CN111996802B - Photodynamic sterilization ZIF-8 modified diacetate fiber and preparation method thereof - Google Patents
Photodynamic sterilization ZIF-8 modified diacetate fiber and preparation method thereof Download PDFInfo
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- CN111996802B CN111996802B CN202010870248.9A CN202010870248A CN111996802B CN 111996802 B CN111996802 B CN 111996802B CN 202010870248 A CN202010870248 A CN 202010870248A CN 111996802 B CN111996802 B CN 111996802B
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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
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
- D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
-
- 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
-
- 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
- D06M2101/08—Esters or ethers of cellulose
Abstract
The invention belongs to the field of functional textile materials, and discloses a preparation method of a photodynamic sterilization ZIF-8 modified diacetate fiber, which comprises the following steps: (1) dissolving cellulose diacetate sheets and zinc salt in a solvent, fully dissolving and uniformly mixing, and then spinning and drafting to prepare zinc salt composite cellulose diacetate tows; (2) soaking the zinc salt composite diacetate fiber tows into a 2-methylimidazole solution for reaction to prepare ZIF-8 modified diacetate fiber tows; (3) and finally, washing and drying the ZIF-8 modified diacetate fiber bundle, and removing the ZIF-8 particles which are not firmly combined to prepare the photodynamic sterilization ZIF-8 modified diacetate fiber. The invention utilizes ZIF-8 to efficiently and durably kill bacteria under the condition of illumination (sunlight or sunlight), has strong broad-spectrum antibacterial property and does not generate drug resistance. The photodynamic sterilization ZIF-8 modified diacetate fiber can be used for design and development of novel environment-friendly antibacterial textiles and medical and health materials.
Description
Technical Field
The invention belongs to the field of functional textile materials, and relates to a photodynamic sterilization ZIF-8 modified diacetate fiber and a preparation method thereof.
Background
Cellulose acetate is the earliest commercial production of cellulose derivatives and is a cellulose organic acid ester that is being developed. Cellulose diacetate is a spinning grade cellulose acetate, the most predominant use being as a filter material, with cigarette filters being the largest in use. In addition, the filter can also be used for medical filter equipment, such as a blood filter and the like. Meanwhile, the cellulose diacetate spinning can be used for manufacturing garment materials, such as linings of high-grade western-style clothes and the like.
The antibacterial modification of diacetate fibers is always a research hotspot at present. The existing modification method mainly comprises the means of adding antibacterial nano particles (such as nano silver, nano copper and the like), finishing after an antibacterial agent (such as quaternary ammonium salt finishing), blending with antibacterial fibers (such as chitosan fibers) and the like. The method has the problems of low antibacterial efficiency, poor antibacterial durability, disputed human body safety of nano materials and the like.
Zeolite imidazolate framework material (ZIF-8) is one of metal organic framework materials, and has certain antibacterial property due to zinc ions. In addition, researches show that ZIF-8 can generate active oxygen free radicals under the irradiation of common sunlight, can kill bacteria efficiently, and has the sterilization efficiency as high as 99.9999%. Patent CN 108589399 a discloses a preparation method based on cellulose base/ZIF-8 composite material. However, the method is similar to surface post-finishing, and the prepared ZIF-8 is not high in binding degree with a cellulose substrate, is easy to fall off and is not beneficial to further application.
Disclosure of Invention
In view of the above, the invention provides a photodynamic sterilization ZIF-8 modified diacetate fiber and a preparation method thereof. The prepared photodynamic sterilization ZIF-8 modified diacetate fiber can generate a large amount of active oxygen free radicals under the irradiation of visible light (sunlight or lamplight), can kill bacteria with high efficiency and long-lasting broad spectrum, and cannot generate drug resistance.
In order to solve the above problems, the technical scheme provided by the invention is as follows:
a preparation method of a photodynamic sterilization ZIF-8 modified diacetate fiber comprises the following steps:
(1) dissolving cellulose diacetate sheets and zinc salt in a solvent, completely dissolving and uniformly mixing to obtain spinning stock solution, spinning and drafting the spinning stock solution, and volatilizing the solvent to obtain zinc salt composite diacetate fiber tows;
(2) soaking the composite diacetate fiber tows obtained in the step (1) into a 2-methylimidazole solution, reacting for 6-24 h, and taking out to obtain ZIF-8 modified diacetate fiber tows;
(3) and (3) flushing the ZIF-8 modified diacetate fiber tows obtained in the step (2) to remove the ZIF-8 particles which are not firmly combined, and then drying to obtain the photodynamic sterilization ZIF-8 modified diacetate fiber.
Preferably, the zinc salt is zinc nitrate hexahydrate or zinc acetate dihydrate, and the solvent is acetone.
Preferably, in the spinning solution, the mass concentration of the cellulose diacetate is 12-30 wt%, and the mass concentration of the zinc salt is 5-10 wt%.
Preferably, the spinning speed is 0.8-3 mL/min.
Preferably, in the step (2), the solvent of the 2-methylimidazole solution is one or more of methanol, ethanol and deionized water, the mass concentration of 2-methylimidazole in the 2-methylimidazole solution is 2-5 wt%, and the reaction temperature is room temperature.
Preferably, the flushing liquid used for flushing is one or more of methanol, ethanol and deionized water.
Preferably, the drying temperature is 20-50 ℃.
The invention also provides the photodynamic sterilization ZIF-8 modified diacetate fiber prepared by the preparation method.
Preferably, the diameter of the photodynamic sterilization ZIF-8 modified diacetate fiber is 0.5-2 μm.
The beneficial technical effects of the invention are as follows:
(1) according to the invention, the ZIF-8 precursor zinc salt and the cellulose diacetate solution are mixed for spinning, and 2-methylimidazole nucleation growth characteristic is utilized to load ZIF-8 particles on the surface of the composite cellulose diacetate fiber in situ, so that the obtained photodynamic sterilization ZIF-8 modified cellulose diacetate fiber has the characteristics of high bonding fastness and large loading capacity, is strong in water washing resistance, and can still maintain the initial antibacterial rate of more than 97.5% after being washed for 50 times. In addition, the preparation method provided by the invention has the advantages of simple process and low energy consumption, and is a clean production mode.
(2) The prepared photodynamic sterilization ZIF-8 modified diacetate fiber can generate a large amount of active oxygen free radicals under the irradiation of visible light (sunlight or lamplight), can kill bacteria efficiently and durably in a broad spectrum, can not generate drug resistance, and is expected to be applied to the design and development of novel environment-friendly antibacterial textiles and medical and sanitary materials.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and substance of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
Example 1
A preparation method of a photodynamic sterilization ZIF-8 modified diacetate fiber comprises the following steps:
(1) 6.3g of cellulose diacetate acetate pieces and 2.8g of zinc nitrate hexahydrate are weighed and added into 50mL of acetone to be stirred at room temperature until the mixture is completely dissolved and mixed to obtain a spinning stock solution, wherein the mass concentration of the cellulose diacetate is 13.1 wt% and the mass concentration of the zinc nitrate is 5.8 wt% in the spinning stock solution. Extruding the spinning stock solution out of a spinneret plate at the speed of 2mL/min, drafting, and standing until the solvent is volatilized to obtain a zinc salt composite diacetate fiber tow;
(2) soaking the zinc salt composite diacetate fiber tows obtained in the step (1) into 50mL of 2-methylimidazole solution with the mass concentration of 3 wt% to react for 12 hours at room temperature to obtain ZIF-8 modified diacetate fiber tows;
(3) washing the ZIF-8 modified diacetate fiber tows prepared in the step (2) by methanol, and drying in an oven at 30 ℃ to prepare the photodynamic sterilizing ZIF-8 modified diacetate fiber with the fiber diameter of 0.8 mu m.
Example 2
A preparation method of a photodynamic sterilization ZIF-8 modified diacetate fiber comprises the following steps:
(1) 8.2g of cellulose diacetate acetate tablets and 3.7g of zinc acetate dihydrate are weighed and added into 50mL of acetone, and stirred at room temperature until the mixture is completely dissolved and mixed to obtain spinning stock solution, wherein the mass concentration of the cellulose diacetate in the spinning stock solution is 16 wt%, and the mass concentration of the zinc acetate is 5.5 wt%. Extruding the spinning stock solution into a spinneret plate at the speed of 1.5mL/min, drafting, and standing until the solvent is volatilized to obtain zinc salt composite diacetate fiber tows;
(2) soaking the zinc salt composite diacetate fiber tows obtained in the step (1) into 50mL of 2-methylimidazole solution with the mass concentration of 4 wt% to react for 15 hours at room temperature to obtain ZIF-8 modified diacetate fiber tows;
(3) washing the ZIF-8 modified diacetate fiber tows prepared in the step (2) by ethanol, and drying in a 50 ℃ oven to prepare the photodynamic sterilization ZIF-8 modified diacetate fiber with the fiber diameter of 1.3 mu m.
Example 3
A preparation method of a photodynamic sterilization ZIF-8 modified diacetate fiber comprises the following steps:
(1) weighing 7.5g of cellulose diacetate acetate tablets and 4.6g of zinc acetate dihydrate, adding the mixture into 50mL of acetone, stirring at room temperature until the mixture is completely dissolved and mixed to obtain a spinning stock solution, wherein the mass concentration of the cellulose diacetate in the spinning stock solution is 14.7 wt%, and the mass concentration of the zinc acetate in the spinning stock solution is 9 wt%. Extruding the spinning stock solution out of a spinneret plate at the speed of 2mL/min, drafting, and standing until the solvent is volatilized to obtain a zinc salt composite diacetate fiber tow;
(2) soaking the zinc salt composite diacetate fiber tows obtained in the step (1) into 50mL of 2-methylimidazole solution with the mass concentration of 5wt% to react for 18 hours at room temperature to obtain ZIF-8 modified diacetate fiber tows;
(3) and (3) washing the ZIF-8 modified diacetate fiber tows prepared in the step (2) by deionized water, and drying in a drying oven at 40 ℃ to prepare the photodynamic sterilization ZIF-8 modified diacetate fiber with the fiber diameter of 1.6 mu m.
Example 4
A preparation method of a photodynamic sterilization ZIF-8 modified diacetate fiber comprises the following steps:
(1) 12.3g of cellulose diacetate acetate pieces and 5.7g of zinc nitrate hexahydrate are weighed and added into 50mL of acetone to be stirred at room temperature until the mixture is completely dissolved and mixed to obtain a spinning stock solution, wherein the mass concentration of the cellulose diacetate in the spinning stock solution is 21.6 wt%, and the mass concentration of the zinc nitrate in the spinning stock solution is 10 wt%. Extruding the spinning stock solution into a spinneret plate at the speed of 1mL/min, drafting, and standing until the solvent is volatilized to obtain a zinc salt composite diacetate fiber tow;
(2) soaking the zinc salt composite diacetate fiber tows obtained in the step (1) into 50mL of 2-methylimidazole solution with the mass concentration of 5wt% to react for 24 hours at room temperature to obtain ZIF-8 modified diacetate fiber tows;
(3) washing the ZIF-8 modified diacetate fiber tows prepared in the step (2) by ethanol, and drying in a 50 ℃ oven to prepare the photodynamic sterilization ZIF-8 modified diacetate fiber with the fiber diameter of 2 microns.
Test example 1
Respectively carrying out an antibacterial test on the common diacetate fibers and the photodynamic sterilization ZIF-8 modified diacetate fibers prepared in the embodiments 1-4, which specifically comprises the following steps:
and (3) antibacterial testing: selecting two environments of a darkroom and illumination (visible light) respectively, selecting staphylococcus aureus as a representative bacterium, and according to GB/T20944.2-2007 evaluation part 3 of antibacterial performance of textiles: the antibacterial performance of the diacetate fibers is tested by the oscillation method, and the test results are shown in table 1.
TABLE 1
As can be seen from table 1, the photodynamic sterilization ZIF-8 modified diacetate fibers prepared in embodiments 1 to 4 of the present invention have a bacterial survival rate of less than 1 ‰underillumination conditions, and compared with common diacetate fibers, the ZIF-8 modified diacetate fibers of the present invention have efficient and durable antibacterial properties.
Test example 2
Water wash resistance test: the photodynamic sterilization ZIF-8 modified diacetate fibers prepared in examples 1-4 were subjected to a water washing resistance test with reference to AATCC61-2010 color fastness to washing, and the test results are shown in Table 2 with the photodynamic sterilization retention rate after 50 washes as an evaluation parameter.
TABLE 2
| Test conditions | Example 1 | Example 2 | Example 3 | Example 4 |
| No water washing | 100％ | 100％ | 100％ | 100％ |
| Washing with water for 50 times | 97.8％ | 98.1％ | 98.6％ | 97.5％ |
As can be seen from Table 2, the photodynamic sterilization ZIF-8 modified diacetate fibers prepared in the embodiments 1-4 of the invention can still maintain the initial antibacterial rate of not less than 97.5% after being washed with water for 50 times. The ZIF-8 modified diacetate fiber has excellent washing resistance, and shows that ZIF-8 particles have high bonding fastness on the surface of the diacetate fiber and are not easy to fall off.
It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. A preparation method of a photodynamic sterilization ZIF-8 modified diacetate fiber is characterized by comprising the following steps:
(1) dissolving cellulose diacetate sheets and zinc salt in a solvent, completely dissolving and uniformly mixing to obtain spinning stock solution, spinning and drafting the spinning stock solution, and volatilizing the solvent to obtain zinc salt composite diacetate fiber tows;
the zinc salt is zinc nitrate hexahydrate or zinc acetate dihydrate, and the solvent is acetone;
in the spinning solution, the mass concentration of cellulose diacetate is 12-30 wt%, and the mass concentration of zinc salt is 5-10 wt%;
(2) soaking the composite diacetate fiber tows obtained in the step (1) into a 2-methylimidazole solution, reacting for 6-24 h, and taking out to obtain ZIF-8 modified diacetate fiber tows;
the solvent of the 2-methylimidazole solution is one or more of methanol, ethanol and deionized water, the mass concentration of 2-methylimidazole in the 2-methylimidazole solution is 2-5 wt%, and the reaction temperature is room temperature;
(3) washing the ZIF-8 modified diacetate fiber tows obtained in the step (2) to remove the ZIF-8 particles which are not firmly bonded, and then drying to obtain the photodynamic sterilization ZIF-8 modified diacetate fiber;
the flushing fluid used for flushing is one or more of methanol, ethanol and deionized water;
the drying temperature is 20-50 ℃.
2. The method of claim 1, wherein the spinning speed is 0.8 to 3 mL/min.
3. The photodynamic sterilized ZIF-8 modified diacetate fiber prepared by the preparation method of claim 1 or 2.
4. The photodynamic sterilization ZIF-8 modified diacetate fiber according to claim 3, wherein the diameter of the photodynamic sterilization ZIF-8 modified diacetate fiber is 0.5-2 μm.
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