CN104230177A - Preparation method of nano ATO aqueous slurry - Google Patents

Abstract

The invention relates to a preparation method of nano ATO slurry. The present invention disperses nano-ATO powder in water; adds defoamer and dispersant at normal temperature and pressure, adjusts pH value to 3.0-7.0, and obtains nano-ATO slurry by high-speed shearing-ultrasonic dispersion-high-speed centrifugation. The preparation cost of the present invention is low, the process is simple, the solid content of the prepared water-based slurry is 3%-30%, the dispersant accounts for 0.5%-6% of the mass of nano-ATO, and the ATO water-based dispersion liquid prepared by this method can be stored stably More than 3 months, can be widely used in various antistatic, radiation protection, transparent heat insulation coating materials.

Description

A kind of preparation method of nanometer ATO aqueous slurry

(1) Technical field

The invention relates to a nano-ATO aqueous slurry.

(2) Background technology

In recent years, with the development of economy and science and technology, people pay more and more attention to energy conservation and environmental protection. The poor thermal insulation performance of building doors and windows accounts for a large proportion of the energy consumption of heating and cooling equipment, which is an important factor in energy conservation and reduction of energy consumption. object.

Nano-ATO is an n-type transparent semiconductor material, which combines the properties of ATO and nano-materials, and has excellent transparent heat insulation, electrical conductivity, weather resistance and stability. Nano-ATO transparent heat insulation can well solve the contradiction between lighting and heat insulation of architectural glass, and nano-ATO transparent heat-insulation coating has a broad application market. Compared with nano-ITO, nano-ATO has similar performance but lower cost, and has higher cost performance in transparent heat-insulating coatings, and has become a superior alternative material.

Due to the small particle size, large specific surface area, high surface energy and rich hydroxyl groups on the surface, nano-ATO is easy to agglomerate during preparation, storage, transportation and application. After agglomeration, many superior properties of nanomaterials are greatly reduced or even lost. In addition, nano-ATO Direct application of particles not only seriously agglomerates, but also makes it difficult to disperse evenly. Therefore, nano-ATO needs to be made into a dispersion liquid to achieve the purpose of preventing agglomeration and being easy to disperse. Nano-ATO water-based dispersions use water as a solvent for low cost, and have no organic volatiles to meet environmental protection requirements, and have become the direction of development.

At present, silane coupling agent and ball milling are used in the preparation of nano-ATO dispersion liquid, which has the disadvantages of expensive dispersant and long preparation time. The present invention uses low-priced dispersant to efficiently and rapidly prepare nano-ATO dispersion liquid.

(3) Contents of the invention

The object of the present invention is to disclose a kind of low-cost, high-efficiency, the method for preparing nano-ATO water-based slurry rapidly, and its preparation steps are as follows;

The first step is to mix nano-ATO powder, deionized water, defoamer and dispersant in proportion, and stir to obtain a mixed solution.

Among them, the mass of nano ATO accounts for 3%-30% of the whole system, the mass of defoamer accounts for 0.05%-1% of the whole system, and the mass of dispersant accounts for 0.5%-6% of the mass of nano-ATO powder.

The dispersant is one or more of citric acid, sodium oleate, polyvinylpyrrolidone and polyacrylic acid.

The second step is to adjust the pH value of the above mixed solution with lye, high-speed shear dispersion at normal temperature and pressure, and then ultrasonic treatment and high-speed centrifugation to obtain the nano-ATO slurry

The lye is one of sodium hydroxide and ammonia water.

The mechanical dispersion process is to adjust the pH value of the mixture to 3-7, the high-speed shear time is 2-8 hours, and the ultrasonic time is 5-30 minutes.

The ultrasonic treatment is carried out under the cooling condition of water circulation.

The high-speed centrifugation speed is 1000-4000 rpm, and the centrifugation time is 10-30 minutes.

(4) Specific implementation methods

Example 1

At room temperature, measure 45mL of deionized water, 5g of nano-ATO, 0.05g of defoamer, and 0.15g of citric acid, put the above substances in a 250mL three-necked flask, and adjust the pH to 4.5 with 2mol L-1 sodium hydroxide solution, Under normal temperature and pressure, shear at high speed for 5 hours, ultrasonically disperse for 20 minutes under circulating water cooling, and then centrifuge to remove larger particles at a speed of 3000rpm, centrifuge for 20 minutes to obtain a well-dispersed nano-ATO dispersion, which can be placed stably More than 3 months without obvious settlement and precipitation visible to the naked eye.

Example 2

At room temperature, measure 40mL of deionized water, 2g of ATO, 0.03g of defoamer, 0.06g of citric acid, and 0.03g of sodium oleate. Adjust the pH of the sodium solution to 4.5, under normal temperature and pressure, high-speed shear for 4 hours, ultrasonically disperse for 20 minutes under the cooling of circulating water, and then centrifuge to remove larger particles at a speed of 3000rpm, and centrifuge for 20 minutes to obtain well-dispersed nanoparticles. ATO dispersion can be placed stably for more than 3 months without obvious settlement and precipitation visible to the naked eye.

The above descriptions are only preferred specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto.

Claims (7)

1. a nano ATO water paste, its characteristic sum is preparation method comprise the steps:

The first step, is mixed in proportion nano ATO powder, deionized water, defoamer and dispersion agent, stirs to obtain mixed solution;

Second step, by above-mentioned mixed solution alkali lye adjusted to ph, high speed shear dispersion under normal temperature and pressure, then supersound process, high speed centrifugation, obtains described nano ATO slurry.

2. mixed solution nano ATO quality according to claim 1 accounts for 3% ~ 30% of whole system, and defoamer quality accounts for 0.05% ~ 1% of whole system, and dispersion agent quality accounts for 0.5% ~ 6% of nano ATO powder quality.

3. dispersion agent according to claim 1 is citric acid, sodium oleate, polyvinylpyrrolidone, one or more in polyacrylic acid.

4. alkali lye according to claim 1 is the one in sodium hydroxide, ammoniacal liquor.

5. adjustment mixed solution pH value to 3 ~ 7 according to claim 1, the high speed shear time is 2 ~ 8 hours, and ultrasonic time is 5 ~ 30 minutes.

6. ultrasonic for carry out under water cycle cooling conditions according to claim 1.

7. high speed centrifugation rotating speed is 1000-4000rpm according to claim 1, and centrifugation time is 10-30 minute.