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Method and device for preparing nano-TiO2 functionalized micro-/nano-dispersion by supercritical CO2 fluid method

A supercritical, functionalized technology, applied in chemical instruments and methods, colloidal chemistry, colloidal chemistry, etc., can solve problems such as general dispersion conditions, and achieve the effect of preventing agglomeration and good dispersion.

Pending Publication Date: 2017-02-22
罗道友
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Comprehensive literature and patent reports, in the use of supercritical fluid technology to prepare functional nano-TiO 2 On the one hand, although supercritical technology can basically keep TiO 2 The liquid phase is removed under the original structure of the wet gel to prepare ultra-fine particles with low agglomeration, but in the application process of downstream products, nano-TiO 2 The degree of agglomeration of ultrafine particles is still relatively large, and the dispersion state is average, which limits the further development of its nano-efficiency and its application in different fields. In addition, the supercritical device for preparing ultrafine particles is different from the process and equipment to solve the problems of nanomaterials. Agglomeration is not the same as dispersion, and there is room for continuous improvement

Method used

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  • Method and device for preparing nano-TiO2 functionalized micro-/nano-dispersion by supercritical CO2 fluid method
  • Method and device for preparing nano-TiO2 functionalized micro-/nano-dispersion by supercritical CO2 fluid method
  • Method and device for preparing nano-TiO2 functionalized micro-/nano-dispersion by supercritical CO2 fluid method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: (1) take nanometer TiO 2 Powder (P25) 30g, absolute ethanol 386.1g, acetylacetone 2.1g, Triton X-1001.5g, copper phthalocyanine / dichloromethane mixed solution 0.30g (mass ratio of copper phthalocyanine / dichloromethane is 1 : 1, stirred and mixed in advance at normal temperature and pressure for 1 hour, the following examples are the same), added in the reactor D, after the reactor was sealed, heated to 45°C, stirred for 30min, and the rotating speed was 300rpm.

[0033] (2) The valve K1 will be opened, and the CO 2 into CO 2 Refrigerate to 5-6°C in the refrigerator, open the valve K2 after boosting by the booster pump, CO 2 The liquid is passed into the reactor D through the valve K3, and the supercritical temperature is kept at 45°C. After the pressure of the reactor reaches 8.5MPa, the valves K2 and K3 are closed, the stirring speed is 150-200rpm, and the supercritical time is 20min;

[0034] (3) Open the valve K5 or K6, feed 22-25°C circulating cooli...

Embodiment 2

[0035] Embodiment 2: (1) take by weighing nanometer TiO Powder (P25) 30g, dehydrated alcohol 382.1g, acetylacetone 4.2g, Triton X-1003.0g, copper phthalocyanine / dichloromethane mixed solution 0.30g, Add it into the reaction kettle D. After the reaction kettle is sealed, heat it to 45°C, stir for 30min, and rotate at 300rpm. Obtain the functionalized TiO of embodiment 2 by (2) and (3) steps in embodiment 1 2 micro-nano dispersion. Contrast the amount of surfactant on nano-TiO 2 The influence of the particle size and distribution of the agglomeration state of the agglomeration.

Embodiment 3

[0036] Embodiment 3: (1) take nanometer TiO 2 65g of powder (P25), 381.55g of absolute ethanol, 4.55g of acetylacetone, 3.25g of Triton X-100, and 0.65g of copper phthalocyanine / dichloromethane mixture were added to reactor D. After the reactor was sealed, , heated to 45°C, stirred for 30min, and the rotation speed was 300rpm. Obtain the functionalized TiO of embodiment 3 by (2) and (3) steps in embodiment 1 2 micro-nano dispersion. Contrast Nano TiO 2 The powder concentration (14.28%) on nano TiO 2 The effect of particle size and distribution on the state of agglomeration.

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Abstract

The invention relates to a method and device for preparing a nano-TiO2 functionalized micro- / nano-dispersion by a supercritical CO2 fluid method. The method comprises the specific steps of adding TiO2 nano-powder, anhydrous ethanol, surfactants such as acetylacetone and triton, and functionalization modified or doped adjuvants such as copper phthalocyanine into a reactor according to a certain ratio, carrying out heating and stirring dissolution, introducing refrigerated CO2 fluid into the reactor, and carrying out a supercritical mixing reaction, cooling depressurizing, exhausting decompression and cooling, thereby obtaining the concentration-adjustable functionalized TiO2 micro- / nano-dispersion. According to the device for preparing the nano-TiO2 functionalized micro- / nano-dispersion by the supercritical CO2 fluid method, disclosed by the invention, a U-shaped cooling coil in the reactor, a cooling water recirculating system, a three-layer-paddle stirrer and a CO2 liquefaction and re-pressurization system are designed, so that the control on nano particle size of the micro- / nano-dispersion is facilitated, and the agglomeration of nanoparticles is reduced. The method and the device are similarly applicable to the preparation of functionalized micro- / nano-dispersions of other nano-powders and organic solid compounds.

Description

technical field [0001] The invention relates to a method for preparing nano TiO 2 Method and device for functionalizing micro / nano dispersions, in particular using a supercritical CO 2 Preparation of Nano-TiO by Fluid Method 2 Methods and devices for functionalizing micro / nano dispersions. Background technique [0002] In recent years, nanomaterials have become a research and development hotspot in developed countries in the world, among which the research on nanometer metal oxides is one of the key directions. The functionalized nano-metal oxides and products researched and developed are used as photocatalytic materials, anti-pollution self-cleaning coatings, antibacterial materials, anti-ultraviolet absorbers, cosmetics, functional ceramics, photosensitive sensors, thermal / conductive and other high-efficiency functional materials. It has been widely used in the fields of pollution, sewage treatment and purification, and daily life. [0003] At present, most of the wide...

Claims

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Application Information

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IPC IPC(8): B01J13/00
CPCB01J13/0065B01J13/0069Y02P20/54
Inventor 罗道友
Owner 罗道友
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