CN108609646B - Preparation method and application of nano silver chloride - Google Patents
Preparation method and application of nano silver chloride Download PDFInfo
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Abstract
The invention discloses a preparation method and application of nano silver chloride. The preparation method comprises the following steps: (1) respectively preparing 25 wt% silver nitrate glycol solutions A; a 10 wt% soluble chloride in ethylene glycol solution B; and a glycol solution C of a protective agent with the concentration of 1-3 wt%; (2) the solution A, B, C obtained in step (1) was heated to 40 ℃. Dropwise adding the solution A and the solution B into the solution C at the speed of 0.5-100 mL/min; stirring the solution C at the speed of 500 r/min while dropwise adding; (3) after the dropwise addition is finished, keeping the temperature at 30 ℃ and continuously reacting for 15-90 min to obtain the nano silver chloride colloid. The nano silver chloride prepared by the invention has small particle size and uniform appearance and particle size, and can be used for preparing photochromic glass, photocatalysts, medicines, antibacterial materials, composite materials, electrode materials and photocatalysts for degrading organic matters.
Description
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a preparation method and application of nano silver chloride applied to a reference electrode.
Background
The nano material has the characteristics of quantum size effect, small size effect, surface effect, macroscopic quantum tunneling effect and the like, presents unique physical and chemical properties, and particularly has huge potential application prospects in the aspects of light, sound, electricity, magnetism, heat, catalysis, medicine, environmental protection, chemical activity and the like.
Silver chloride has very important application in the fields of electrochemistry, light-sensitive films, sterilization, disinfection and the like. The nano silver chloride has the remarkable characteristics of a nano structure and photochromism, and is widely applied to the fields of photochromism glass, photocatalysts, medicines, antibacterias, composite materials, electrode materials, photocatalysts for degrading organic matters and the like. The preparation method of the nano silver chloride is various, and mainly comprises a hydrothermal method, a homogeneous precipitation method, a sol-gel method, a template method, a microemulsion method, a microwave-assisted method and the like. The average grain diameter of the nano silver chloride prepared by the technical methods is about 50-500nm, the grain diameter distribution is uneven, and the nano particles are easy to agglomerate and the like. Wherein, various technologies have complex operation and harsh conditions, which are not beneficial to industrial application.
Chinese patent CN100427402C discloses a method for preparing temperature-resistant nano silver chloride sol, which comprises placing a solution system of soluble chloride, silver nitrate and a dispersant in an ultrasonic field, and shearing by using mechanical and hydraulic forces generated by a high-shear dispersion emulsifying machine to obtain nano sol. The average particle size of the silver chloride particles is 20nm-70 nm. Chinese patent CN101774630B discloses a method for preparing water-soluble silver halide nanoparticles, which uses Hyperbranched Polyglycidyl (HPG) as a stabilizer, and the obtained silver halide nanoparticles have the particle size of 2-20nm and good crystallization. But the HPG is a dendritic polymer with a three-dimensional spherical molecular structure, a large number of cavities exist inside the HPG, and the performances of the prepared HPG-AgX colloid on various aspects of a microscopic level are obviously changed compared with the silver halide nanoparticles prepared by a traditional precipitation method. Particularly, the ionization capacity of the nano silver halide ions is shown, and the reduction capacity of HPG-AgX particles is reduced due to the special molecular structure of the stabilizer in the preparation process, so that when the HPG-AgX particles are applied to a reference electrode, the electrode potential is unstable.
The conductive material of the conductive ink used at present is generally gold, silver or carbon. The nano silver conductive ink has the disadvantages that various protective agents are required to be added, but the viscosity of the ink is increased due to the protective agents, and the ink is difficult to completely remove in the sintering process, so that the conductivity of the ink is influenced; in addition, the nano silver can flocculate, precipitate and block the nozzle after being placed for a long time, and the concentration of the nano silver ink can be changed.
Therefore, in order to overcome the above problems in the prior art, a new method for preparing nano silver chloride is needed, which improves the nano colloidal properties, makes the nano silver chloride have smaller particle size, more uniform particle size distribution and enhanced colloidal stability, and is applied to silver conductive ink to form conductive ink with electrodes.
Disclosure of Invention
The invention aims to provide a preparation method and application of nano silver chloride.
The preparation method provided by the invention comprises the following steps:
(1) respectively preparing 25 wt% silver nitrate glycol solutions A; a 10 wt% soluble chloride in ethylene glycol solution B; and a glycol solution C of a protective agent with the concentration of 1-3 wt%;
(2) the solution A, B, C obtained in step (1) was heated to 40 ℃. Dropwise adding the solution A and the solution B into the solution C at the speed of 0.5-100 mL/min; stirring the solution C at the speed of 500 r/min while dropwise adding;
(3) after the dropwise addition is finished, keeping the temperature at 30 ℃ and continuously reacting for 15-90 min to obtain the nano silver chloride colloid.
Further, the whole procedure was carried out in a dark environment.
The mass ratio of the silver nitrate to the soluble chloride is 1.5-3: 1.
The mass ratio of the silver nitrate to the protective agent is 10-20: 1.
The soluble chloride is one or more of sodium chloride, potassium chloride, iron dichloride, ferric trichloride, calcium chloride, magnesium chloride, zinc chloride and copper chloride. The soluble chloride is preferably a composition of sodium chloride and potassium chloride, and the mass ratio of the soluble chloride to the potassium chloride is specifically 1.3: 1.
The protective agent is one or more of polyvinylpyrrolidone (PVP), polyvinyl butyral (PVB) and hydroxypropyl cellulose (PHC). The protective agent is preferably a composition of polyvinylpyrrolidone (PVP) and polyvinyl butyral (PVB) in a mass ratio of 2: 1.
The invention also provides the nano silver chloride prepared by the preparation method.
The invention also provides application of the nano silver chloride.
The application fields of the nano silver chloride comprise photochromic glass, photocatalyst, medicine, antibiosis, composite material, electrode material and photocatalyst for degrading organic matters.
The application of the nano silver chloride is that silver conductive ink is added to prepare conductive ink containing an electrode.
The nano silver chloride has a special structure and unique electrochemical performance, is added into conductive ink containing silver particles, and forms a silver-silver chloride reference electrode by taking a solvent in the conductive ink as an electrolyte solution, silver as an anode and silver chloride as a cathode.
The technical scheme of the invention has the following beneficial effects:
(1) the preparation method has simple process, the selected raw materials have no toxicity and pollution to human bodies and environment, the production cost is low, the energy consumption is low, and the preparation method is suitable for mass preparation;
(2) compared with the traditional wet preparation method, the preparation method provided by the invention has the advantages that the nano silver chloride prepared in the glycol system has smaller particle size, is more uniformly distributed in the dispersion liquid, has the average particle size of 5-15 nm, and has the characteristics of small particle size, high yield and uniform and stable product;
(3) the nano silver chloride prepared by the invention can be widely applied to the fields of photochromic glass, photocatalyst, medicine, antibiosis, composite material, electrode material, photocatalyst for degrading organic matters and the like;
(4) the nano silver chloride prepared by the invention is added into the silver conductive ink, the stability of a dispersion system is enhanced, and the electrode potential stabilization time of the conductive ink is prolonged.
Detailed Description
The present invention will be described in further detail with reference to the following data in conjunction with specific examples. The following examples are intended to illustrate the invention and are not intended to limit the scope of the invention in any way.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials, instruments and the like used in the following examples are commercially available unless otherwise specified.
Preparation of nano silver chloride by different preparation methods
Example 1
Preparing 25 wt% silver nitrate ethylene glycol solution A: 20g of ethylene glycol solution B with a concentration of 5.6% by weight of sodium chloride, 4.4% by weight of potassium chloride: 23g of a 1.3% strength by weight polyvinyl pyrrolidone, 0.67% strength by weight polyvinyl butyral in ethylene glycol solution C: 15 g. And (3) respectively heating the solution A, B, C to 40 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 15mL/min, stirring at the speed of 500 r/min, and after the addition is finished, keeping the mixed solution at 30 ℃ and stirring for 60min to obtain the nano silver chloride sol.
Example 2
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B with a concentration of 5.6% by weight of sodium chloride, 4.4% by weight of potassium chloride: 50g, a 2% strength by weight polyvinyl pyrrolidone, a 1% strength by weight polyvinyl butyral in ethylene glycol solution C: 25 g. And (3) respectively heating the solution A, B, C to 40 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 30 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Example 3
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B with a concentration of 5.6% by weight of sodium chloride, 4.4% by weight of potassium chloride: 25g, 2% strength by weight polyvinylpyrrolidone, 1% strength by weight polyvinyl butyral in ethylene glycol solution C: 12.5 g. And (3) respectively heating the solution A, B, C to 40 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 30 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Comparative example 1
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B with a concentration of 7.5% by weight of sodium chloride, 2.5% by weight of potassium chloride: 50g, a 2% strength by weight polyvinyl pyrrolidone, a 1% strength by weight polyvinyl butyral in ethylene glycol solution C: 25 g. And (3) respectively heating the solution A, B, C to 40 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 30 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Comparative example 2
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g, 5 wt% sodium chloride, 5 wt% ferrous chloride in ethylene glycol solution B: 50g, a 2% strength by weight polyvinyl pyrrolidone, a 1% strength by weight polyvinyl butyral in ethylene glycol solution C: 25 g. And (3) respectively heating the solution A, B, C to 40 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 30 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Comparative example 3
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B of sodium chloride with a concentration of 5.5% by weight, copper chloride with a concentration of 4.5% by weight: 50g, a 2% strength by weight polyvinyl pyrrolidone, a 1% strength by weight polyvinyl butyral in ethylene glycol solution C: 25 g. And (3) respectively heating the solution A, B, C to 40 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 30 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Comparative example 4
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g, ethylene glycol solution B of 4.5 wt% sodium chloride, 5.5 wt% ferrous chloride: 50g, a 2% strength by weight polyvinyl pyrrolidone, a 1% strength by weight polyvinyl butyral in ethylene glycol solution C: 25 g. And (3) respectively heating the solution A, B, C to 40 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 30 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Comparative example 5
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B of 5% by weight sodium chloride, 5% by weight copper chloride: 50g, a 2% strength by weight polyvinyl pyrrolidone, a 1% strength by weight polyvinyl butyral in ethylene glycol solution C: 25 g. And (3) respectively heating the solution A, B, C to 40 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 30 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Comparative example 6
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B with a concentration of 5.6% by weight of sodium chloride, 4.4% by weight of potassium chloride: 50g of a 1.5% strength by weight polyvinyl pyrrolidone, 1.5% strength by weight polyvinyl butyral in ethylene glycol solution C: 25 g. And (3) respectively heating the solution A, B, C to 40 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 30 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Comparative example 7
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B with a concentration of 5.6% by weight of sodium chloride, 4.4% by weight of potassium chloride: 50g, 2% strength by weight polyvinylpyrrolidone, 1% strength by weight hydroxypropylcellulose in ethylene glycol solution C: 25 g. And (3) respectively heating the solution A, B, C to 40 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 30 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Comparative example 8
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B with a concentration of 5.6% by weight of sodium chloride, 4.4% by weight of potassium chloride: 50g, 1.5% by weight polyvinylpyrrolidone, 1.5% by weight hydroxypropylcellulose in ethylene glycol solution C: 25 g. And (3) respectively heating the solution A, B, C to 40 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 30 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Comparative example 9
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B with a concentration of 5.6% by weight of sodium chloride, 4.4% by weight of potassium chloride: 50g, a 2% strength by weight polyvinyl pyrrolidone, a 1% strength by weight polyvinyl butyral in ethylene glycol solution C: 25 g. The solution A, B, C was heated to 40 ℃ separately, and then solution A was added to solution C at a rate of 18mL/min, and solution B was added to the mixed solution at a rate of 18mL/min with stirring at 500 rpm. After the addition was completed, the mixed solution was kept at 30 ℃ and stirred for 75min to obtain a nano silver chloride sol.
Comparative example 10
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B with a concentration of 5.6% by weight of sodium chloride, 4.4% by weight of potassium chloride: 50g, a 2% strength by weight polyvinyl pyrrolidone, a 1% strength by weight polyvinyl butyral in ethylene glycol solution C: 25 g. The solution A, B, C was heated to 40 ℃ separately, and then solution B was added to solution C at a rate of 18mL/min, and solution A was added to the mixed solution at a rate of 18mL/min with stirring at 500 rpm. After the addition was completed, the mixed solution was kept at 30 ℃ and stirred for 75min to obtain a nano silver chloride sol.
Comparative example 11
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B with a concentration of 5.6% by weight of sodium chloride, 4.4% by weight of potassium chloride: 50g, a 2% strength by weight polyvinyl pyrrolidone, a 1% strength by weight polyvinyl butyral in ethylene glycol solution C: 25 g. And (3) respectively heating the solution A, B, C to 30 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 30 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Comparative example 12
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B with a concentration of 5.6% by weight of sodium chloride, 4.4% by weight of potassium chloride: 50g, a 2% strength by weight polyvinyl pyrrolidone, a 1% strength by weight polyvinyl butyral in ethylene glycol solution C: 25 g. And (3) respectively heating the solution A, B, C to 40 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 40 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Comparative example 13
Preparing 25 wt% silver nitrate ethylene glycol solution A: 30g of ethylene glycol solution B with a concentration of 5.6% by weight of sodium chloride, 4.4% by weight of potassium chloride: 50g, a 2% strength by weight polyvinyl pyrrolidone, a 1% strength by weight polyvinyl butyral in ethylene glycol solution C: 25 g. And (3) respectively heating the solution A, B, C to 30 ℃, then simultaneously adding the solution A and the solution B into the solution C at the speed of 18mL/min, stirring at the speed of 500 rpm, and after the addition is finished, keeping the mixed solution at 40 ℃ and stirring for 75min to obtain the nano silver chloride sol.
Evaluation of particle size of silver chloride nanoparticles
Scanning Electron Microscope (SEM) tests are carried out on the products obtained in examples 1-3 and comparative examples 1-13, the particle size of the product is recorded, and the average particle size results are shown in tables 1 and 2:
TABLE 1 EXAMPLES 1-3 average particle diameter of Nano silver chloride particles
| Examples | 1 | 2 | 3 |
| Average particle diameter (nm) | 13 | 6 | 10 |
TABLE 2 comparative examples 1-13 average particle diameter of nano silver chloride particles
The average particle size of the nano silver chloride prepared under the preparation conditions of the embodiments 1 to 3 is less than 15nm, wherein the particle size of the nano silver chloride particles obtained in the embodiment 2 is 6 nm. The preparation conditions of the invention have obvious influence on the nano-particle size.
Evaluation of electrode potential of three-nanometer silver chloride-silver conductive ink
5g of each of the products obtained in examples 1 to 3 and comparative examples 1 to 13 was added to 50g of conductive ink, wherein the conductive ink was NT-ST60 type silk-screen silver paste produced by Zhongkongtong. The electrode potentials of the conductive inks at 25 ℃ were measured, and the results are shown in tables 3 and 4:
TABLE 3 conductive ink electrode potentials
TABLE 4 conductive ink electrode potentials
The standard electrode potential of the silver-silver chloride reference electrode was 0.2224V at 25 ℃.
As can be seen from tables 3 and 4, the potential difference between the nano silver chloride prepared under the preparation conditions of the embodiments 1 to 3 and the reference electrode prepared by adding the nano silver chloride into the conductive ink is 0.1V at most. The electrode potential of example 2 is comparable to the standard electrode potential of a silver-silver chloride reference electrode. The reference electrode prepared by adding the nano silver chloride prepared under the preparation conditions of comparative examples 1-13 into the conductive ink has a larger potential difference with the standard electrode potential of the silver-silver chloride reference electrode. The nano silver chloride prepared under the condition of the invention has larger influence on the electrode potential after the reference electrode is formed due to the shape and the uniform degree of the grain diameter.
Since the reference electrode is an electrode used as a reference for comparison in measuring various electrode potentials, the value of the electrode potential thereof is very important.
Evaluation of potential stability of electrode of four-nanometer silver chloride-silver conductive ink
5g of each of the products obtained in examples 1 to 3 and comparative examples 1 to 13 was added to 50g of conductive ink, wherein the conductive ink was NT-ST60 type silk-screen silver paste produced by Zhongkongtong. The electrode potentials of the conductive inks at different times and at 25 ℃ were measured, and the results are shown in tables 5 and 6:
TABLE 5 conductive ink electrode potentials
| Time of day | Example 1 | Example 2 | Example 3 |
| 1h | 0.3V | 0.2V | 0.3V |
| 5h | 0.3V | 0.2V | 0.3V |
| 12h | 0.3V | 0.2V | 0.3V |
| 1d | 0.3V | 0.2V | 0.3V |
| 2d | 0.3V | 0.2V | 0.3V |
| 3d | 0.3V | 0.2V | 0.3V |
| 4d | 0.3V | 0.2V | 0.3V |
| 5d | 0.3V | 0.2V | 0.2V |
| 10d | 0.3V | 0.2V | 0.1V |
| 15d | 0.3V | 0.2V | 0.05V |
| 20d | 0.1V | 0.1V | 0 |
| 30d | 0.1V | 0.1V | 0 |
TABLE 6 conductive ink electrode potentials
As can be seen from tables 5 and 6, the potential stability of the nano silver chloride prepared under the preparation conditions of examples 1 to 3 and the reference electrode prepared by adding the nano silver chloride into the conductive ink changes on day 4, wherein the stability period of example 2 reaches 15 days. Comparative examples 1 to 13 were poor in potential stability, wherein the potential of comparative example 5 was changed on day 5.
The shape and the grain diameter uniformity of the nano silver chloride prepared under the condition of the invention have great influence on the stability of the electrode potential after the reference electrode is formed.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (2)
1. A preparation method of nano silver chloride is characterized by comprising the following steps: (1) respectively preparing 25 wt% silver nitrate glycol solutions A; a 10 wt% soluble chloride in ethylene glycol solution B; and a glycol solution C of a protective agent with the concentration of 1-3 wt%; (2) heating the solution A, B, C obtained in step (1) to 40 ℃; dropwise adding the solution A and the solution B into the solution C at the speed of 0.5-100 mL/min; stirring the solution C at the speed of 500 r/min while dropwise adding; (3) after the dropwise addition is finished, keeping the temperature at 30 ℃ and continuously reacting for 15-90 min to obtain nano silver chloride colloid;
the mass ratio of the silver nitrate to the soluble chloride is 1.5-3: 1; the mass ratio of the silver nitrate to the protective agent is 10-20: 1;
the soluble chloride is a composition of sodium chloride and potassium chloride, and the mass ratio of the soluble chloride to the potassium chloride is 1.3: 1;
the protective agent is a composition of polyvinylpyrrolidone (PVP) and polyvinyl butyral (PVB) in a mass ratio of 2: 1.
2. The method for preparing nano silver chloride according to claim 1, wherein the whole step is carried out in a dark environment.
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