A method for preparing nano silver fiber film
By impregnating PANI and PANI:PSS aqueous solutions and using the reduction characteristics of polyaniline to form a silver particle catalytic center on the nano-silver fiber film, the preparation process is simplified, the problems of cumbersome preparation and high cost of precious metals are solved, and the problems of traditional nano-silver films are improved. Preparation efficiency and reduce costs.
Patent Information
- Application Number
- CN202211510829.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-11-29
- Publication Date
- 2025-01-17
- Estimated Expiration
- 2042-11-29
AI Technical Summary
The preparation process of traditional nano silver fiber films is cumbersome and the cost of using precious metal palladium is high, resulting in low efficiency and high cost.
Hydrophilic fibers were used to immerse PANI and PANI:PSS aqueous solutions and prepare conductive high-component films through drying. The complexing ability of PSS and polyaniline to silver ions and the reduction characteristics of polyaniline were used to reduce silver silver particles on the film as Catalytic center, reduces oil removal and roughening processes, and reduces the use of precious metals.
The preparation process is simplified, the preparation efficiency of nano-silver film is improved, the cost is reduced, and conductive polymer films with excellent mechanical properties and certain reduction characteristics are obtained.
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Figure CN115976833B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of fiber film production, and in particular to a method for preparing a nano silver fiber film. Background Art
[0002] Nanosilver film has high application value in electromagnetic shielding and sterilization. At present, the preparation of nanosilver fiber network is often prepared by chemical plating. The traditional whole process includes degreasing, roughening, sensitization, activation, chemical plating and other process flows. Degreasing in the process is to remove the grease on the surface of the fabric to increase the fastness of the coating. Roughening is to form pits on the fiber surface to increase the surface area and hydrophilicity. Sensitization and activation are to use tin chloride to adsorb on the fiber first and then reduce palladium chloride to produce catalytic centers that can be chemically plated. The traditional preparation process is relatively cumbersome, and the palladium used is a precious metal with high cost. The invention utilizes hydrophilic fibers to be impregnated with PANI and PANI:PSS aqueous solutions and prepares a conductive polymer film with excellent mechanical properties and certain reduction characteristics through a drying process. The complexing ability of PSS and polyaniline with silver ions and the reduction characteristics of polyaniline are utilized, and silver particles are reduced as catalytic centers on the film through impregnation with a silver nitrate solution, and then a chemical plating process is performed. The whole process reduces the degreasing and roughening processes of traditional fibers, reduces the use of precious metals in traditional sensitization and activation processes, and increases the efficiency of preparing the nano silver film and reduces the cost. Summary of the invention
[0003] 1. Technical issues to be resolved
[0004] The whole traditional process includes degreasing, roughening, sensitization, activation, chemical plating and other process flows. Degreasing in the process is to remove grease on the surface of the fabric to increase the fastness of the coating. Roughening is to form pits on the fiber surface to increase the surface area and hydrophilicity. Sensitization and activation are to use tin chloride to be adsorbed on the fiber first and then reduce palladium chloride to produce catalytic centers that can be chemically plated. The traditional preparation process is relatively cumbersome, and the palladium used is a precious metal with a high cost. A method for preparing a nano silver fiber film is provided.
[0005] (II) Technical solution
[0006] A method for preparing a nano silver fiber film.
[0007] The following steps are involved:
[0008] In the first step, PANI powder chemically polymerized by ammonium persulfate is dispersed into a PANI:PSS water system with a mass fraction of 1.2%, and PANI is dispersed to form a water slurry with a polyaniline solid content of 0.2% and good dispersion; the slurry is sprayed onto glycerol-modified polyacrylonitrile fibers, and dried under stretching conditions to obtain a conductive high-resolution film with reducing properties;
[0009] In the second step, the film was impregnated with 1-1.5 g L -1 Silver nitrate solution for 1.5-3 hours and dried to obtain a fiber film with silver particles attached;
[0010] The third step is chemical plating. This process is a general process. The chemical plating method is similar and is divided into silver plating solution and reducing solution. Glucose or hydrazine hydrate can be used as a reducing agent.
[0011] The method of using glucose in the third step is as follows:
[0012] Silver plating liquid configuration method:
[0013] Dissolve silver nitrate in deionized water, add ammonia water until it is clear, and add ethylenediamine 20 mg L -1 Then, potassium hydroxide solution is used to adjust the pH to about 11 to prepare a silver plating solution;
[0014] Reduction solution preparation method:
[0015] Mix 20-25g / L glucose and 2 g / L potassium sodium tartrate and boil for 5-10 minutes, then add 35-40mg / L polyethylene glycol and 40ml / L ethanol;
[0016] As a preferred technical solution, the two are mixed and ultrasonically silver-plated at 40 degrees Celsius for 2 hours, and the film is taken out, washed with water, and dried to obtain a nanosilver fiber film.
[0017] As a preferred technical solution, ammonium persulfate chemically polymerized PANI powder is a commercial product.
[0018] As a preferred technical solution, the PANI:PSS water system with a mass fraction of 1.2% is a commercial product.
[0019] (III) Beneficial effects
[0020] The beneficial effects of the present invention are:
[0021] 1. The present invention utilizes hydrophilic fibers to be impregnated with PANI and PANI:PSS aqueous solutions and prepares a conductive polymer film with excellent mechanical properties and certain reduction characteristics through a drying process. The complexing ability of PSS and polyaniline with silver ions and the reduction characteristics of polyaniline are utilized to reduce silver particles on the film as catalytic centers by impregnating the film with a silver nitrate solution, and then a chemical plating process is performed. The whole process reduces the degreasing and roughening processes of traditional fibers, reduces the use of precious metals in traditional sensitization and activation processes, and increases the efficiency of preparing nano silver films and reduces the cost.
[0022] 2. The present invention utilizes electrostatically spun glycerol-modified nano hydrophilic fiber film to impregnate PANI and PANI:PSS aqueous solutions and prepares a conductive polymer film with excellent mechanical properties and certain reduction characteristics through a drying process. The complexing ability of PSS and polyaniline with silver ions and the reduction characteristics of polyaniline are utilized to reduce silver particles on the film as catalytic centers by impregnating silver nitrate solution, and then a chemical plating process is performed. The entire process reduces the degreasing and roughening processes of traditional fibers, reduces the use of precious metals in traditional sensitization and activation processes, and increases the efficiency of preparing nano silver film and reduces the cost. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0024] Figure 1 It is a scan of chemically plated silver film;
[0025] Figure 2 It is a chemically silver-plated fiber;
[0026] Figure 3 yes Figure 2 A partial enlarged view of the part. DETAILED DESCRIPTION
[0027] The preparation method of a nano silver fiber film of the present invention is further described in conjunction with the accompanying drawings. The present invention is further described in detail below in conjunction with embodiments:
[0028] As attached Figure 1-3 The method for preparing a nano silver fiber film is characterized by:
[0029] The following steps are involved:
[0030] In the first step, PANI powder chemically polymerized by ammonium persulfate is dispersed into a PANI:PSS water system with a mass fraction of 1.2%, and PANI is dispersed to form a water slurry with a polyaniline solid content of 0.2% and good dispersion; the slurry is sprayed onto glycerol-modified polyacrylonitrile fibers, and dried under stretching conditions to obtain a conductive high-resolution film with reducing properties;
[0031] It should be noted that PANI:PSS has good hydrophilicity and can be well attached to the glycerol-modified electrospun hydrophilic fiber through a spraying process, thus eliminating the oiling and coarsening process of traditional fibers. PANI has poor dispersion performance and only provides reducing ability, so its solid content is controlled within 0.2% to achieve a better dispersion effect.
[0032] In the second step, the film was impregnated with 1-1.5 g L -1 Silver nitrate solution for 1.5-3 hours and dried to obtain a fiber film with silver particles attached;
[0033] It should be noted that the silver particles can serve as catalytic centers to initiate chemical plating.
[0034] The third step is chemical plating. This process is a general process. The chemical plating method is similar and is divided into silver plating solution and reducing solution. Glucose or hydrazine hydrate can be used as a reducing agent.
[0035] The method of using glucose in the third step is as follows:
[0036] Silver plating liquid configuration method:
[0037] Dissolve silver nitrate in deionized water, add ammonia water until it is clear, and add ethylenediamine 20 mg L -1 Then, potassium hydroxide solution is used to adjust the pH to about 11 to prepare a silver plating solution;
[0038] Reduction solution preparation method:
[0039] Mix 20-25g / L glucose and 2 g / L potassium sodium tartrate and boil for 5-10 minutes, then add 35-40mg / L polyethylene glycol and 40ml / L ethanol;
[0040] Further, the two were mixed and subjected to ultrasonic silver plating at 40 degrees Celsius for 2 hours, and the film was taken out and washed with water and dried to obtain a nanosilver fiber film. Figure 2 The silver coating on the fiber of the film is relatively uniform, and the scanning magnification Figure 3 It was also confirmed that the silver particles were uniformly attached to the fibers.
[0041] It should be noted that the ammonium persulfate chemically polymerized PANI powder is a commercial product.
[0042] The PANI:PSS water system with a mass fraction of 1.2% is a commercial product.
[0043] The above embodiments are merely descriptions of preferred implementations of the present invention, and are not intended to limit the concept and scope of the present invention. Without departing from the design concept of the present invention, various modifications and improvements made to the technical solution of the present invention by ordinary personnel in the field should fall within the protection scope of the present invention. The technical contents for which protection is sought in the present invention have all been recorded in the claims.
Claims
1. A method for preparing a nano silver fiber film, characterized in that: The following steps are involved: In the first step, polyaniline powder chemically polymerized by ammonium persulfate is dispersed into a PANI:PSS water system with a mass fraction of 1.2% to form a water system slurry with a polyaniline solid content of 0.2% and good dispersion; the slurry is sprayed onto a glycerol-modified polyacrylonitrile hydrophilic fiber, and dried under a stretching condition to obtain a conductive polymer film with reducing properties; The second step is to immerse the film in a 1-1.5 g / L silver nitrate solution for 1.5-3 hours and air dry to obtain a conductive polymer film with attached nano-silver particles; The third step is chemical silver plating. This process is similar to the traditional chemical silver plating method and is divided into silver plating solution and reducing solution. Glucose or hydrazine hydrate can be used as a reducing agent.
2. The method for preparing a nano silver fiber film according to claim 1, characterized in that: The method of adopting glucose in the described third step is as follows: Silver plating liquid configuration method: Dissolve silver nitrate in deionized water, add ammonia water until it is clear, add 20 mg / L ethylenediamine, and then adjust the pH to about 11 with potassium hydroxide solution to prepare a silver plating solution; Reduction solution preparation method: Mix 20-25 g / L of glucose and 2 g / L of potassium sodium tartrate and boil for 5-10 minutes, then add 35-40 mg / L of polyethylene glycol and 40 ml / L of ethanol; The silver plating solution and the reducing solution are mixed, and the conductive polymer film with the nanosilver particles attached is immersed in the mixed solution, and the film is ultrasonically silver-plated at 40 °C for 2 hours. After the film is taken out, it is washed with water and dried to obtain a nanosilver fiber film.
3. The method for preparing a nano silver fiber film according to claim 1, characterized in that: The polyaniline powder chemically polymerized from ammonium persulfate is a commercial product.
4. The method for preparing a nano silver fiber film according to claim 1, characterized in that: The PANI:PSS water system with a mass fraction of 1.2% is a commercial product.
Citation Information
Patent Citations
Method for making conductive fabric through polyaniline-triggered chemical slivering
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CN114974932A