureus (AATCC6538), escherichia coli (AATCC8739) and candida albicans (AATCC 10231) were performed on the acrylic fibers prepared in examples 1 to 3 of the present invention, and the test results are shown in table 2.
Table 2 examples 1-3 antibacterial far infrared health acrylic fiber antibacterial property test results
By adopting the method, the tai chi stone nano powder has higher antibacterial performance by the surface modification of the antibacterial reinforcing agent trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, and the amino group of the aminosilane coupling agent can be used as the adhesion promoter of the nitrile polymer to tightly combine the antibacterial reinforcing tai chi stone and the acrylic fiber; the acrylic fiber has remarkable antibacterial and far infrared effects, can keep permanent antibacterial and far infrared performances, is soaked and washed for multiple times, and the antibacterial and far infrared performances of a test sample after being soaked and washed for 30 times are almost not weakened.
The above embodiments of the present invention and the experimental results thereof are described in detail, and it will be apparent to those skilled in the art that the embodiments may be changed, modified, replaced, integrated and modified in the process parameters without departing from the spirit and the principle of the present invention.
Claims (9)
1. The preparation method of the antibacterial far infrared health acrylic fiber is characterized by comprising the following steps:
(1) taiji stone surface antibacterial enhancement modification
Dispersing a certain amount of the tai chi stone nano powder into deionized water, enabling the proportion of the tai chi stone nano powder to be 10-20 g/100mL, adding an inorganic dispersing agent accounting for 1-5 wt% of the tai chi stone nano powder, stirring to enable the tai chi stone nano powder to be fully dispersed to form a uniform dispersion liquid, then dropwise adding an antibacterial reinforcing agent trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride into the dispersion liquid while stirring, enabling the proportion of the antibacterial reinforcing agent to be 0.5-1.2 g/100mL, adjusting the pH value to be 4-7, continuously reacting for 12-24 hours at the temperature of 60-80 ℃, centrifugally purifying by using a precipitating agent after the reaction is finished, and drying a final product in a vacuum drying oven at a high temperature after centrifugal purification to obtain the antibacterial reinforced modified tai chi stone nano powder;
(2) preparation of antibacterial far infrared health acrylic fiber
Mixing the antibacterial enhanced modified tai chi stone nano powder obtained in the step (1) with an amino coupling agent in a proportion of 5: 1-5: 2 in a mass ratio of 50 to 80mL/g, and then, mixing acrylic fibers in a bath ratio of 1:20 to 1:50, adding the mixture into the dispersion, reacting at 40-100 ℃ for 8-12 h, washing with a large amount of organic solvent after the reaction is finished, washing with a large amount of deionized water, and drying in the air under natural conditions to obtain the antibacterial far infrared health acrylic fiber.
2. The method for preparing antibacterial far infrared health acrylic fiber as claimed in claim 1, wherein in step (1), the inorganic dispersant is sodium tripolyphosphate, sodium hexametaphosphate or sodium pyrophosphate.
3. The method for preparing antibacterial far infrared health acrylic fiber as claimed in claim 1, wherein in the step (1), the pH value is adjusted by adding dilute nitric acid, acetic acid or phosphoric acid.
4. The method for preparing antibacterial far infrared health care acrylic fiber according to any one of claims 1 to 3, characterized in that in the step (1), the precipitant is absolute ethyl alcohol, and the addition amount is 1/5-1/3 of the volume of the solution after reaction.
5. The method for preparing antibacterial far infrared health acrylic fiber as claimed in any one of claims 1 to 3, wherein in the step (2), the amino coupling agent is aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane or gamma-aminoethylaminopropyltrimethoxysilane.
6. The method for preparing antibacterial far infrared health acrylic fiber as claimed in any one of claims 1 to 3, wherein in the step (2), the organic solvent is a mixture of tetrahydrofuran and deionized water, ethanol and deionized water, or ethyl acetate and deionized water.
7. The method for preparing antibacterial far infrared health acrylic fiber according to any one of claims 1 to 3, wherein in the step (1), the taalite nano powder is fully dried to remove surface moisture before being dispersed in deionized water.
8. An antibacterial far infrared health acrylic fiber prepared by the preparation method of the antibacterial far infrared health acrylic fiber according to any one of claims 1 to 7.
9. The use of the antibacterial far infrared health acrylic fiber according to claim 8, characterized in that it is applied to underwear, underpants, socks, sportswear, swimwear, sun protection clothes and home textile fabrics.
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