CN113275586B - Method for preparing nano silver with different particle sizes by using surfactant - Google Patents
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Abstract
A method for preparing nano silver with different particle sizes by utilizing a surfactant is characterized in that the preparation of the nano silver comprises the following three steps: (1) Slowly dripping the surfactant solution into a silver nitrate solution with a certain concentration within 30-60min to prepare a solution a; (2) Dissolving sufficient reducing agent and surfactant in water to obtain solution b, slowly dripping the solution b into the solution a within 60-150min to obtain solution c, and (3) cooling the solution c to room temperature, and adjusting the pH value of the solution to 3.0-9.5 by using a pH regulator to complete the preparation of the nano silver; stirring is needed when dripping, and the temperature is 20-50 ℃. The method can realize the control of the particle size in the preparation process of the nano silver according to the type and the dosage of the surfactant, the particle size of the prepared nano silver is 20.6-129.5nm, and the prepared nano silver has good compatibility with anion, cation and nonionic materials. The method has the advantages of simple preparation process operation, mild reaction conditions, wide raw material sources and strong practicability.
Description
Technical Field
The invention belongs to the technical field of nano-silver antibacterial agent preparation, and particularly relates to a method for obtaining nano-silver with different particle sizes by using nonionic surfactants with different types and dosages in the nano-silver preparation process.
Background
The nano particles are endowed with a plurality of special properties superior to the traditional antibacterial materials due to the unique small size effect, quantum size effect, surface effect and macroscopic quantum tunneling effect. Wherein the antibacterial property of the nano-silver is far higher than that of other metal nano-particles, and the common dosage is 10 -6 (24h) Or less than or equal to 0.5 mu g/mL, and has strong effects on 12 gram-negative bacteria, 8 gram-positive bacteria and 6 moldsThe killing effect is the most widely accepted nano antibacterial agent. The nano silver particles can enter pathogens and are rapidly combined with sulfydryl in enzyme protein in a bacterial body, and some enzymes taking the sulfydryl as an essential group lose activity, so that the pathogens cannot metabolize to die. According to the antibacterial mechanism of the nano silver, the particle size of the nano silver directly influences the antibacterial performance of the nano silver.
The preparation method of nano silver is divided into two main categories of chemical method and physical method. The chemical method is mainly to reduce silver ions in the solution into silver simple substance through a certain chemical reaction, while the physical method is mainly to obtain nano silver particles through means of mechanical grinding, radiation and the like. Currently, there are some published technical documents about methods for preparing nano silver with different particle sizes, such as: silver nitrate reacts with a precipitator to form uniform silver-containing precursor precipitate, and then a reducing agent is added to reduce the silver-containing precursor precipitate under the condition of adding silver seed crystals to obtain simple substance silver (a preparation method of nano silver powder with accurately controllable particle size, CN 201110336268.9) with good powder dispersibility, different particle sizes and uniform distribution; dissolving silver nitrate and a surfactant in ethylene glycol, reacting with a sodium chloride aqueous solution under microwave irradiation, and controlling the diameter of the silver nanoparticles to be between 100 and 250nm by controlling reaction conditions (a preparation method of the silver nanoparticles with controllable particle size, CN 201410508324.6); the silver nanoparticles with different particle sizes can be obtained by injecting the metal silver particles into the substrate under the vacuum condition and only selecting a proper oblique incidence deposition angle, and the particle sizes can be accurately controlled (a preparation method of the silver nanosphere with continuously adjustable particle size, CN 201510799828.2). However, special equipment and solvents are often used in the methods, the operation conditions are harsh and difficult, and the prepared nano silver particles have overlarge particle size and poor antibacterial performance.
Therefore, the method which is simple to operate, does not need special reaction equipment, utilizes conventional chemical reagents and chemical reaction equipment, and can prepare the nano silver with different particle sizes under conventional conditions is developed, so that the nano silver with better antibacterial effect can be prepared, and the nano silver with different particle sizes can be prepared and purposefully applied to other fields.
Disclosure of Invention
The inventor deeply researches the mechanism of nano-silver preparation and colloid stabilization on the basis of the technical data disclosed in the fields of the disclosed nano-silver preparation method, colloid chemistry and the like, and provides a method for preparing nano-silver with different particle sizes by changing the type and the dosage of a surfactant based on a template method.
The template method can control the size and the shape of the silver nanoparticles by regulating and controlling the directional growth of the silver nanoparticles, and the method has simple operation and mild reaction conditions. Cationic surfactants and anionic surfactants are adopted as templates for preparing nano silver particles in the prior template method, and the anionic surfactants and the cationic surfactants have charges, so that the sol is easily influenced by acid, alkali and salt in solution and has limited use conditions; the problems can be well solved by adopting the nonionic surfactant as a template, the nonionic surfactant is not ionized in an aqueous solution, is not influenced by the existence of electrolytes such as acid, alkali, salt and the like, and has good compatibility with other types of surfactants. Although the nano silver can be prepared by using the surfactant as a template, it is critical how to control the particle size of the nano silver by the surfactant.
In the process of reducing silver ions into silver simple substance, if the generated silver simple substance cannot be dispersed and form a relatively stable system, silver precipitate is formed. When the concentration of the surfactant in the aqueous solution is greater than the Critical Micelle Concentration (CMC), micelles are formed, the hydrophilic end of the surfactant faces outwards, and the hydrophobic end is wrapped in. In the presence of micelles, silver elementary substances generated by reduction are wrapped to form relatively stable colloidal solution. Due to the difference of the structures of the hydrophilic end and the hydrophobic end of the surfactant, the diameter of the formed micelle, the diameter of the hydrophobic core and the hydrophilicity of the periphery of the micelle are also different.
When the content of the hydrophobic groups in the surfactant is higher, namely the hydrophilic-lipophilic balance (HLB) is smaller, the periphery of the formed micelle has poorer hydrophilicity, and the diameter of the hydrophobic core is larger; when the content of hydrophilic groups in the surfactant is higher, namely HLB is higher, the formed micelle has good periphery hydrophilicity and the diameter of a hydrophobic core is smaller. When the hydrophobic core of the micelle is large in diameter and the hydrophilicity of the micelle is poor, the particle size of the prepared nano silver is larger, but the stability of the colloidal solution is lower; when the micelle is better in hydrophilicity, the nano silver particle size is smaller although the colloidal solution is better in stability. In addition, for the same surfactant, when the concentration of the surfactant is close to CMC, the formed micelle has larger particle size and less hydrophilic groups at the periphery, and when the concentration of the surfactant is obviously higher than CMC, the micelle has better hydrophilicity and smaller particle size. Therefore, the HLB value of the surfactant can be changed, and the concentration of the surfactant in the solution can be controlled, so that the nano silver with different particle sizes can be prepared.
On the basis of the research, the inventor proposes a method for preparing nano silver with different particle sizes by using a surfactant, and a method for preparing nano silver with different particle sizes by using the surfactant, and is characterized in that the preparation of the nano silver comprises the following three steps: (1) Preparing a silver nitrate solution with a certain concentration, slowly dripping a surfactant solution into the silver nitrate solution within 30-60min to prepare a solution a, and stirring the solution a when dripping the solution a at the temperature of 20-50 ℃; (2) Dissolving sufficient reducing agent and surfactant in water to obtain solution b, slowly dripping the solution b into the solution a within 60-150min to obtain solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a, and stirring is required during dripping at the temperature of 20-50 ℃; (3) And cooling the solution c to room temperature, and adjusting the pH value of the solution to 3.0-9.5 by using a pH regulator to finish the preparation of the nano silver.
Wherein the concentration of the silver nitrate solution is 0.1-2g/L. The surfactant is any one of nonionic surfactants, and the surfactant needs to meet the requirements that the Critical Micelle Concentration (CMC) is 0.016-0.593mmol/L and the hydrophilic-lipophilic balance (HLB) is 7.9-14.2. The reducing agent is any one of sodium borohydride, ascorbic acid, sodium citrate, tannic acid and glucose. The pH regulator is any one of 0.01mol/L hydrochloric acid or 0.01mol/L sodium hydroxide. The stirring speed during the reaction is 200-900rpm.
The concentration of silver nitrate is 0.1-2g/L, the concentration is less than 0.1g/L, the concentration of the prepared nano silver is too thin, the using amount is large when the nano silver is used, the concentration is more than 2g/L, and the surfactant can not completely load the generated silver simple substance to form stable nano silver colloidal solution. The reaction temperature is 20-50 ℃, the reaction is too slow and the time consumption is long when the reaction temperature is lower than 20 ℃, the production of silver simple substance is too fast when the reaction temperature is higher than 50 ℃, the stability of the nonionic surfactant micelle is reduced, and a stable nano silver colloidal solution cannot be formed. The stirring speed is 200-900rpm, the stirring speed is too slow to fully wrap the surfactant micelle with the nano silver, and the stirring speed is too fast, so that the stability of the nano silver colloidal solution is damaged. After the reaction is finished, the pH value is adjusted to 3.0-9.5, which is beneficial to improving the stability of the nano silver colloid. In the process of preparing the nano-silver, the dripping time of the first step reaction is 30-60min, and the dripping time of the second step reaction is 60-150min, wherein the adding reaction speed is controlled according to the total volume of the prepared nano-silver, so that the surfactant micelle can completely wrap the nano-silver.
The method for preparing the nano silver can realize the control of the particle size in the preparation process of the nano silver according to the type and the dosage of the surfactant, and can prepare the nano silver with different particle sizes according to the final application. In addition, the method provided by the invention also has the following advantages:
1. the used reaction equipment is a sandwich reaction kettle commonly used in the chemical field, and the used materials are conventional chemical materials, so that the source is wide, the cost is low, and the large-scale popularization and use are facilitated;
2. the reaction condition is mild in the process of preparing the nano-silver, and the practicability is strong;
3. because the nonionic surfactant is used as the template, the obtained nano silver has good compatibility with anion, cation and nonionic materials, and the application field is greatly widened.
Detailed Description
The following examples are given to illustrate the invention in more detail, and it should be noted that the following examples are not to be construed as limiting the scope of the invention, and that the invention is not limited thereto since modifications and variations which are insubstantial to those skilled in the art can be made in the light of the above disclosure.
Example 1
Preparing a silver nitrate solution with the concentration of 0.1g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 30min to prepare a solution a; dissolving sufficient tannic acid and surfactant in water to obtain solution b, wherein the concentration of the surfactant in the solution b is the same as that of the solution a, and slowly dripping the solution b into the solution a within 60min to obtain solution c; and cooling the solution c to room temperature, and adjusting the pH value to 5.0 by using 0.01mol/L hydrochloric acid to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 20 ℃, the concentration of the surfactant in the solution a and the solution b is 0.7mmol/L, the stirring speed is 300rpm, and the surfactant is a nonionic surfactant with CMC of 0.593mmol/L, HLB of 7.9.
Example 2
Preparing a silver nitrate solution with the concentration of 2g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 60min to prepare a solution a; dissolving sufficient ascorbic acid and surfactant in water to obtain solution b, wherein the concentration of the surfactant in the solution b is the same as that of the solution a, and slowly dripping the solution b into the solution a within 150min to obtain solution c; and cooling the solution c to room temperature, and adjusting the pH value to 3.0 by using 0.01mol/L hydrochloric acid to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 50 ℃, the concentration of the surfactant in the solution a and the solution b is 1.0mmol/L, the stirring speed is 500rpm, and the surfactant is a nonionic surfactant with CMC of 0.593mmol/L, HLB of 7.9.
Example 3
Preparing a silver nitrate solution with the concentration of 0.15g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 60min to prepare a solution a; dissolving sufficient sodium borohydride and a surfactant in water to obtain a solution b, slowly dripping the solution b into the solution a within 90min, wherein the concentration of the surfactant in the solution b is the same as that of the solution a, and thus obtaining a solution c; and cooling the solution c to room temperature, and adjusting the pH value to 6.0 by using 0.01mol/L hydrochloric acid to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 40 ℃, the concentration of the surfactant in the solution a and the solution b is 1.3mmol/L, the stirring speed is 600rpm, and the surfactant is a nonionic surfactant with CMC of 0.593mmol/L, HLB of 7.9.
Example 4
Preparing a silver nitrate solution with the concentration of 0.8g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 40min to prepare a solution a; dissolving sufficient sodium citrate and surfactant in water to obtain solution b, slowly dripping the solution b into the solution a within 120min to obtain solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a; and cooling the solution c to room temperature, and adjusting the pH value to 6.0 by using 0.01mol/L hydrochloric acid to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 30 ℃, the concentration of the surfactant in the solution a and the solution b is 1.6mmol/L, the stirring speed is 900rpm, and the surfactant is a nonionic surfactant with CMC of 0.593mmol/L, HLB of 7.9.
Example 5
Preparing a silver nitrate solution with the concentration of 1.2g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 45min to prepare a solution a; dissolving enough glucose and surfactant in water to obtain solution b, slowly dropping the solution b into the solution a within 75min to obtain solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a; and cooling the solution c to room temperature, and adjusting the pH value to 5.5 by using 0.01mol/L hydrochloric acid to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 25 ℃, the concentration of the surfactant in the solution a and the solution b is 0.2mmol/L, the stirring speed is 500rpm, and the surfactant is a nonionic surfactant with CMC of 0.127mmol/L, HLB of 10.6.
Example 6
Preparing a silver nitrate solution with the concentration of 1.8g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 50min to prepare a solution a; dissolving sufficient sodium borohydride and a surfactant in water to obtain a solution b, slowly dropping the solution b into the solution a within 90min to obtain a solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a; and cooling the solution c to room temperature, and adjusting the pH value to 9.0 by using 0.01mol/L sodium hydroxide to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 45 ℃, the concentration of the surfactant in the solution a and the solution b is 0.225mmol/L, the stirring speed is 700rpm, and the surfactant is a nonionic surfactant with CMC of 0.127mmol/L, HLB of 10.6.
Example 7
Preparing a silver nitrate solution with the concentration of 0.9g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 35min to prepare a solution a; dissolving sufficient ascorbic acid and surfactant in water to obtain solution b, wherein the concentration of the surfactant in the solution b is the same as that of the solution a, and slowly dropping the solution b into the solution a within 100min to obtain solution c; and cooling the solution c to room temperature, and adjusting the pH value to 9.5 by using 0.01mol/L sodium hydroxide to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 30 ℃, the concentration of the surfactant in the solution a and the solution b is 0.25mmol/L, the stirring speed is 800rpm, and the surfactant is a nonionic surfactant with CMC of 0.127mmol/L, HLB of 10.6.
Example 8
Preparing a silver nitrate solution with the concentration of 2g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 60min to prepare a solution a; dissolving sufficient sodium citrate and surfactant in water to obtain solution b, slowly dripping the solution b into the solution a within 150min to obtain solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a; and cooling the solution c to room temperature, and adjusting the pH value to 8.0 by using 0.01mol/L sodium hydroxide to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 30 ℃, the concentration of the surfactant in the solution a and the solution b is 0.29mmol/L, the stirring speed is 600rpm, and the surfactant is a nonionic surfactant with CMC of 0.127mmol/L, HLB of 10.6.
Example 9
Preparing a silver nitrate solution with the concentration of 0.25g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 40min to prepare a solution a; dissolving sufficient tannic acid and surfactant in water to obtain solution b, wherein the concentration of the surfactant in the solution b is the same as that of the solution a, and slowly dripping the solution b into the solution a within 135min to obtain solution c; and cooling the solution c to room temperature, and adjusting the pH value to 7.5 by using 0.01mol/L sodium hydroxide to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 40 ℃, the concentration of the surfactant in the solution a and the solution b is 0.06mmol/L stirring speed 650rpm, and the surfactant is a nonionic surfactant with CMC of 0.051mmol/L, HLB of 12.2.
Example 10
Preparing a silver nitrate solution with the concentration of 0.5g/L, and slowly dripping the surfactant solution into the silver nitrate solution within 40min to prepare a solution a; dissolving sufficient tannic acid and surfactant in water to obtain solution b, wherein the concentration of the surfactant in the solution b is the same as that of the solution a, and slowly dripping the solution b into the solution a within 140min to obtain solution c; and cooling the solution c to room temperature, and adjusting the pH value to 4.5 by using 0.01mol/L hydrochloric acid to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 40 ℃, the concentration of the surfactant in the solution a and the solution b is 0.075mmol/L, the stirring speed is 850rpm, and the surfactant is a nonionic surfactant with CMC of 0.051mmol/L, HLB of 12.2.
Example 11
Preparing a silver nitrate solution with the concentration of 0.3g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 30min to prepare a solution a; dissolving sufficient glucose and a surfactant in water to obtain a solution b, slowly dripping the solution b into the solution a within 75min to obtain a solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a; and cooling the solution c to room temperature, and adjusting the pH value to 6.0 by using 0.01mol/L hydrochloric acid to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 45 ℃, the concentration of the surfactant in the solution a and the solution b is 0.09mmol/L, the stirring speed is 400rpm, and the surfactant is a nonionic surfactant with CMC of 0.051mmol/L, HLB of 12.2.
Example 12
Preparing a silver nitrate solution with the concentration of 0.4g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 40min to prepare a solution a; dissolving enough glucose and surfactant in water to obtain solution b, slowly dropping the solution b into the solution a within 80min to obtain solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a; and cooling the solution c to room temperature, and adjusting the pH value to 5.0 by using 0.01mol/L hydrochloric acid to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 30 ℃, the concentration of the surfactant in the solution a and the solution b is 0.105mmol/L, the stirring speed is 300rpm, and the surfactant is a nonionic surfactant with CMC of 0.051mmol/L, HLB of 12.2.
Example 13
Preparing a silver nitrate solution with the concentration of 0.6g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 60min to prepare a solution a; dissolving sufficient sodium citrate and surfactant in water to obtain solution b, slowly dripping the solution b into the solution a within 90min to obtain solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a; and cooling the solution c to room temperature, and adjusting the pH value to 3.0 by using 0.01mol/L hydrochloric acid to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 45 ℃, the concentration of the surfactant in the solution a and the solution b is 0.03mmol/L, the stirring speed is 300rpm, and the surfactant is a nonionic surfactant with CMC of 0.020mmol/L, HLB of 13.3.
Example 14
Preparing a silver nitrate solution with the concentration of 0.22g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 60min to prepare a solution a; dissolving sufficient sodium borohydride and a surfactant in water to obtain a solution b, slowly dropping the solution b into the solution a within 90min to obtain a solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a; and cooling the solution c to room temperature, and adjusting the pH value to 6.0 by using 0.01mol/L hydrochloric acid to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 40 ℃, the concentration of the surfactant in the solution a and the solution b is 0.06mmol/L, the stirring speed is 450rpm, and the surfactant is a nonionic surfactant with CMC of 0.020mmol/L, HLB of 13.3.
Example 15
Preparing a silver nitrate solution with the concentration of 0.45g/L, and slowly dripping the surfactant solution into the silver nitrate solution within 60min to prepare a solution a; dissolving sufficient sodium borohydride and a surfactant in water to obtain a solution b, slowly dripping the solution b into the solution a within 60min, wherein the concentration of the surfactant in the solution b is the same as that of the solution a, and thus obtaining a solution c; and cooling the solution c to room temperature, and adjusting the pH value to 8.5 by using 0.01mol/L sodium hydroxide to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 25 ℃, the concentration of the surfactant in the solution a and the solution b is 0.09mmol/L, the stirring speed is 900rpm, and the surfactant is a nonionic surfactant with CMC of 0.020mmol/L, HLB of 13.3.
Example 16
Preparing a silver nitrate solution with the concentration of 0.6g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 40min to prepare a solution a; dissolving sufficient sodium borohydride and a surfactant in water to obtain a solution b, slowly dropping the solution b into the solution a within 120min to obtain a solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a; and cooling the solution c to room temperature, and adjusting the pH value to 9.0 by using 0.01mol/L sodium hydroxide to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 20 ℃, the concentration of the surfactant in the solution a and the solution b is 0.12mmol/L, the stirring speed is 800rpm, and the surfactant is a nonionic surfactant with CMC of 0.020mmol/L, HLB of 13.3.
Example 17
Preparing a silver nitrate solution with the concentration of 1.8g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 60min to prepare a solution a; dissolving sufficient sodium borohydride and a surfactant in water to obtain a solution b, slowly dropping the solution b into the solution a within 150min to obtain a solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a; and cooling the solution c to room temperature, and adjusting the pH value to 9.5 by using 0.01mol/L sodium hydroxide to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 35 ℃, the concentration of the surfactant in the solution a and the solution b is 0.03mmol/L, the stirring speed is 900rpm, and the surfactant is a nonionic surfactant with CMC of 0.016mmol/L, HLB of 14.2.
Example 18
Preparing a silver nitrate solution with the concentration of 1.5g/L, and slowly dripping the surfactant solution into the silver nitrate solution within 45min to prepare a solution a; dissolving enough glucose and surfactant in water to obtain solution b, slowly dropping the solution b into the solution a within 150min to obtain solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a; and cooling the solution c to room temperature, and adjusting the pH value to 7.5 by using 0.01mol/L sodium hydroxide to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 30 ℃, the concentration of the surfactant in the solution a and the solution b is 0.045mmol/L stirring speed 600rpm, and the surfactant is a nonionic surfactant with CMC of 0.016mmol/L, HLB of 14.2.
Example 19
Preparing a silver nitrate solution with the concentration of 1.0g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 50min to prepare a solution a; dissolving sufficient ascorbic acid and surfactant in water to obtain solution b, wherein the concentration of the surfactant in the solution b is the same as that of the solution a, and slowly dropping the solution b into the solution a within 130min to obtain solution c; and cooling the solution c to room temperature, and adjusting the pH value to 4.5 by using 0.01mol/L hydrochloric acid to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 40 ℃, the concentration of the surfactant in the solution a and the solution b is 0.09mmol/L, the stirring speed is 700rpm, and the surfactant is a nonionic surfactant with CMC of 0.016mmol/L, HLB of 14.2.
Example 20
Preparing a silver nitrate solution with the concentration of 0.6g/L, and slowly dripping a surfactant solution into the silver nitrate solution within 35min to prepare a solution a; dissolving sufficient sodium citrate and surfactant in water to obtain solution b, slowly dripping the solution b into the solution a within 90min to obtain solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a; and cooling the solution c to room temperature, and adjusting the pH value to 3.0 by using 0.01mol/L hydrochloric acid to complete the preparation of the nano silver. Wherein the reaction temperature in the preparation process of the solution a and the solution c is 50 ℃, the concentration of the surfactant in the solution a and the solution b is 0.018mmol/L, the stirring speed is 600rpm, and the surfactant is a nonionic surfactant with CMC of 0.016mmol/L, HLB of 14.2.
The Nano silver colloidal solution obtained in the above example was measured for particle size using a Nano ZS laser particle size analyzer (Malvern instruments, uk), the test was performed at 25 ℃, the sample was kept constant for 3min in the apparatus before the test, and the average of the results of the three tests was taken as a report, and the results are shown in table 1.
TABLE 1
Claims (3)
1. A method for preparing nano silver with different particle diameters by utilizing a surfactant is characterized in that the preparation of the nano silver comprises the following three steps: (1) Preparing a silver nitrate solution with a certain concentration of 0.1-2g/L, slowly dripping a surfactant solution into the silver nitrate solution within 30-60min to prepare a solution a, and stirring the solution a when dripping the solution a at a stirring speed of 200-900rpm and a temperature of 20-50 ℃; (2) Dissolving sufficient reducing agent and surfactant in water to obtain solution b, slowly dripping the solution b into the solution a within 60-150min to obtain solution c, wherein the concentration of the surfactant in the solution b is the same as that of the solution a, and stirring is required during dripping at the speed of 200-900rpm and the temperature of 20-50 ℃; (3) Cooling the solution c to room temperature, and adjusting the pH value of the solution to 3.0-9.5 by using a pH regulator to finish the preparation of the nano silver; wherein the surfactant is any one of nonionic surfactants, the critical micelle concentration CMC is 0.016-0.593mmol/L, and the hydrophilic-lipophilic balance HLB is 7.9-14.2.
2. The method for preparing nano silver with different particle diameters by using the surfactant according to claim 1, wherein the reducing agent is any one of sodium borohydride, ascorbic acid, sodium citrate, tannic acid and glucose.
3. The method for preparing nano silver with different particle diameters by using the surfactant according to claim 1, wherein the pH regulator is any one of 0.01mol/L hydrochloric acid and 0.01mol/L sodium hydroxide.
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Non-Patent Citations (2)
| Title |
|---|
| 张万忠;乔学亮;陈建国.银纳米材料的可控合成研究.稀有金属材料与工程.2008,(第11期),第2059-2064页. * |
| 闫方存;滕媛;严继康;李文琳;易健宏;甘国友.分散体系对微米银粉微观形貌及粒径影响研究.稀有金属.2017,(第02期),第173-178页. * |
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