A method for preparing nano-zinc oxide loaded on the surface of cellulose fibers such as cotton and ramie.
By preparing sodium zincate solution and cationizing it on cotton and ramie cellulose fibers, combined with a double hydrolysis reaction, the problems of low loading and agglomeration of nano zinc oxide were solved, achieving uniform loading and efficient production.
Patent Information
- Application Number
- CN202410357553.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-27
- Publication Date
- 2025-12-02
- Estimated Expiration
- 2044-03-27
AI Technical Summary
Existing technologies for loading nano-zinc oxide onto cellulose fibers such as cotton and ramie suffer from problems such as low loading capacity and easy agglomeration.
By preparing sodium zincate solution as a precursor for nano-zinc oxide, and combining sodium hydroxide treatment and cationization treatment of cellulose fibers, nano-zinc oxide is generated on the surface of cellulose fibers through a double hydrolysis reaction, and then loaded using a simple aqueous phase process.
This method achieves uniform loading of nano-zinc oxide on the surface of cotton and ramie cellulose fibers, increases the loading capacity, and is simple, low-cost, suitable for large-scale production, and environmentally friendly.
Smart Images

Figure CN118065126B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a method for preparing functional textiles, and more particularly to a method for preparing nano-zinc oxide loaded on the surface of cellulose fibers such as cotton and ramie. Background Technology
[0002] Nano-zinc oxide is a widely used photocatalytic material with advantages such as low cost, non-toxicity, and stable performance, and is listed as a recognized safe substance by the U.S. Food and Drug Administration. In the textile industry, the combination of nano-zinc oxide and fibers can endow textiles with functional properties such as UV resistance, antibacterial properties, self-cleaning properties, and super-wetting properties. Currently, there are various methods for in-situ preparation of nano-zinc oxide on cellulose fibers (CF) such as cotton and ramie, including sol-gel method, hydrothermal method, chemical bath deposition, vapor deposition, magnetron sputtering, and atomic layer deposition. Among these methods, chemical bath deposition for forming a nano-zinc oxide layer on the surface of cellulose fibers such as cotton and ramie has a series of significant advantages. First, the reaction conditions of chemical bath deposition are mild, which can maximize the preservation of the excellent properties of cellulose fibers such as cotton and ramie, which is difficult to achieve with most processing methods. In addition, unlike vapor deposition and magnetron sputtering, chemical bath deposition methods do not require expensive equipment; and unlike hydrothermal methods and sol-gel methods, the reaction conditions of this method are easy to control, the cost is low, and it is more suitable for industrial-scale production. However, when chemical bath deposition technology is applied to the technical system of loading cellulose fibers such as cotton and ramie with nano zinc oxide, there is a problem of insufficient loading of nano zinc oxide due to the high crystallinity of cellulose fibers such as cotton and ramie, and the nano zinc oxide is prone to agglomeration on the fiber surface. Summary of the Invention
[0003] The technical problem to be solved by the present invention is to provide a method for preparing nano-zinc oxide loaded on the surface of cellulose fibers such as cotton and ramie, wherein the prepared cellulose fibers such as cotton and ramie are uniformly loaded with nano-zinc oxide, and the content of nano-zinc oxide exceeds 5%.
[0004] To solve the above-mentioned technical problems, the technical solution of the present invention is to provide a method for preparing nano-zinc oxide loaded on the surface of cotton and ramie cellulose fibers, characterized by comprising the following steps:
[0005] Step 1: Prepare sodium zincate (Na2ZnO2) solution as a precursor for nano-zinc oxide;
[0006] Step 2: Alkalinize cotton, ramie and other cellulose fibers in a 30% sodium hydroxide solution for 2 hours, then dehydrate and dry to obtain alkaline cellulose fibers;
[0007] Step 3: Impregnate the basic cellulose fibers obtained in Step 2 with a solution of 3-chloro-2-hydroxypropyltrimethylammonium chloride, react at 80°C for 20 min, wash with water and dry to obtain cationic cellulose fibers;
[0008] Step 4: Immerse the cationic cellulose fibers in the sodium zincate solution obtained in Step 1, and roll them dry after 2 hours, with a residual rate of 70%~120%;
[0009] Step 5: Immerse the treated cellulose fibers in zinc sulfate solution for 20 minutes, remove them and steam at 120°C for 20 minutes, wash with water and dry to prepare cellulose fibers with nano zinc oxide loaded on the surface.
[0010] Preferably, in step 1, the sodium zincate solution is prepared by completely dissolving 0.5g~1.0g of zinc hydroxide in 100mL of sodium hydroxide solution.
[0011] Preferably, in step 3, the concentration of the 3-chloro-2-hydroxypropyltrimethylammonium chloride solution is 10% to 30%.
[0012] Preferably, in step 5, the concentration of the zinc sulfate solution is 2% to 5%.
[0013] This invention first involves alkalizing cellulose fibers such as cotton and ramie in a 30% sodium hydroxide solution for 2 hours, followed by dehydration and drying to obtain alkaline cellulose fibers. These alkaline fibers are then reacted with a 3-chloro-2-hydroxypropyltrimethylammonium chloride solution to obtain cationic cellulose fibers. The cationic cellulose fibers can adsorb negatively charged zincate ions in a sodium zincate solution. Subsequently, in a zinc sulfate solution, sodium zincate and zinc sulfate undergo a double hydrolysis precipitation reaction on the surface of the cellulose fibers to generate zinc hydroxide. Finally, the zinc hydroxide is dehydrated during steaming, further growing to obtain nano-zinc oxide. Because sodium zincate adsorbs onto the cation sites of cellulose macromolecules, the cellulose macromolecules create a steric hindrance effect on the double hydrolysis precipitation reaction, inhibiting the growth of zinc oxide and promoting the formation of uniformly distributed nano-zinc oxide. Simultaneously, the double hydrolysis reaction fully utilizes the zinc element in sodium zincate and zinc sulfate to grow and prepare nano-zinc oxide, which helps to increase the loading of nano-zinc oxide on the surface of cellulose fibers such as cotton and ramie.
[0014] Compared with the prior art, the method provided by the present invention has the following beneficial effects:
[0015] (1) The method and process are simple, efficient and do not require special equipment;
[0016] (2) Low raw material costs are conducive to large-scale production;
[0017] (3) The preparation process is carried out in the aqueous phase without the need to add any organic solvents, which is environmentally friendly;
[0018] (4) Nano zinc oxide has a high loading capacity and uniform dispersion on the surface of cellulose fibers such as cotton and ramie. Attached Figure Description
[0019] Figure 1 The image shows a scanning electron microscope (SEM) image of the surface-loaded zinc oxide nanofibers prepared in Example 1.
[0020] Figure 2 The elemental distribution of the surface-loaded zinc oxide nanofibers prepared in Example 1 is shown in the energy dispersive X-ray spectroscopy (EDS) diagram.
[0021] Figure 3 The X-ray diffraction (XRD) pattern of the cotton fiber with surface-loaded zinc oxide nanoparticles prepared in Example 1.
[0022] Figure 4 The image shows the X-ray photoelectron spectroscopy (XPS) spectrum of the cotton fiber with surface-loaded zinc oxide nanoparticles prepared in Example 1. Detailed Implementation
[0023] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims. Example
[0024] (1) Sodium zincate solution was prepared by completely dissolving 1.0 g of zinc hydroxide in 100 mL of sodium hydroxide solution, and used as a precursor for nano zinc oxide;
[0025] (2) The cotton fibers were alkalized in a 30% sodium hydroxide solution for 2 hours, and then dehydrated and dried to obtain alkaline cotton fibers;
[0026] (3) The alkaline cotton fibers obtained in step 2 were impregnated with 30% 3-chloro-2-hydroxypropyltrimethylammonium chloride solution, reacted at 80°C for 20 min, washed with water and dried to obtain cationic cotton fibers;
[0027] (4) The cationic cotton fibers were impregnated in the sodium zincate solution obtained in step 1, and then squeezed dry after 2 hours, with a residual rate of 70%;
[0028] (5) The cotton fibers treated above were immersed in 5% zinc sulfate solution for 20 min, then steamed at 120°C for 20 min, washed with water and dried to prepare cotton fibers with nano zinc oxide loaded on the surface. Example
[0029] (1) Sodium zincate solution was prepared by completely dissolving 0.5g of zinc hydroxide in 100mL of sodium hydroxide solution, and used as a precursor for nano zinc oxide;
[0030] (2) The ramie fibers were alkalized in a 30% sodium hydroxide solution for 2 hours, and then dehydrated and dried to obtain alkaline ramie fibers;
[0031] (3) The alkaline ramie fibers obtained in step 2 were impregnated with a 10% solution of 3-chloro-2-hydroxypropyltrimethylammonium chloride, reacted at 80°C for 20 min, washed with water and dried to obtain cationic ramie fibers;
[0032] (4) The cationic ramie fibers were impregnated in the sodium zincate solution obtained in step 1, and then rolled dry after 2 hours, with a roll-off rate of 120%.
[0033] (5) The ramie fibers treated above were immersed in 2% zinc sulfate solution for 20 min, taken out and steamed at 120°C for 20 min, washed with water and dried to prepare ramie fibers with nano zinc oxide loaded on the surface.
Claims
1. A method for preparing nano-zinc oxide loaded on the surface of cellulose fibers, characterized in that, Includes the following steps: Step 1: Prepare sodium zincate (Na2ZnO2) solution as a precursor for nano-zinc oxide; Step 2: Alkalinize the cellulose fibers in a 30% sodium hydroxide solution for 2 hours, then dehydrate and dry to obtain alkaline cellulose fibers; Step 3: Impregnate the basic cellulose fibers obtained in Step 2 with a solution of 3-chloro-2-hydroxypropyltrimethylammonium chloride, react at 80°C for 20 min, wash with water and dry to obtain cationic cellulose fibers; Step 4: Immerse the cationic cellulose fibers in the sodium zincate solution obtained in Step 1, and roll them dry after 2 hours, with a residual rate of 70% to 120%. Step 5: Immerse the above-treated cellulose fibers in zinc sulfate solution for 20 min, remove them and steam at 120℃ for 20 min, wash with water and dry to prepare cellulose fibers with nano zinc oxide loaded on the surface. The cellulose fiber is cotton or ramie.
2. The method for preparing nano-zinc oxide loaded on the surface of cellulose fibers as described in claim 1, characterized in that: In step 1, the sodium zincate solution is prepared by completely dissolving 0.5g to 1.0g of zinc hydroxide in 100mL of sodium hydroxide solution.
3. The method for preparing nano-zinc oxide loaded on the surface of cellulose fibers as described in claim 1, characterized in that: In step 3, the concentration of the 3-chloro-2-hydroxypropyltrimethylammonium chloride solution is 10% to 30%.
4. The method for preparing nano-zinc oxide loaded on the surface of cellulose fibers as described in claim 1, characterized in that: In step 5, the concentration of the zinc sulfate solution is 2% to 5%.
Citation Information
Patent Citations
Nano-zinc oxide-based multifunctional cellulosic fiber
CN107460724A
Preparation method of nanometer zinc oxide in-situ modified antibacterial fibers
CN109162086A