Method for preparing nano material

A nanomaterial and nanotechnology, applied in the field of preparation of nanomaterials, can solve the problems of high cost, small particle diameter, easy agglomeration and other problems, and achieve the effects of energy saving, high product quality and no secondary pollution.

Inactive Publication Date: 2011-04-27
XIANGTAN UNIV
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Problems solved by technology

However, because the traditional chemical reaction precipitation process is often carried out in a stirred tank or packed tower reactor, it is difficult to control the product quality, and there are great differences in the particle diameter distribution and crystal phase of the product in different processing batches
[0004] Take the method of preparing α-alumina as an example: the solid-phase method is to grind and calcinate aluminum or aluminum salt to undergo a solid-phase reaction to directly obtain nano-alumina, but the particle size distribution of the obtained product is uneven, and agglomeration is prone to occur; The phase method is currently the most commonly used method for synthesizing nanomaterials. However, this method is easy to introduce impurities, which makes the product purity not high; the product obtained by the gas phase method has less agglomeration, good dispersion, small particle diameter and narrow distribution, but the yield is low. Powder is difficult to collect and expensive
Alumina is prone to particle agglomeration during the crystal transformation process, so it is difficult to obtain nano-scale products; in addition, due to the low purity of the alumina crystal phase and many miscellaneous peaks, the final product α-Al is calcined from different precursors. 2 o 3 The temperature range fluctuates typically between 1000 and 1500°C
Therefore, it is difficult to produce products with high crystallinity by ordinary methods of producing alumina

Method used

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Embodiment 1

[0037] Embodiment 1: Preparation of nanometer α-alumina

[0038] First prepare the precursor of nano pseudo-boehmite in the supergravity field: make the sodium metaaluminate solution and carbon dioxide gas contact and react in the supergravity to obtain the pseudo-boehmite suspension, and then perform aging, filtration, aging treatment, After the solid product is separated and dried, a solid nanoscale pseudo-boehmite precursor is obtained. Specifically, the gas-liquid ratio of sodium metaaluminate aqueous solution to carbon dioxide gas is 1-10:1, preferably 1-5:1; the carbon dioxide gas introduced consumes excess sodium hydroxide in the solution and destroys the aluminum Equilibrium system in sodium bicarbonate solution, resulting in pseudo-boehmite precipitate (AlOOH·nH 2 O). Therefore, the temperature for the reaction is 0-35°C, the rotational speed is controlled at 1000rpm, and the centrifugal acceleration in the supergravity field is 180-10000m / s 2 , preferably 1000-6000g...

Embodiment 11

[0043] Take a certain mass of sodium metaaluminate solution with a concentration of 0.15-0.30 mol / L, add 1-2% polyethylene glycol 400 organic polymer surface dispersant according to its mass ratio, and mix the mixed solution uniformly for use. CO 2 Gas backup. Start the spiral channel type rotating field supergravity bed to drive the reactor to rotate, control its speed at 1000-1200rpm, add the mixed liquid into the rotating reactor through the valve that can adjust the flow rate, adjust and control the mixed liquid flow rate to 400L / h, wait for After the flow stabilizes, open the CO 2 Gas valve, adjust the gas flow to make the gas-liquid flow ratio 1.5:1, so that CO 2 It also enters the rotating reactor, and carries out carbonization reaction with the existing sodium metaaluminate solution in the reactor, controls the reaction temperature below 35°C, measures the pH of the solution during the reaction, closes all valves when it reaches around 10.5, and the screw The channe...

Embodiment 12

[0047] The pseudo-boehmite was prepared according to the same method as in Example 1.1, except that the concentration of the sodium metaaluminate solution was 0.3-0.5 mol / L. Experiments show that: increasing the concentration of reactants will prolong the carbonization reaction time. When the concentration is higher than 0.5mol / L, the solution will return to alkali during the carbonization process, which is not conducive to the carbonization reaction to prepare nano-pseudo-boehmite.

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Abstract

The invention relates to a method for preparing a nano material, which comprises the step of: preparing a nano material precursor and a nano material. The method for preparing the nano material precursor comprises the step of: placing reacting raw materials in a supergravity filed reactor for gas-liquid reaction or liquid-liquid reaction to obtain the nano material precursor. The method for preparing the nano material comprises the step of heating and roasting the nano material precursor with a microwave field to ensure that the nano material precursor generates decomposition or recrystallization to obtain the nano material. The method for preparing the nano material precursor also comprises the step of: in a process of accelerating and enhancing the mass transfer with the supergravity filed, enabling a metal salt water solution in the reactor to be uniformly mixed with a liquid precipitator or gas precipitator in a molecule size manner for chemical reaction to obtain the nano material precursor of carbonate materials or nano oxyhydrate materials or hydrous oxide materials of the metal, wherein the prepared nano material is used as a nano metal oxide. The method has the advantagesof scientific and reasonable structure, high quality of products, energy saving, no secondary pollution and the like.

Description

technical field [0001] The invention relates to a method for preparing nanomaterials. Background technique [0002] The study of nanomaterials is a frontier field in today's scientific research, and it is also a hot spot studied by many scientists all over the world. The magic and unknown aspects of nanomaterials have aroused people's widespread attention; the research and application of nanomaterials are currently hot spots and difficulties, and are also the focus of high-tech development. [0003] After continuous research and exploration, some methods for preparing nanomaterials have been developed. These methods include: physical vapor deposition, chemical vapor deposition, reactive precipitation, sol-gel, microemulsion , sonochemical processing, supercritical chemical processing, etc. Some nanomaterials are also synthesized by hydrothermal method. Among them, the chemical reaction precipitation method is easy to process, low in cost, and can be produced in large qua...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/14C01G9/02C01G45/02C01G23/00C09K11/80B82Y40/00
Inventor 周继承肖伶俐谢放华孟翔曾敏
Owner XIANGTAN UNIV
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