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Hydration and anhydrous multistage porous calcium borate microsphere low-temperature hydrothermal-thermal conversion synthetic method

A synthetic method, calcium borate technology, applied in the direction of boron oxides, borates, etc., to achieve the effect of pure composition, cheap and easy-to-obtain raw materials, and low energy consumption

Inactive Publication Date: 2015-08-05
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For calcium borate nanomaterials with specific three-dimensional morphology, Liu Zhihong et al. reported an oval 4CaO?5B synthesized with PEG-300 as a surfactant. 2 o 3 ?7H 2 Except for O microspheres, the synthesis and application of other calcium borate-related three-dimensional hierarchical materials are rarely reported.

Method used

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  • Hydration and anhydrous multistage porous calcium borate microsphere low-temperature hydrothermal-thermal conversion synthetic method
  • Hydration and anhydrous multistage porous calcium borate microsphere low-temperature hydrothermal-thermal conversion synthetic method
  • Hydration and anhydrous multistage porous calcium borate microsphere low-temperature hydrothermal-thermal conversion synthetic method

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Embodiment 1

[0033] A low-temperature hydrothermal-thermal conversion synthesis method of hydrated and anhydrous multi-level porous calcium borate microspheres, comprising the following steps: (1) adding 10 ml of ammonia water to 10 ml of 0.5 mol / L calcium chloride solution, Mix evenly to obtain a mixed solution; (2) Add 0.005 mol of borax solid powder to the mixed solution, add 20 ml of water, and stir for 10 min to obtain a slurry; (3) Put the slurry in a hydrothermal reaction kettle, Heat up to 120 oC, react at constant temperature for 9.0 h, then cool down to room temperature naturally to obtain the hydrothermal product; (4) wash and filter the hydrothermal product in sequence, and dry at 70 oC for 12.0 h to obtain Ca 4 B 10 o 19 ?7H 2 O microspheres; (5) Ca 4 B 10 o 19 ?7H 2 O microspheres were placed in a calcination furnace, and the temperature was raised to 650 oC at a rate of 5 oC / min. After calcination for 12.0 h, the crude product was naturally cooled to room temperature t...

Embodiment 2

[0036] A low-temperature hydrothermal-thermal conversion synthesis method of hydrated and anhydrous multi-level porous calcium borate microspheres, comprising the following steps: (1) adding 2 ml of ethylenediamine to 10 ml of 0.8 mol / L calcium chloride solution , mixed evenly to obtain a mixed solution; (2) Add 0.005 mol of borax solid powder to the mixed solution, add 20 ml of water, and stir for 10 min to obtain a slurry; (3) Put the slurry in a hydrothermal reaction kettle Inside, heat up to 100 oC, react at constant temperature for 12.0 h, then naturally cool to room temperature to obtain the hydrothermal product; (4) The hydrothermal product was washed, filtered, and dried at 70 oC for 12.0 h to obtain Ca 4 B 10 o 19 ?7H 2 O microspheres; (5) Ca 4 B 10 o 19 ?7H 2 O microspheres were placed in a calcination furnace, and the temperature was raised to 750 oC at a rate of 5 oC / min. After calcination for 2.0 h, the crude product was naturally cooled to room temperature ...

Embodiment 3

[0040] A low-temperature hydrothermal-thermal conversion synthesis method of hydrated and anhydrous multi-level porous calcium borate microspheres, comprising the following steps: (1) adding 10 ml of 0.4 mol / L hydroxylamine hydrochloride solution to 10 ml of 0.8 mol / L Calcium chloride solution, mixed evenly to obtain a mixed solution; (2) Add 0.016mol boric acid solid powder to the mixed solution, add 10 ml of water, and stir for 10 min to obtain a slurry; (3) Put the slurry in In a hydrothermal reaction kettle, heat up to 150 oC, react at constant temperature for 6.0 h, then cool to room temperature to obtain a hydrothermal product; (4) wash and filter the hydrothermal product in sequence, and dry at 70 oC for 12.0 h to obtain Ca 4 B 10 o 19 ?7H 2 O microspheres; (5) Ca 4 B 10 o 19 ?7H 2 O microspheres were placed in a calcination furnace, and the temperature was raised to 650 oC at a rate of 10 oC / min. After calcination for 2.0 h, the crude product was naturally cooled...

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Abstract

The invention discloses a hydration and anhydrous multistage porous calcium borate microsphere low-temperature hydrothermal-thermal conversion synthetic method. The method comprises the steps of adding aqueous alkali into a calcium salt solution, adding borate solid powder into the mixture, supplementing water and performing stirring; putting the obtained slurry in a hydrothermal reaction kettle, raising the temperature to enable the slurry to be reacted, and washing, filtering and drying hydrothermal products to obtain hydration calcium borate (Ca4B10O19. 7H2O) microspheres; putting the microspheres in a roaster to be roasted, washing, filtering and drying the roasted microspheres to obtain anhydrous multistage porous calcium borate (Ca (BO2)2) microspheres. By the aid of the method, hydrothermal controllable preparation of Ca4B10O19.7H2O is achieved, subsequent medium-temperature roasting of hydrothermal products is used for achieving crystal water removal to obtain three-dimensional anhydrous multistage porous Ca (BO2)2 microspheres. The method has the advantages of being simple to operate, mild in condition, cheap and easy to obtain in material, capable of not adding any additives and the like and easy to produce industrially.

Description

technical field [0001] The invention relates to a low-temperature hydrothermal-thermal conversion synthesis method of hydrated and anhydrous multi-stage porous calcium borate microspheres, belonging to the technical field of inorganic chemical engineering. Background technique [0002] In recent years, three-dimensional multi-level porous materials have been widely used in electrochemistry, organic catalysis, sewage treatment and other fields due to their unique structure, large specific surface area, and low density, and have been favored by researchers. However, three-dimensional hierarchical porous materials are currently mainly synthesized by hydrothermal and solvothermal methods, and hydrothermal methods often need to add templates or inducers to the reaction system to assist their growth, but the addition of templates / inducers will not only bring The cumbersome follow-up treatment process is easy to cause product pollution, and it is easy to cause the collapse and dam...

Claims

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Application Information

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IPC IPC(8): C01B35/12
Inventor 朱万诚张照强张恒朱林张强
Owner QUFU NORMAL UNIV
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