CN114277576A - Preparation method of Cu-MOFs-loaded multifunctional cotton fabric - Google Patents
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Abstract
本发明涉及功能纺织品制备技术领域，具体涉及一种负载Cu‑MOFs的多功能棉织物的制备方法，包括以下步骤：步骤一、采用多元羧酸对棉织物进行改性；步骤二、采用层层组装法在室温下将Cu‑MOFs负载到棉织物上，赋予棉织物抗菌、吸附、光催化等多种功能。本发明通过先在棉织物上引入羧基，吸附铜离子，再采用层层组装法，利用铜离子与ZnO纳米粒子结合，形成(Zn、Cu)羟基双盐中间体，提高阴离子交换速率，在室温下快速将Cu‑MOFs负载到棉织物上。本发明具有能耗小，设备简单，操作方便等特点。所制备的负载Cu‑MOFs的多功能棉织物具有广阔的应用前景。
The invention relates to the technical field of preparation of functional textiles, in particular to a preparation method of a multifunctional cotton fabric loaded with Cu-MOFs, comprising the following steps: step 1, modifying the cotton fabric with polybasic carboxylic acid; step 2, adopting layer by layer The assembly method loads Cu-MOFs onto cotton fabrics at room temperature, which endow cotton fabrics with multiple functions such as antibacterial, adsorption, and photocatalysis. The invention firstly introduces carboxyl groups on cotton fabrics, absorbs copper ions, and then adopts a layer-by-layer assembly method to combine copper ions with ZnO nano-particles to form (Zn, Cu) hydroxyl double salt intermediates, improve the anion exchange rate, at room temperature. The Cu-MOFs were rapidly loaded onto cotton fabrics. The invention has the characteristics of low energy consumption, simple equipment, convenient operation and the like. The prepared multifunctional cotton fabric loaded with Cu-MOFs has broad application prospects.
Description
Technical Field
The invention relates to the technical field of functional textile preparation, in particular to a preparation method of a Cu-MOFs loaded multifunctional cotton fabric.
Background
Metal organic framework Materials (MOFs), as a class of novel porous materials formed by coordination assembly of organic ligands and inorganic structural units (metal ions or metal clusters), have microporous, mesoporous, and macroporous structures. The method has wide application in the fields of gas phase adsorption and separation, liquid phase adsorption and separation, drug release, photocatalysis, antibiosis and the like. Copper is one of the essential trace elements for human body, and although copper has good biocompatibility, the release rate of metal ions is difficult to control in the antibacterial process of the traditional copper nanoparticles, and certain damage can be caused to the normal tissues of the human body. Compared with copper nanoparticles, the Cu-MOFs has the characteristics of high specific surface area, controllable ion release speed, flexible chemical structure and the like, and has larger application potential.
The common preparation method of Cu-MOFs is a solvothermal method. For example, patent No. cn202111084845.x discloses a method for preparing copper metal organic frame material, which promotes the growth of crystal nucleus by high temperature condition, and consumes a large amount of energy. 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; the problem of poor water stability in the catalytic process and the like, researchers are dedicated to combining Cu-MOFs and fiber materials to improve the performance and widen the application. The common methods mainly comprise in-situ growth, electrostatic spinning, self-assembly and the like. The in-situ growth method is that metal ions or organic ligands in precursor solution are attached to the fiber and are used as nucleation sites to continuously grow crystals, and Cu-MOFs are induced to be generated on the surface of the fiber. However, because of the fast nucleation speed, the final particle size is generally large, and is difficult to be firmly attached to the fiber, and the water stability of the Cu-MOFs is also poor, the structure is easy to collapse, and the method has certain limitations. The electrostatic spinning method is to mix Cu-MOFs with polymer solution and carry out jet spinning in a strong electric field to form the nano-fiber. Compared with the traditional in-situ growth method, the Cu-MOFs can be more uniformly dispersed on the fiber and has higher specific surface area and porosity, but part of the Cu-MOFs is encapsulated by hydrophobic polymers, and the use performance is limited. The layer-by-layer assembly method is characterized in that the fiber base material is alternately immersed into a solution of metal ion solution and ligand at normal temperature, and the reaction is repeated for many times in a circulating manner so as to increase the number of nucleation sites for Cu-MOFs crystal growth and synthesize Cu-MOFs on the surface of the fiber layer by layer. The method is simple to operate, the generated particles are uniformly distributed, but the process takes longer time.
In order to solve the problems, the application needs to provide a preparation method of the multifunctional cotton fabric loaded with the Cu-MOFs.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a multifunctional cotton fabric loaded with Cu-MOFs, which comprises the steps of introducing carboxyl on the cotton fabric, adsorbing copper ions, adopting a layer-by-layer assembly method, forming a (Zn, Cu) hydroxyl double-salt intermediate by combining the copper ions and ZnO nanoparticles, improving the anion exchange rate, and quickly loading the Cu-MOFs on the cotton fabric with wide application and low cost at room temperature, so that the problems that powdery Cu-MOFs are easy to agglomerate, difficult to recover, low in reuse rate and the like can be solved, and meanwhile, multiple functions of antibiosis, adsorption, photocatalysis and the like can be endowed to the cotton fabric, and the method has the advantages of low energy consumption, simple equipment, convenience in operation and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a Cu-MOFs loaded multifunctional cotton fabric comprises the following specific steps:
step one, modifying cotton fabrics by adopting polycarboxylic acid: soaking the cotton fabric in an aqueous solution containing 4 wt% of polycarboxylic acid and 4 wt% of sodium hypophosphite for 5min, rolling by using a padder, and soaking and rolling twice; pre-baking the padded cotton fabric at 100 ℃ for 3min, and finally baking at 180 ℃ for 3min to obtain a modified cotton fabric;
step two, loading Cu-MOFs on the cotton fabric by adopting a layer-by-layer assembly method: preparing 0.02-0.1M copper salt aqueous solution A, and soaking the modified cotton fabric obtained in the step one in the solution A for 10 min; then adding 0.02-0.1M nano ZnO dispersion liquid into the solution A, quickly stirring to form a hydroxyl double-salt solution B, continuously soaking the modified cotton fabric in the solution B for 10-20min, and taking out; taking ethanol and N, N-dimethylformamide with a volume ratio of 1:1 as solvents, preparing 0.05-0.1M trimesic acid solution C, dipping the taken modified cotton fabric in the solution C for 10-20min, and taking out; and (3) circularly and alternately dipping the modified cotton fabric in the solution B and the solution C, assembling the modified cotton fabric layer by layer, taking out the fabric, washing the fabric with water, and drying the fabric to obtain the multifunctional cotton fabric.
Preferably, in the first step, the cotton fabric can be cotton woven fabric or knitted fabric; the polycarboxylic acid is one of citric acid, butanetetracarboxylic acid and polymaleic acid.
Preferably, in the second step, the copper salt is one of copper nitrate, copper sulfate and copper chloride.
Preferably, in the second step, the added nano ZnO has the particle size of 30-50 nm.
Preferably, in the second step, the layer-by-layer assembly method is performed at room temperature.
Preferably, in the second step, the dipping bath ratio of the modified cotton fabric is 1: 10-1: 30.
Preferably, in the second step, the number of times of circularly and alternately impregnating is 1-10 times.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, carboxyl is introduced on the cotton fabric to adsorb copper ions, so that the binding fastness of Cu-MOFs and the cotton fabric can be improved.
2. According to the method, copper ions are combined with ZnO nanoparticles to form a (Zn, Cu) hydroxyl double-salt intermediate, the anion exchange rate is improved, and Cu-MOFs can be quickly loaded on cotton fabrics only at room temperature.
3. According to the invention, the Cu-MOFs is uniformly distributed on the cotton fabric which is wide in application and low in cost, so that the problems that powdery Cu-MOFs is easy to agglomerate and difficult to recover and the reuse rate is low can be solved, meanwhile, the cotton fabric can be endowed with multiple functions of antibiosis, adsorption, photocatalysis and the like, and the application prospect is wide.
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 Scanning Electron Microscope (SEM) photograph of a product of example 1 of the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of a product in example 2 of the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) photograph of the product of example 3 of the 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, a preparation method of a Cu-MOFs loaded multifunctional cotton fabric comprises the following specific steps:
step one, modifying cotton fabrics by adopting butanetetracarboxylic acid: soaking the cotton fabric in an aqueous solution containing 4 wt% of butanetetracarboxylic acid and 4 wt% of sodium hypophosphite for 5min, rolling by using a padder, and soaking twice and rolling twice. Pre-baking the padded cotton fabric at 100 ℃ for 3min, and finally baking the padded cotton fabric at 180 ℃ for 3min to obtain the modified cotton fabric.
Step two, loading Cu-MOFs on the cotton fabric by adopting a layer-by-layer assembly method: preparing 0.02M aqueous solution A of copper nitrate trihydrate, and soaking the modified cotton fabric in the solution A for 10 min. And then adding 0.02M nano ZnO dispersion liquid into the solution A, quickly stirring to form a hydroxyl double-salt solution B, continuously soaking the modified cotton fabric in the solution B for 10min, and taking out the modified cotton fabric. Ethanol and N, N-dimethylformamide with the volume ratio of 1:1 are used as solvents, 0.05M trimesic acid solution C is prepared, and the taken modified cotton fabric is taken out after being soaked in the solution C for 10 min. And (3) circularly and alternately dipping the modified cotton fabric in the solution B and the solution C for 3 times, taking out the fabric, washing with water, and drying to obtain the multifunctional cotton fabric.
Example 2:
referring to fig. 2, a preparation method of a Cu-MOFs loaded multifunctional cotton fabric comprises the following specific steps:
step one, modifying cotton fabrics by adopting citric acid: soaking the cotton fabric in an aqueous solution containing 4 wt% of citric acid and 4 wt% of sodium hypophosphite for 5min, rolling by using a padder, and soaking and rolling twice. Pre-baking the padded cotton fabric at 100 ℃ for 3min, and finally baking the padded cotton fabric at 180 ℃ for 3min to obtain the modified cotton fabric.
Step two, loading Cu-MOFs on the cotton fabric by adopting a layer-by-layer assembly method: preparing 0.1M aqueous solution A of copper sulfate pentahydrate, and soaking the modified cotton fabric in the solution A for 10 min. And then adding 0.1M nano ZnO dispersion liquid into the solution A, quickly stirring to form a hydroxyl double-salt solution B, continuously soaking the modified cotton fabric in the solution B for 10min, and taking out the modified cotton fabric. Ethanol and N, N-dimethylformamide with the volume ratio of 1:1 are used as solvents, 0.1M trimesic acid solution C is prepared, and the taken modified cotton fabric is taken out after being soaked in the solution C for 10 min. And (3) circularly and alternately dipping the modified cotton fabric in the solution B and the solution C for 10 times, taking out the fabric, washing with water, and drying to obtain the multifunctional cotton fabric.
Example 3:
referring to fig. 3, a preparation method of a Cu-MOFs loaded multifunctional cotton fabric comprises the following specific steps:
step one, modifying cotton fabrics by adopting butanetetracarboxylic acid: soaking the cotton fabric in an aqueous solution containing 4 wt% of butanetetracarboxylic acid and 4 wt% of sodium hypophosphite for 5min, rolling by using a padder, and soaking twice and rolling twice. Pre-baking the padded cotton fabric at 100 ℃ for 3min, and finally baking the padded cotton fabric at 180 ℃ for 3min to obtain the modified cotton fabric.
Step two, loading Cu-MOFs on the cotton fabric by adopting a layer-by-layer assembly method: preparing 0.05M aqueous solution A of copper chloride dihydrate, and soaking the modified cotton fabric in the solution A for 10 min. And then adding 0.05M nano ZnO dispersion liquid into the solution A, quickly stirring to form a hydroxyl double-salt solution B, continuously soaking the modified cotton fabric in the solution B for 10min, and taking out the modified cotton fabric. Ethanol and N, N-dimethylformamide with the volume ratio of 1:1 are used as solvents, 0.05M trimesic acid solution C is prepared, and the taken modified cotton fabric is taken out after being soaked in the solution C for 10 min. And (3) circularly and alternately dipping the modified cotton fabric in the solution B and the solution C for 5 times, taking out the fabric, washing with water, and drying to obtain the multifunctional cotton fabric.
In conclusion, the invention firstly introduces carboxyl on the cotton fabric to adsorb copper ions, and then adopts a layer-by-layer assembly method to quickly load Cu-MOFs on the cotton fabric at room temperature, so as to prepare the cotton fabric with multiple functions of antibiosis, adsorption, photocatalysis and the like. The method has the advantages of low energy consumption, simple equipment, convenience in operation and the like, can solve the problems that powdery Cu-MOFs is easy to agglomerate and difficult to recover, has low reuse rate and the like, can endow cotton fabrics with multiple functions of antibiosis, adsorption, photocatalysis and the like, and 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 (7)
1. A preparation method of a Cu-MOFs loaded multifunctional cotton fabric is characterized by comprising the following specific steps:
step one, modifying cotton fabrics by adopting polycarboxylic acid: soaking the cotton fabric in an aqueous solution containing 4 wt% of polycarboxylic acid and 4 wt% of sodium hypophosphite for 5min, rolling by using a padder, and soaking and rolling twice; pre-baking the padded cotton fabric at 100 ℃ for 3min, and finally baking at 180 ℃ for 3min to obtain a modified cotton fabric;
step two, loading Cu-MOFs on the cotton fabric by adopting a layer-by-layer assembly method: preparing 0.02-0.1M copper salt aqueous solution A, and soaking the modified cotton fabric obtained in the step one in the solution A for 10 min; then adding 0.02-0.1M nano ZnO dispersion liquid into the solution A, quickly stirring to form a hydroxyl double-salt solution B, continuously soaking the modified cotton fabric in the solution B for 10-20min, and taking out; taking ethanol and N, N-dimethylformamide with a volume ratio of 1:1 as solvents, preparing 0.05-0.1M trimesic acid solution C, dipping the taken modified cotton fabric in the solution C for 10-20min, and taking out; and (3) circularly and alternately dipping the modified cotton fabric in the solution B and the solution C, assembling the modified cotton fabric layer by layer, taking out the fabric, washing the fabric with water, and drying the fabric to obtain the multifunctional cotton fabric.
2. The method for preparing the multifunctional cotton fabric loaded with the Cu-MOFs according to claim 1, wherein in the first step, the cotton fabric can be a cotton fabric or a knitted fabric; the polycarboxylic acid is one of citric acid, butanetetracarboxylic acid and polymaleic acid.
3. The method for preparing the multifunctional cotton fabric loaded with the Cu-MOFs according to claim 1, wherein in the second step, the copper salt is one of copper nitrate, copper sulfate and copper chloride.
4. The preparation method of the Cu-MOFs-loaded multifunctional cotton fabric according to claim 1, wherein in the second step, nano ZnO is added, and the particle size is 30-50 nm.
5. The method for preparing the multifunctional cotton fabric loaded with the Cu-MOFs according to claim 1, wherein in the second step, a layer-by-layer assembly method is performed at room temperature.
6. The preparation method of the Cu-MOFs-loaded multifunctional cotton fabric according to claim 1, wherein in the second step, the dipping bath ratio of the modified cotton fabric is 1: 10-1: 30.
7. The method for preparing the multifunctional cotton fabric loaded with the Cu-MOFs according to claim 1, wherein in the second step, the number of times of cyclic alternate dipping is 1-10.
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| CN114870817A (en) * | 2022-05-06 | 2022-08-09 | 南通大学 | Preparation method for improving water stability of Cu-BTC and application thereof |
| CN114875674A (en) * | 2022-05-06 | 2022-08-09 | 南通大学 | A kind of preparation method of antibacterial wool fabric loaded with PVP/Cu-MOFs |
| CN116676779A (en) * | 2023-06-09 | 2023-09-01 | 南通大学 | A kind of preparation method of antibacterial antiultraviolet multifunctional cotton fabric |
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