CN105215348A - A kind of containing Nano Silver anhydrous glycerol colloidal sol and preparation method thereof - Google Patents

Abstract

The invention discloses an anhydrous glycerol sol containing nanometer silver and a preparation method thereof. The characteristics of the sol are: the appearance is a yellow transparent liquid, and its dispersion medium is anhydrous glycerin; the dispersed phase particles are silver single particles with a particle size range of 2-70 nanometers, which can be stably dispersed in the glycerin medium; the auxiliary dispersant is polyethylene Pyrrolidone K30. The preparation method of the sol is as follows: first, mix anhydrous glycerin and polyvinylpyrrolidone K30 in a round bottom flask, heat to form a clear glycerin solution, then add solid silver nitrate to the solution, stir and dissolve with a magnetic stirrer, and heat up Continue to stir and react at a certain temperature, and obtain anhydrous glycerol sol containing nano-silver after cooling. The invention has simple process and low cost, and the obtained sol has good stability and can be stored at room temperature and air atmosphere.

Description

A kind of nano-silver anhydrous glycerol sol and preparation method thereof

technical field

The invention relates to a stable anhydrous glycerol sol containing nanometer silver and a preparation method thereof, belonging to the field of nanometer material technology and interface chemistry.

Background technique

Nano-silver and the assembly system containing nano-silver particles have excellent performance in biological activity, electricity, heat, optics, catalysis, etc., and have broad application prospects in industrial catalysis, electronics and electrical engineering, medical and health, and fine chemicals. In particular, nano-silver particles have a huge surface area and can release a large amount of active silver ions (Ag ⁺ ) uniformly, efficiently and continuously, thus having a good and long-lasting antibacterial effect, and are ideal antibacterial additives in various skin care and cosmetic applications. There have been many reports on methods for preparing nano-silver, most of which are chemical reduction methods. In these methods, silver salts and appropriate reducing agents are reacted in water as a solvent, and appropriate surfactants are added to obtain particle diameters between Nanoscale Silver Elemental Particles (Zhang Xiaomin, Zhang Zhenzhong, Zhao Fangxia, Qiu Tai, Research on Preparation of Highly Dispersive Nano Silver Powder by Orthogonal Design Optimization, Materials Engineering, 2013, November, 38-42; Liu Yan'e, Yin Lisong, Fan Hailu, Yang Suyu, Lu Yu'e, Guo Zhibo, Chen Qipeng, Synthesis and Characterization of Spherical Silver Nanoparticles by Hydrothermal Method, Materials Review, 2010, 24, 132-134), and the Formation of Aqueous Sol System Containing Nanosilver (Luo Xiaohong, Jiang Yucai, Wang Yanlei, A Nanosilver The preparation method of sol, Chinese invention patent CN1669914A; Jiang Xuhong, Li Yan, Gu Chuanhu, Niu Yanyan, the preparation method of nano-silver sol, Chinese invention patent CN101885072A).

Glycerin is a colorless, odorless, sweet viscous liquid. It is not only cheap, but also has good moisture absorption and moisturizing effects. It is widely used in food, medicine, daily chemical and other industries. Glycerin has reducing properties at higher temperatures and can reduce silver ions to elemental silver. Reported a kind of adopting glycerol as reductive agent like Wei Qunyan, add organic macromolecular dispersant, under alkaline environment medium, reduce AgNO Aqueous solution prepares the method for nano _- silver powder (Wei Qunyan, Xie Gang, Yang Xiangjun, Li Rongxing, Wang Yu, Chen Jing, industrialized preparation of nano-silver powder with good dispersibility, non-ferrous metals (smelting part), 2006, 6, 46-54); Chen Jianbo et al. reported that silver oxide (Ag ₂ O) was used as In the aqueous solution containing polyvinylpyrrolidone and inorganic alkali, superfine silver powder was prepared by precipitation conversion method (Chen Jianbo, Li Qihou, Li Yuhu, Liu Zhiyong, Liu Zhihong, Preparation of superfine silver powder by precipitation conversion method using glycerol as reducing agent, Powder Metallurgy Material Science and Engineering, 2013, 18, 874-881).

However, in the current reports on the preparation of elemental silver particles involving glycerol, glycerol is only used as a reducing agent, and it is carried out under alkaline conditions, and the solvent is water. At present, there is no report on the preparation of nano-silver particles in anhydrous glycerin system, and there is no report on a stable nano-silver-containing sol using anhydrous glycerol as a dispersion medium.

Contents of the invention

The object of the present invention is to provide a stable anhydrous glycerol sol containing nano-silver and its preparation method, comprising anhydrous glycerin as a dispersion medium, silver simple substance as dispersed phase particles and polyvinylpyrrolidone K30 as an auxiliary dispersant, said nano-silver-containing The anhydrous glycerol sol of silver is characterized by:

1. The anhydrous glycerol sol containing nano-silver does not contain water, and its appearance is a transparent, light yellow liquid with obvious Tyndall effect.

2. The silver single substance dispersed phase particles are in the nanometer scale, the particle diameter ranges from 2 to 70 nanometers, the appearance is nearly spherical, and can be uniformly dispersed in the glycerin dispersion medium.

3. The sol has good stability, can be stored at room temperature and air atmosphere for more than one month, and can resist high temperature less than 130°C and 100 times water dilution without being destroyed.

The technical scheme adopted to realize the object of the present invention is:

Step 1: Mix anhydrous glycerin and polyvinylpyrrolidone K30 in a round bottom flask with a mass ratio of 20: (0.3~1), place it in an oil bath, add a magnetic stirrer, stir with a magnetic stirrer, and stir at 90 Heat at ℃ for 20 minutes to dissolve polyvinylpyrrolidone K30 in anhydrous glycerin to form a clear glycerol solution.

Step 2: Add silver nitrate solid equivalent to 0.25%~1% of the glycerol mass fraction to the glycerin solution obtained in step 1, keep the heating temperature at 90°C and continue magnetic stirring to dissolve the silver nitrate in the glycerin solution to form a clear solution .

Step 3: Warm up the clear solution formed in step 2 to 110°C, and stir it magnetically at this temperature, react for 0.5-3 hours, and then cool to room temperature to obtain a yellow transparent anhydrous glycerol sol containing nano-silver.

The invention has simple steps, low cost of raw materials, low technical difficulty, and no waste discharge, and is environmentally friendly. The obtained anhydrous glycerin sol containing nano-silver can be stored and used stably for a long time, and the sol has good bactericidal effect of nano-silver particles , and the moisturizing and emollient effect of glycerin, it has good application prospects in the fields of skin care products, cosmetics, and personal care products.

Description of drawings

1. Fig. 1 is the transmission electron microscope figure of the silver element particle in the example one;

2. Fig. 2 is the transmission electron microscope picture of silver element particle in the example two;

3. Figure 3 is a transmission electron microscope image of the silver elemental particles in Example 3.

detailed description

Embodiment one,

1. Take 20g of glycerin and place it in a round bottom flask, add 0.3g of polyvinylpyrrolidone K300, place it in an oil bath, add a magnetic stirrer, stir with a magnetic stirrer, and heat at 90°C for 20 minutes to make the polyvinylpyrrolidone Vinylpyrrolidone K30 was dissolved in anhydrous glycerol to form a clear glycerol solution.

2. Add 0.07 g of silver nitrate solid equivalent to the mass fraction of glycerin to the glycerin solution obtained in step 1, keep the heating temperature at 90° C. and continue magnetic stirring to dissolve the silver nitrate in the anhydrous glycerin solution to form a clear solution.

3. Heat up the clear solution formed in step 2 to 110°C, and stir it magnetically at this temperature, react for 0.5 hours, and then cool to room temperature to obtain a yellow transparent anhydrous glycerin sol containing nano-silver.

After the silver element in the sol was separated, the obtained silver element was tested with a transmission electron microscope, which proved that the appearance of the obtained nano-silver particles was nearly spherical, and the particle size ranged from 2 to 17 nanometers (see Figure 1).

Embodiment two,

1. Put 20g of glycerin in a round bottom flask, add 0.5g of polyvinylpyrrolidone K3, place it in an oil bath, add magnets, stir with a magnetic stirrer, and heat at 90°C for 20 minutes to make the polyvinylpyrrolidone K30 was dissolved in anhydrous glycerol to form a clear glycerol solution.

2. Add silver nitrate solid equivalent to 0.1 g of glycerol mass fraction to the glycerin solution obtained in step 1, keep the heating temperature at 90° C. and continue magnetic stirring to dissolve the silver nitrate in the anhydrous glycerin solution to form a clear solution.

3. Heat up the clear solution formed in step 2 to 110°C, and stir it magnetically at this temperature, react for 1 hour, and then cool to room temperature to obtain a yellow transparent anhydrous glycerol sol containing nano-silver.

After the elemental silver in the sol was separated, the obtained elemental silver was tested with a transmission electron microscope, which proved that the obtained elemental silver particles were nearly spherical in appearance, and the particle size ranged from 3 to 15 nanometers (see Figure 2).

Embodiment three,

1. Put 20g of glycerin in a round bottom flask, add 0.3g of polyvinylpyrrolidone K3, place it in an oil bath, add magnets, stir with a magnetic stirrer, and heat at 90°C for 20 minutes to make the polyvinylpyrrolidone K30 was dissolved in anhydrous glycerol to form a clear glycerol solution.

2. Add silver nitrate solid equivalent to 0.1 g of glycerol mass fraction to the glycerin solution obtained in step 1, keep the heating temperature at 90° C. and continue magnetic stirring to dissolve the silver nitrate in the anhydrous glycerin solution to form a clear solution.

3. Heat up the clear solution formed in step 2 to 110°C, and stir it magnetically at this temperature, react for 3 hours, and then cool to room temperature to obtain a yellow transparent anhydrous glycerol sol containing nano-silver.

After the elemental silver in the sol was separated, the obtained elemental silver was tested with a transmission electron microscope, which proved that the obtained elemental silver particles were nearly spherical in appearance, and the particle size ranged from 15 to 70 nanometers (see Figure 3).

Claims (3)

1. containing an anhydrous glycerol colloidal sol for Nano Silver, comprising anhydrous glycerol is decentralized medium, and silver-colored simple substance is dispersed phase particles and PVP K30 is auxiliary dispersants, and the feature of the described anhydrous glycerol colloidal sol containing Nano Silver is:

The described anhydrous glycerol colloidal sol containing Nano Silver is not moisture, and outward appearance is yellow transparent liquid, has obvious Tyndall effect; Described silver-colored simple substance dispersed phase particles is in nanoscale, and its particle size range is 2-70 nanometer, and outward appearance is subsphaeroidal, can be dispersed in glycerine decentralized medium.

2. the anhydrous glycerol colloidal sol containing Nano Silver as claimed in claim 1, can in room temperature and air atmosphere long-term stable storage, and the high temperature and the water-reducible effect of 100 times amount that are less than 130 DEG C can be resisted and be not destroyed.

3. a preparation method for the anhydrous glycerol colloidal sol containing Nano Silver as claimed in claim 1, is characterized in that carrying out according to following steps:

Step 1: by anhydrous glycerol and PVP K30 with mass ratio 20:(0.3 ~ 1) be mixed in a round-bottomed flask, be placed in oil bath pan, add magnetic stir bar, by magnetic stirrer, heat 20 minutes at 90 DEG C, make PVP K30 be dissolved in anhydrous glycerol the glycerite forming clarification;

Step 2: add the silver nitrate solid being equivalent to qualities of glycerin number 0.25% ~ 1% in the glycerite of step 1 gained, heating-up temperature remains 90 DEG C and continues magnetic agitation, makes silver nitrate be dissolved in glycerite and forms settled solution;

Step 3: settled solution step 2 formed is warmed up to 110 DEG C, and magnetic agitation at this temperature, reaction 0.5-3 hour, then cool to room temperature, namely obtain the anhydrous glycerol colloidal sol containing Nano Silver of yellow transparent.