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Preparation method of magnesium oxide nanocrystalline

A nanocrystalline and magnesium oxide technology, applied in the direction of magnesium oxide, nanotechnology, nanotechnology, etc., can solve the problems of limited shape and poor dispersion, and achieve the effects of fine particle size, improved dispersion and reduced production cost

Active Publication Date: 2016-01-27
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the bubbling method can effectively control the particle size and distribution of magnesium oxide nanocrystals, the control over its morphology is relatively limited, and the shape control of nanocrystals can only be realized through a few reaction factors.
In addition, the dispersibility of the samples prepared by the aforementioned method is poor, which needs to be improved

Method used

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  • Preparation method of magnesium oxide nanocrystalline
  • Preparation method of magnesium oxide nanocrystalline
  • Preparation method of magnesium oxide nanocrystalline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Weigh MgCl 2 ·6H 2 O18.52g, dissolved in 400mL of pH=10.0 buffer solution (buffer pair formed by ammonium chloride and ammonia water), added 1.8g of PEG1000 and 35mL of deionized water to form a transparent solution; the concentration can be adjusted as required;

[0042] (2) Heating while continuously feeding high-purity carbon dioxide gas into the transparent solution, raising the temperature to 60 degrees, and reacting for 2 hours; the feeding speed of carbon dioxide can be adjusted between 0.005 / 0.015, and the system is controlled at 0.01 L / h is suitable.

[0043] (3) quickly place the reaction system in an ice-water bath after the reaction;

[0044](4) The cooled product is subjected to suction filtration, washed with a large amount of deionized water to neutrality, and the obtained product is washed 1 to 2 times with absolute ethanol;

[0045] (5) the white reactant after suction filtration is dried overnight in an oven at 80 degrees;

[0046] (6) Calcinin...

Embodiment 2

[0050] This comparative example is basically the same as Example 1, the only difference being that the pH of the buffer solution is 11.0;

[0051] Among the magnesium oxide nanomaterials synthesized in this ratio, at first its intermediate products are different ( Figure 4 ), compared with figure 1 It can be found that when the alkalinity of the buffer solution used is enhanced, the intermediate product is basic magnesium carbonate. After calcining at 800 degrees, the obtained product is magnesia with higher crystallinity and purity ( Figure 5 ). From the FE-SEM characterization results of the samples before and after firing, it can be seen that ( Figure 6a and Figure 6b ), the intermediate is in the form of flakes before calcination, and becomes a three-dimensional short-forked magnesium oxide nanopowder after calcination. The longest branch is about 100nm, and the diameter is about 30nm.

Embodiment 3

[0053] This comparative example is substantially the same as Example 1, except that the reaction temperature is 40 degrees at room temperature;

[0054] In the magnesium oxide nanomaterial synthesized in this comparative example, its yield is low at first, only about 70% in the example. Contrast with example 1, in the same reaction time, by Figure 7 As can be seen, its intermediate product is different from example 1 ( Figure 7 ), generating basic magnesium carbonate. And in the sample after 800 degree of high temperature roasting, impurity is less, and product purity and crystallinity are high ( Figure 8 ). Referring to the FE-SEM figure ( Figure 9a and Figure 9b ), the intermediate product of the sample was fibrous before roasting, and granular after roasting, with a particle size of about 20nm and good dispersibility.

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Abstract

The invention discloses a preparation method of magnesium oxide nanocrystalline. The method comprises the following steps that 1, soluble magnesium salt or a hydrate of the soluble magnesium salt and surfactants are dissolved in an alkaline buffer solution; 2, carbon dioxide gas is introduced into the transparent solution in a bubbling mode; 3, the solution is heated for reacting for 1-4 hours; 4, products obtained in the step 3 are filtered, washed with deionized water until the washed water is neutral and then washed with absolute ethyl alcohol for 1-2 times; 5, white precipitates obtained in the step 4 are dried for 10 hours at the temperature of 50 DEG C-80 DEG C; 6, white solids dried in the step 5 are calcined to obtain the magnesium oxide nanocrystalline. According to the preparation method of the magnesium oxide nanocrystalline, on the basis of all the excellent properties of a carbonization method, all the surfactants serve as morphology guiding agents, the defect that a sample prepared through an ordinary carbonization method is prone to being influenced by Na<+> and K<+>, and the problems that the ordinary carbonization method is heavy in environmental pollution, high in cost and the like are also solved.

Description

technical field [0001] The invention belongs to the field of nanomaterial preparation, and in particular relates to a preparation method of magnesium oxide nanocrystals. Background technique [0002] Magnesium oxide powder is not only widely used in aerospace, chemical industry, etc., but the optical, magnetic and mechanical properties of magnesium oxide nanocrystals with greatly reduced size have changed to varying degrees due to quantum effects, thus endowed with different performance. The application requirements of magnesium oxide nanocrystals in various transparent devices and high-performance catalyst supports make the effective control of their morphology particularly important. [0003] Up to now, in addition to the direct calcination of magnesite to prepare magnesium oxide powder, liquid magnesium resources are usually used through the milk of lime method, ammonium bicarbonate method, ammonia method, soda ash method, ammonium bicarbonate ammonia water pyrolysis met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F5/02B82Y30/00
Inventor 海春喜周园李松都永生任秀峰申月曾金波董欧阳李翔张丽娟
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI