CN114481621A - Preparation method of Cu-MOFs-loaded multifunctional wool - Google Patents
Preparation method of Cu-MOFs-loaded multifunctional wool Download PDFInfo
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- CN114481621A CN114481621A CN202210063530.5A CN202210063530A CN114481621A CN 114481621 A CN114481621 A CN 114481621A CN 202210063530 A CN202210063530 A CN 202210063530A CN 114481621 A CN114481621 A CN 114481621A
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
- D06M2101/12—Keratin fibres or silk
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- Polymers & Plastics (AREA)
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- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention relates to the technical field of functional fiber material preparation, in particular to a preparation method of Cu-MOFs loaded multifunctional wool, which comprises the following steps: step one, dissolving copper salt in deionized water to obtain a solution A, dispersing nano ZnO in the deionized water to obtain a dispersion liquid B, and adding the dispersion liquid B into the solution A under rapid stirring to obtain a hydroxyl double-salt solution C; step two, adding wool into the hydroxyl double-salt solution C, soaking for 10-30min, and taking out; dissolving trimesic acid in ethanol to obtain a solution D; soaking the wool taken out in the solution D for 10-30min and then taking out; and step five, circularly and alternately impregnating the wool in the solution C and the solution D. According to the invention, ethanol and water are used as solvents, and Cu-MOFs are rapidly loaded on wool at room temperature by a layer-by-layer assembly method, so that the wool has multiple functions of antibiosis, adsorption, drug release, photocatalysis and the like. The method has the characteristics of low cost, environmental protection, mild conditions and the like, and is convenient for industrial production.
Description
Technical Field
The invention relates to the technical field of functional fiber material preparation, in particular to a preparation method of Cu-MOFs loaded multifunctional wool.
Background
The copper-based metal organic framework material (Cu-MOFs) is made of Cu2+The novel three-dimensional organic-inorganic composite material is formed by connecting an organic ligand through a coordination bond, has a unique structure with extremely high specific surface area and abundant metal active sites, and has wide application in the fields of gas phase adsorption and separation, liquid phase adsorption and separation, drug release, photocatalysis, antibiosis and the like.
As the powdery Cu-MOFs have some disadvantages in application, such as the external force of a fluidized bed is needed to overcome the resistance among particles during gas adsorption, and the reduction of the contact area between the solid and the gas caused by particle deposition is prevented; the powder particles are difficult to collect during liquid adsorption, and the repeated utilization rate is low; poor water stability in the catalysis process and the like. The Cu-MOFs loaded on the fiber can effectively solve the problems.
The current common preparation method for loading Cu-MOFs on fabrics is a one-pot solvothermal method. For example, patent CN201811529778.6 discloses a preparation method of a fabric-based carrier modified organic metal framework compound, which promotes the growth of crystal nuclei on a fiber substrate through long-term high-temperature conditions, but the final product needs to be cooled to room temperature to precipitate, which wastes energy, and the organic solvent used in the patent contains a toxic solvent, N-dimethylformamide. Jianjiragku P et al convert Cu2+The solution, the organic ligand solution and the chitosan/PVA solution are directly mixed and are subjected to electrostatic spinning to form the nanofiber membrane, and the specific surface area of the composite material is improved by about 11 times compared with that of pure PVA nanofiber, so that the composite material becomes a potential material for selective gas adsorption and separation. However, the electrostatic spinning method can lead part of Cu-MOFs to be encapsulated by hydrophobic polymers, and the service performance is limited.
In order to solve the problems, the application needs to provide a preparation method of multifunctional wool loaded with Cu-MOFs.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of multifunctional wool loaded with Cu-MOFs, which comprises the steps of taking ethanol and water as solvents, firstly combining copper ions with ZnO nanoparticles to form a layered structure of a (Zn, Cu) hydroxyl double-salt intermediate, then alternately and circularly dipping wool in a hydroxyl double-salt solution and a ligand trimesic acid solution by a layer-by-layer assembly method, and loading the Cu-MOFs onto the wool at room temperature.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of Cu-MOFs loaded multifunctional wool comprises the following specific steps:
dissolving copper salt in deionized water to obtain a solution A, dispersing nano ZnO in the deionized water to obtain a dispersion liquid B, and adding the dispersion liquid B into the solution A under the condition of rapid stirring to obtain a hydroxyl double-salt solution C;
step two, adding wool into the hydroxyl double-salt solution C, soaking for 10-30min, and taking out;
dissolving trimesic acid in ethanol to obtain a solution D;
soaking the wool taken out in the solution D for 10-30min and then taking out;
and step five, circularly and alternately dipping the wool in the solution C and the solution D, finally taking out the wool, washing the wool with water, and drying the wool to obtain the multifunctional wool.
Preferably, in the first step, the copper salt is one of copper nitrate, copper sulfate and copper chloride, and the concentration of the copper salt aqueous solution is 15-30 g/L.
Preferably, in the first step, the diameter of the nano ZnO is 30-50nm, and the concentration is 20-40 g/L.
Preferably, in the third step, the concentration of the trimesic acid solution is 10-20 g/L.
Preferably, the bath ratio of the wool to the solution C and the solution D is 1:10 to 1: 30.
Preferably, in the fifth step, the number of times of circularly and alternately dipping is 1-5 times, and the dipping temperature is room temperature.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, copper ions are combined with ZnO nanoparticles to form a (Zn, Cu) hydroxyl double-salt intermediate, so that the anion exchange rate is improved, and Cu-MOFs can be rapidly loaded on wool at room temperature.
2. The invention loads Cu-MOFs to contain more functional groups (such as-COOH and-NH)2OH, etc.), not only can solve the problems that the powdery Cu-MOFs is easy to agglomerate and difficult to recycle, the reuse rate is low, etc., but also can improve the binding force of the Cu-MOFs and the fiber, and simultaneously can endow the wool with multiple functions of antibiosis, adsorption, drug release, photocatalysis, etc., and has wide application prospect.
3. The solvent used in the invention is only water and ethanol, and no other organic solvent is used, so that the method is green and environment-friendly, and can be recycled.
4. The invention has the advantages of low energy consumption, simple equipment, convenient operation and the like, and is convenient for industrial production.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of a sample in example 1 of the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) photograph of a sample in example 2 of the present invention;
FIG. 4 is a Scanning Electron Microscope (SEM) photograph of a sample in example 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings, so that those skilled in the art can better understand the advantages and features of the present invention, and thus the scope of the present invention is more clearly defined. The embodiments described herein are only a few embodiments of the present invention, rather than all embodiments, and all other embodiments that can be derived by one of ordinary skill in the art without inventive faculty based on the embodiments described herein are intended to fall within the scope of the present invention.
Example 1:
referring to fig. 1 and 2, a preparation method of multifunctional wool loaded with Cu-MOFs includes the following specific steps:
the method comprises the following steps: dissolving copper nitrate trihydrate into deionized water to obtain a copper nitrate solution A with the concentration of 20g/L, dispersing nano ZnO into the deionized water to obtain a dispersion liquid B with the concentration of 30g/L, and adding the dispersion liquid B into the copper nitrate solution A under the condition of rapid stirring to obtain a hydroxyl double-salt solution C.
Step two: adding wool into the solution C according to a bath ratio of 1:20, soaking for 20min, and taking out.
Step three: dissolving trimesic acid in ethanol to obtain a ligand solution D with the concentration of 15 g/L.
Step four: soaking the wool in the solution D for 20min at a bath ratio of 1:20, and taking out.
Step five: and (3) circularly and alternately dipping the wool in the solution C and the solution D for 5 times, finally taking out, washing with water, and drying to obtain the multifunctional wool.
The results of this example: the Scanning Electron Microscope (SEM) picture of the prepared multifunctional wool is shown in figure 2; reference is made to GB/T20944.3-2008 textile antibacterial performance evaluation part 3: the oscillation method tests show that the prepared multifunctional wool has the bacteriostasis rate of 100 percent to escherichia coli and staphylococcus aureus.
Example 2:
referring to fig. 1 and 3, a preparation method of multifunctional wool loaded with Cu-MOFs includes the following specific steps:
the method comprises the following steps: dissolving copper sulfate pentahydrate in deionized water to obtain a copper nitrate solution A with the concentration of 30g/L, dispersing nano ZnO in the deionized water to obtain a dispersion liquid B with the concentration of 40g/L, and adding the dispersion liquid B into the copper nitrate solution A under the condition of rapid stirring to obtain a hydroxyl double-salt solution C.
Step two: adding wool into the solution C according to the bath ratio of 1:30, soaking for 30min, and taking out.
Step three: dissolving trimesic acid in ethanol to obtain ligand solution D with the concentration of 20 g/L.
Step four: soaking the wool in the solution D for 30min at a bath ratio of 1:30, and taking out.
Step five: and (3) circularly and alternately dipping the wool in the solution C and the solution D for 3 times, finally taking out, washing with water, and drying to obtain the multifunctional wool.
The results of this example: the Scanning Electron Microscope (SEM) picture of the prepared multifunctional wool is shown in figure 3; reference is made to GB/T20944.3-2008 < evaluation of antibacterial properties of textiles part 3: the multifunctional wool prepared by the test of the oscillation method has the bacteriostasis rate of more than 95 percent to escherichia coli and staphylococcus aureus.
Example 3:
referring to fig. 1 and 4, a preparation method of multifunctional wool loaded with Cu-MOFs includes the following specific steps:
the method comprises the following steps: dissolving copper chloride dihydrate in deionized water to obtain a copper nitrate solution A with the concentration of 15g/L, dispersing nano ZnO in the deionized water to obtain a dispersion liquid B with the concentration of 20g/L, and adding the dispersion liquid B into the copper nitrate solution A under the condition of rapid stirring to obtain a hydroxyl double-salt solution C.
Step two: adding wool into the solution C according to a bath ratio of 1:10, soaking for 10min, and taking out.
Step three: dissolving trimesic acid in ethanol to obtain a ligand solution D with the concentration of 10 g/L.
Step four: and soaking the wool taken out in the solution D for 10min according to the bath ratio of 1:10, and then taking out.
Step five: and (3) circularly and alternately dipping the wool in the solution C and the solution D for 5 times, finally taking out, washing with water, and drying to obtain the multifunctional wool.
The results of this example: the Scanning Electron Microscope (SEM) picture of the prepared multifunctional wool is shown in figure 4; reference is made to GB/T20944.3-2008 < evaluation of antibacterial properties of textiles part 3: the multifunctional wool prepared by the test of the oscillation method has the bacteriostasis rate of more than 90 percent to escherichia coli and staphylococcus aureus.
In conclusion, ethanol and water are used as solvents, the (Zn, Cu) hydroxyl double salt is used for increasing the anion exchange rate, and Cu-MOFs are loaded on wool at room temperature by a layer-by-layer assembly method, so that the wool with multiple functions of antibiosis, adsorption, drug release, photocatalysis and the like is prepared. The method is energy-saving and environment-friendly, and is convenient for industrial production; the prepared multifunctional wool has wide application prospect.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (6)
1. A preparation method of Cu-MOFs loaded multifunctional wool is characterized by comprising the following specific steps:
dissolving copper salt in deionized water to obtain a solution A, dispersing nano ZnO in the deionized water to obtain a dispersion liquid B, and adding the dispersion liquid B into the solution A under the condition of rapid stirring to obtain a hydroxyl double-salt solution C;
step two, adding wool into the hydroxyl double-salt solution C, soaking for 10-30min, and taking out;
dissolving trimesic acid in ethanol to obtain a solution D;
soaking the wool taken out in the solution D for 10-30min and then taking out;
and step five, circularly and alternately dipping the wool in the solution C and the solution D, finally taking out the wool, washing the wool with water, and drying the wool to obtain the multifunctional wool.
2. The method as claimed in claim 1, wherein in the first step, the copper salt is one of copper nitrate, copper sulfate and copper chloride, and the concentration of the copper salt aqueous solution is 15-30 g/L.
3. The method for preparing multifunctional wool supporting Cu-MOFs according to claim 1, wherein in the first step, the diameter of nano ZnO is 30-50nm, and the concentration is 20-40 g/L.
4. The method for preparing multifunctional wool supporting Cu-MOFs according to claim 1, wherein in said step three, the concentration of the trimesic acid solution is 10-20 g/L.
5. The method for preparing the multifunctional wool supporting the Cu-MOFs according to claim 1, wherein the bath ratio of the wool to the solution C and the solution D is 1: 10-1: 30.
6. The method for preparing multifunctional wool supporting Cu-MOFs according to claim 1, wherein in the fifth step, the number of times of cyclically and alternately dipping is 1-5 times, and the dipping temperature is room temperature.
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2022
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