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Preparation method of basic magnesium borate nanorods

A magnesium borate and nanorod technology, applied in borates, nanotechnology, nanotechnology and other directions, can solve the problems affecting the mechanical properties of composite materials, increase the complexity of the process, increase the production cost, etc., so as to improve the mechanical properties, Good dispersibility and the effect of improving flame retardant properties

Active Publication Date: 2019-02-01
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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Problems solved by technology

[0004] Although there are some reports on the synthesis of basic magnesium borate by hydrothermal method at present, the basic magnesium borate of existing hydrothermal synthesis often has stricter requirements on the pH value, and it is necessary to continuously control the pH value in the process, which increases the complexity of the process. the complexity
In addition, since basic magnesium borate nanorods react in the saturated state of salt solution during the synthesis process, the prepared basic magnesium borate nanorods have serious flocculent aggregates. When magnesium borate is used as a reinforcing agent, it will seriously affect the mechanical properties of the composite material, so it cannot be directly used in the composite material to improve its mechanical properties; and the method to solve this problem in the existing preparation method is often to add a crystal form inducer and surfactants to realize the directional growth of its crystal form, which not only increases the production cost, but also introduces unnecessary impurities

Method used

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  • Preparation method of basic magnesium borate nanorods
  • Preparation method of basic magnesium borate nanorods
  • Preparation method of basic magnesium borate nanorods

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preparation example Construction

[0043] refer to figure 1 , the preparation method of the basic magnesium borate nanorod comprises the following steps:

[0044] In step S1, magnesium nitrate and boric acid are formulated into a mixed solution according to the ratio of 1-3:1-4, and the temperature of the mixed solution is raised to not lower than 40°C.

[0045] The temperature of the mixed solution is preferably raised to 40°C to 60°C.

[0046]Specifically, in the mixed solution, the concentration of magnesium nitrate is controlled to be 0.5 mol / L-2 mol / L, and the concentration of boric acid is 0.75 mol / L-3 mol / L.

[0047] Preferably, in order to obtain a uniformly dispersed mixed solution, the stirring speed is controlled at 150 rpm to 450 rpm, that is, the temperature of the mixed solution is raised to not lower than 40° C. under strong stirring conditions.

[0048] In step S2, the mixed solution is passed into the ammonia solution at a rate of 0.5 mL / min-1.5 mL / min for reaction to obtain a suspension.

...

Embodiment 1

[0062] (1) Magnesium nitrate hexahydrate and boric acid are added in open container A, and 300mL mixed solution is configured; in this mixed solution, the molar concentration of magnesium nitrate is 0.5mol / L, and the molar concentration of boric acid is 0.75 mol / L; and the mixed solution was heated up to 50°C and stirred vigorously until the solute magnesium nitrate hexahydrate and boric acid were completely dissolved.

[0063] (2) Take 22 mL of ammonia water with a mass concentration of 28% and add it into the open container B as an ammonia solution, heat up to 50° C., and stir vigorously.

[0064] (3) Add the mixed solution in the open container A to the ammonia solution in the open container B at a rate of 1.5 mL / min to react to obtain a white suspension.

[0065] (4) Add the above white suspension into the high-temperature reactor C, and conduct a hydrothermal reaction at 190° C. under strong stirring for 10 hours to obtain a slurry.

[0066] (5) Filter the slurry and was...

Embodiment 2

[0068] (1) Magnesium nitrate hexahydrate and boric acid are added in open container A, and 300mL mixed solution is configured; in this mixed solution, the molar concentration of magnesium nitrate is 0.5mol / L, and the molar concentration of boric acid is 0.75 mol / L; and the mixed solution was heated up to 50°C and stirred vigorously until the solute magnesium nitrate hexahydrate and boric acid were completely dissolved.

[0069] (2) Take 22 mL of ammonia water with a mass concentration of 28% and add it into the open container B as an ammonia solution, heat up to 50° C., and stir vigorously.

[0070] (3) Add the mixed solution in the open container A to the ammonia solution in the open container B at a rate of 1.5 mL / min to react to obtain a white suspension.

[0071] (4) The above white suspension was added to the high-temperature reactor C, and hydrothermally reacted at 190° C. for 10 h under vigorous stirring to obtain a slurry, which was aged at room temperature for 15 days...

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Abstract

The invention provides a preparation method of basic magnesium borate nanorods, comprising the steps of S1, mixing magnesium nitrate and boric acid in a mass ratio of (1-3):(1-4) to form a mixed solution, and heating the mixed solution to not less than 40 DEG C; S2, introducing the mixed solution into an ammonia solution at a speed of 0.5-1.5 mL / min to carry out reacting to obtain a suspension, wherein the mass ratio of NH3 H2O in the mixed solution to a water-soluble magnesium salt in the mixed solution is (1-5):(1-3); S3, subjecting the suspension to hydrothermal reaction at 190-220 DEG C for 10-25 h to obtain a slurry; S4, subjecting the slurry to solid-liquid separation, washing, and drying to obtain the basic magnesium borate nanorods. The materials used in the preparation method areeasy to obtain, the preparation method is environmentally friendly, and energy consumption is low; without precisely controlling pH value of a reaction system or adding a shape control agent during reaction, the basic magnesium borate nanorods which are good in dispersibility and regular in shape can be prepared.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic materials, and specifically relates to a preparation method of basic magnesium borate nanorods. Background technique [0002] In recent years, nanostructured materials, such as nanotubes, nanoribbons, nanowires, nanorods, and nanowhiskers, have received extensive attention. Because nanostructured materials have high strength, heat resistance, corrosion resistance, electrical conductivity, excellent mechanical and thermal properties, they are widely used in environmental protection, biomedicine, composite materials, optoelectronics and other fields. Today, my country is rich in magnesium and boron resources, but due to the constraints of technology, climate and other reasons, the utilization rate of magnesium and boron resources is low, and resources are seriously wasted. At present, magnesium salt products are mostly low-value-added magnesium hydroxide, magnesium chloride, magnes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/12B82Y30/00
CPCB82Y30/00C01B35/126C01P2002/80C01P2002/72C01P2004/16C01P2004/03
Inventor 刘志启李娜李丽娟
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI