CN103387257B - Method for preparing nano cerium dioxide material by utilizing tween-80 as surfactant - Google Patents

Abstract

The present invention relates to a method for preparing nano ceria material by using Tween-80 as surfactant, comprising: (1) dissolving Ce(NO ₃ ) ₃ .6H ₂ O in deionized water to obtain solution A; Dissolve sodium oleate and Tween-80 in deionized water to obtain solution B; mix solution A and solution B, then add cyclohexane, and react at 38-40°C to obtain an oil-soluble cerium precursor; (2) Dissolve sodium hydroxide in deionized water, stir evenly to obtain a hydroxide precursor; (3) Add the above hydroxide precursor to the above oil-soluble cerium precursor, stir to obtain a precursor solution, and then heat it at 170-190°C Reaction, final separation, washing and drying. The preparation method of the invention is simple, has good repeatability, can be mass-produced, and has low cost; the prepared oil-soluble cerium dioxide superfine powder has uniform particle size distribution, good dispersibility and good application prospect.

Description

Method for preparing nanometer ceria material with Tween-80 as surfactant

technical field

The invention belongs to the field of nano ceria materials, in particular to a method for preparing nano ceria materials by using Tween-80 as a surfactant.

Background technique

As a new type of functional material, nano ceria is widely used as catalytic material, ultraviolet absorber, polishing powder. The performance of nano ceria is closely related to its structure, morphology, size and size distribution, as well as the chemical and physical environment of the material itself. These properties can be adjusted by using different synthesis methods. Therefore, it is of great significance to study the controllable preparation technology of nano-ceria and explore the nucleation and growth mechanism of nano-ceria under different reaction conditions.

At present, the commonly used methods for preparing nano ceria materials mainly include precipitation method and microemulsion method. Although the precipitation method is easy to operate, the prepared nanoparticles are easy to agglomerate, and it needs to be roasted to obtain nano ceria. Nanomaterials synthesized by the microemulsion method have many excellent properties, but this method consumes a lot of surfactants and solvents during the preparation process, and it is difficult to remove these organic substances from the particle surface and the cost is high.

Contents of the invention

The technical problem to be solved by the present invention is to provide a method for preparing nano-cerium dioxide material using Tween-80 as a surfactant. The method is simple and convenient, has good repeatability, low temperature requirements, mass production, and low cost. The excellent oil-soluble ceria superfine powder has uniform particle size distribution, good dispersibility, and has good application prospects.

A kind of method of the present invention prepares nano ceria material with Tween-80 as surfactant, comprises:

(1) Dissolve Ce(NO ₃ ) ₃ .6H ₂ O in deionized water to obtain solution A; dissolve sodium oleate and Tween-80 in deionized water to obtain solution B; mix solution A and solution B , then add cyclohexane, and react at 38-40°C to obtain an oil-soluble cerium precursor;

(2) Dissolve sodium hydroxide in deionized water and stir evenly to obtain a hydroxide precursor;

(3) Add the above-mentioned hydroxide precursor to the above-mentioned oil-soluble cerium precursor, so that the volume ratio of the oil phase to the water phase is 1:1, stir magnetically at 38-40°C to obtain the precursor solution, and then React at 170-190°C for 24-28h, and finally separate, wash and dry.

The concentration of Ce(NO ₃ ) ₃ .6H ₂ O in solution A described in step (1) is 0.5M.

The concentration of sodium oleate in solution B in step (1) is 0.75M, and the dosage ratio of Tween-80 to deionized water is 0.995-5.953mL: 10mL.

The concentration of sodium hydroxide in the hydroxide precursor described in step (2) is 1M.

The addition rate of the hydroxide precursor described in step (3) was 160 mL/h.

The separation and washing described in step (3) is specifically to separate the product, add absolute ethanol to the obtained oil phase to obtain a large amount of precipitate, and then centrifuge at 8000rmp for 10min, and then successively wash the obtained precipitate with deionized water Wash alternately with absolute ethanol, and finally ultrasonically disperse and centrifuge.

The drying described in step (3) is drying at 50° C. for 12 hours.

The oil-water interface method means that the raw materials of the reactants are in the oil phase and the water phase respectively, and lipophilic nanoparticles with small particle size and excellent uniformity are formed at the oil-water interface at a lower temperature; It enters the oil phase under action, and has good dispersion in the oil phase and can be stored stably for a long time. The oil-water interface method has the advantages of mild reaction conditions, simple operation, controllable particle size, high product purity, high yield, good crystallinity, good dispersibility, small particle size, low cost and high efficiency. The oil-soluble nano ceria can be directly used in paints and cosmetics as an ultraviolet absorber, thereby reducing the steps of obtaining the oil-soluble nano ceria through surface modification of the water-soluble nano ceria.

Beneficial effect:

(1) The present invention has simple operation, mild reaction conditions, low price of experimental raw materials, good economy, and can be produced in large quantities;

(2) The obtained nano-cerium dioxide is uniformly dispersed and stable, and has good application prospects.

Description of drawings

Fig. 1 is the process flow diagram of preparing nano-cerium dioxide by the oil-water interface method with tween-80 as surfactant;

Fig. 2 is to take tween-80 as the oil-water interface method of surfactant to prepare nanometer ceria X-ray diffraction pattern;

Fig. 3 is the transmission electron microscope figure of embodiment 1 gained product;

Fig. 4 is the transmission electron microscope figure of embodiment 2 gained product;

Figure 5 is a transmission electron microscope image of the product obtained in Example 3.

Detailed ways

Below in conjunction with specific embodiment, further illustrate the present invention. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the teachings of the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of the present application.

Example 1

(1) Weigh 2.2834g (0.0075mol) sodium oleate and 2.976ml (0.0075mol) tween-80 and dissolve them completely in 10ml deionized water at 40°C, and weigh 1.0855g (0.0025mol) Ce(NO ₃ ) ₃ .6H ₂ O is completely dissolved in 5ml of deionized water, mix the two and add 25ml of cyclohexane, magnetically stir for 0.5h, and save for later use;

(2) Weigh 0.4g (0.01mol) of sodium hydroxide, dissolve it in 10ml of deionized water at room temperature, stir it evenly with magnetic force, and store it for later use;

(3) Add the sodium hydroxide prepared in step (2) dropwise to the cerium precursor solution prepared in step 1 at a rate of 160ml/h, and stir magnetically at 40°C for 10h (the volume ratio of the oil phase to the water phase is 1 :1) to obtain the precursor solution; transfer the obtained precursor solution to the reaction kettle, react at 180°C for 24 hours, stop the reaction, cool to room temperature naturally, separate the oil phase with a separatory funnel, add absolute ethanol to produce a large amount of precipitation, 8000rmp Centrifuge for 10 min, wash with deionized water and absolute ethanol three times alternately, and finally dry at 50° C. for 12 h to obtain the product.

Example 2

(1) Weigh 2.2834g (0.0075mol) sodium oleate, 5.953ml (0.015mol) tween-80 is completely dissolved in 10ml deionized water at 40°C, and weigh 1.0855g (0.0025mol) Ce(NO ₃ ) ₃ .6H ₂ O is completely dissolved in 5ml of deionized water, mix the two and add 25ml of cyclohexane, magnetically stir for 0.5h, and save for later use;

(2) Weigh 0.4g (0.01mol) of sodium hydroxide, dissolve it in 10ml of deionized water at room temperature, stir it evenly with magnetic force, and store it for later use;

(3) Add the sodium hydroxide prepared in step (2) dropwise to the cerium precursor solution prepared in step 1 at a rate of 160ml/h, and stir magnetically at 40°C for 10h (the volume ratio of the oil phase to the water phase is 1 :1) to obtain the precursor solution. Transfer the obtained precursor solution to a reaction kettle, react at 180°C for 24 hours, stop the reaction, cool to room temperature naturally, separate the oil phase with a separatory funnel, add absolute ethanol to produce a large amount of precipitation, centrifuge at 8000rmp for 10min, deionized water and anhydrous Alternately washed with water and ethanol for 3 times, and finally dried at 50°C for 12 hours to obtain the product.

Example 3

(1) Weigh 2.2834g (0.0075mol) of sodium oleate, 0.995ml (0.0025mol) of tween-80 is completely dissolved in 10ml of deionized water at 40°C, and weigh 1.0855g of Ce(NO ₃ ) ₃ .6H ₂ O completely Dissolve in 5ml deionized water, mix the two and add 25ml cyclohexane, stir magnetically for 0.5h, save for later use;

(2) Weigh 0.4g (0.01mol) of sodium hydroxide, dissolve it in 10ml of deionized water at room temperature, stir it evenly with magnetic force, and store it for later use;

(3) Add the sodium hydroxide prepared in step (2) dropwise to the cerium precursor solution prepared in step 1 at a rate of 160ml/h, and stir magnetically at 40°C for 10h (the volume ratio of the oil phase to the water phase is 1 :1) to obtain the precursor solution. Transfer the obtained precursor solution to a reaction kettle, react at 180°C for 24 hours, stop the reaction, cool to room temperature naturally, separate the oil phase with a separatory funnel, add absolute ethanol to produce a large amount of precipitation, centrifuge at 8000rmp for 10min, deionized water and anhydrous Alternately washed with water and ethanol for 3 times, and finally dried at 50°C for 12 hours to obtain the product.

Claims (7)

1. a kind of method that surfactant prepares nano ceria material with Tween-80, comprising: (1) Dissolve Ce(NO ₃ ) ₃ .6H ₂ O in deionized water to obtain solution A; dissolve sodium oleate and Tween-80 in deionized water to obtain solution B; mix solution A and solution B , then add cyclohexane, and react at 38-40°C to obtain an oil-soluble cerium precursor; (2) Dissolve sodium hydroxide in deionized water and stir evenly to obtain a hydroxide precursor; (3) Add the above-mentioned hydroxide precursor to the above-mentioned oil-soluble cerium precursor, so that the volume ratio of the oil phase to the water phase is 1:1, stir magnetically at 38-40°C to obtain the precursor solution, and then React at 170-190°C for 24-28h, and finally separate, wash and dry. 2. A method for preparing nano-cerium oxide materials using Tween-80 as a surfactant according to claim 1, characterized in that: Ce(NO ₃ ) ₃ in solution A described in step (1) The concentration of .6H ₂ O is 0.5M. 3. A kind of method according to claim 1 using Tween-80 as surfactant to prepare nano-cerium oxide material, it is characterized in that: the concentration of sodium oleate in solution B described in step (1) is 0.75 M, the dosage ratio of Tween-80 and deionized water is 0.995-5.953mL: 10mL. 4. A method for preparing nano-cerium oxide materials using Tween-80 as a surfactant according to claim 1, characterized in that: sodium hydroxide in the hydroxide precursor described in step (2) The concentration is 1M. 5. A method for preparing nano-cerium oxide materials with Tween-80 as a surfactant according to claim 1, characterized in that: the addition rate of the hydroxide precursor described in step (3) is 160mL/h. 6. A method for preparing nano-cerium oxide materials using Tween-80 as a surfactant according to claim 1, characterized in that: the separation and washing described in step (3) is specifically after the product is separated, Add absolute ethanol to the obtained oil phase to obtain a large amount of precipitate, then centrifuge at 8000rmp for 10min, then alternately wash the obtained precipitate with deionized water and absolute ethanol, and finally ultrasonically disperse and centrifuge. 7 . A method for preparing nano ceria material by using Tween-80 as surfactant according to claim 1 , characterized in that the drying in step (3) is at 50° C. for 12 hours.