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Mild hydrothermal-thermal transition synthetic method for high-draw-ratio hydrated and anhydrous calcium borate nanowhisker

A calcium borate hydrate and synthesis method technology, applied in chemical instruments and methods, nanotechnology, single crystal growth, etc., can solve the problems of long calcination time, increased cost, small long diameter, etc., and achieve low cost, high crystallinity, The effect of mild conditions

Active Publication Date: 2016-08-03
QUFU NORMAL UNIV
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  • Claims
  • Application Information

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Problems solved by technology

CN102154682A discloses a preparation method of calcium borate whiskers. The precursor is hydrothermally heated at 90-200oC for 1-25h in a homogeneous reactor to obtain fan-shaped bundles of calcium borate hydrate and rod-shaped whiskers (molecular formula Ca 2 B 2 o 5 ·H 2 O), but its diameter is in the order of microns, and the aspect ratio is small
CN103422168A discloses a method for preparing calcium chloroborate whiskers. By using calcium-containing, boron-containing and chlorine-containing compounds as raw materials, the precursor obtained at room temperature is calcined to obtain calcium chloroborate whiskers (molecular formula Ca 2 B 5 o 9 Cl), the particle diameter of the product is micron / submicron, and the length-to-diameter ratio is smaller than that of the previously reported calcium borate hydrate whisker. At the same time, due to the long calcination time and high energy consumption, the cost increases

Method used

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  • Mild hydrothermal-thermal transition synthetic method for high-draw-ratio hydrated and anhydrous calcium borate nanowhisker
  • Mild hydrothermal-thermal transition synthetic method for high-draw-ratio hydrated and anhydrous calcium borate nanowhisker
  • Mild hydrothermal-thermal transition synthetic method for high-draw-ratio hydrated and anhydrous calcium borate nanowhisker

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Embodiment 1

[0042] A mild hydrothermal-thermal conversion synthesis method of high aspect ratio hydrated and anhydrous calcium borate nano-whiskers, comprising the following steps: (1) adding 30ml of H 2 O was added to a beaker containing 0.002mol calcium nitrate and 0.01mol boric acid, and the mixed solution was obtained after heat treatment in a 40oC water bath for 10 minutes; (2) 20mL1.5mol / L NaOH solution was added dropwise to the mixed solution, and continued to Heat treatment for 30 minutes under the same conditions to obtain the slurry; (3) Transfer the slurry to the hydrothermal reaction kettle, raise the temperature to 180oC, keep the temperature for 12.0h, and then naturally cool to room temperature to obtain the hydrothermal product; (4) Wash and filter the hydrothermal product , 70oC drying 12.0h, 0.164gCa 2 B 2 o 5 ?H 2 O nano whiskers; (5) 0.050g Ca 2 B 2 o 5 ?H 2 O nano whiskers are placed in a tube furnace, heated at a rate of 5oC / min to 500oC, roasted under nitroge...

Embodiment 2

[0045] A mild hydrothermal-thermal conversion synthesis method of high aspect ratio hydrated and anhydrous calcium borate nano-whiskers, comprising the following steps: (1) adding 30mL of H 2 O was added to a beaker containing 0.005mol calcium chloride and 0.018mol boric acid, and the mixture was obtained after heat treatment in a 60oC water bath for 5 minutes; (2) 20mL3mol / L KOH solution was added dropwise to the mixed solution, and continued to Heat treatment for 30 minutes to obtain the slurry; (3) Transfer the slurry to the hydrothermal reaction kettle, raise the temperature to 150oC, keep the temperature for 12.0h, and then cool it to room temperature naturally to obtain the hydrothermal product; (4) Wash and filter the hydrothermal product, Dry at 90oC for 16.0h to get 0.237g Ca 2 B 2 o 5 ?H 2 O nano whiskers; (5) 0.100g Ca 2 B 2 o 5 ?H 2 O nano whiskers are placed in a tube furnace, the temperature is raised to 400oC at a rate of 10oC / min, roasted in a water vapo...

Embodiment 3

[0048] A mild hydrothermal-thermal conversion synthesis method of high aspect ratio hydrated and anhydrous calcium borate nano-whiskers, comprising the following steps: (1) adding 30mL of H 2 O was added to a beaker containing 0.006mol calcium acetate and 0.005mol borax, and the mixture was obtained after ultrasonic dispersion for 15 minutes under heat treatment in a water bath at 50oC; (2) 2.5mol / L NaOH and KOH were mixed in a volume ratio of 1:1 20 mL of the obtained mixed solution was added dropwise to the mixed solution, and continued to be heat-treated in a 50oC water bath for 20 minutes to obtain a slurry; (3) Transfer the slurry to a hydrothermal reaction kettle, raise the temperature to 200oC, keep the temperature for 2.0h, and then naturally cool to room temperature The hydrothermal product was obtained; (4) the hydrothermal product was washed, filtered, and dried at 80oC for 12.0h to obtain 0.325g Ca 2 B 2 o 5 ?H 2 O nano whiskers; (5) 0.100g Ca 2 B 2 o 5 ?H 2...

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Abstract

The invention relates to a mild hydrothermal-thermal transition preparation method for high-draw-ratio hydrated and anhydrous calcium borate nanowhisker and belongs to the technical field of chemical new materials. The method comprises the steps of mixing a calcium compound and a boron compound with water, conducting thermal treatment in a water bath at 40-70 DEG C for 5-20 min, adding inorganic base solution to calcium-boron mixed liquor dropwise, and continuing thermal treatment in a water bath at 50-90 DEG C for 10-50 min, so that precursor size is obtained; placing the precursor size in a hydrothermal reaction kettle, and increasing temperature to 120-240 DEG C for thermostatic reaction for 2.0-18.0 h, so that a hydrated calcium borate nanowhisker wet product is obtained. The high-draw-ratio hydrated calcium borate (Ca2B2O5-H2O) nanowhisker high in purity and crystallinity degree is synthesized with the mild hydrothermal method for the first time, then phase transformation is achieved through medium temperature roast thermal transition for crystal water removal to obtain high-draw-ratio anhydrous calcium borate (Ca2B2O5) nanowhisker high in purity and crystallinity degree and staying in good morphology, and then controllable synthesis of the high-draw-ratio 1D calcium borate nanowhisker is achieved.

Description

technical field [0001] The invention relates to a mild hydrothermal-thermal conversion synthesis method of hydrated and anhydrous calcium borate nano-whiskers with high aspect ratio, belonging to the technical field of new chemical materials. Background technique [0002] Nanomaterials such as nanowires / tubes / whiskers have become one of the research hotspots due to their unique one-dimensional (1D) structure and wide application prospects in the fields of electronics, catalysis, optics, and energy. The extent depends on its morphology, aspect ratio and crystallinity, so it is of great practical significance to prepare 1D nanomaterials with high crystallinity, high aspect ratio and special morphology through controllable synthesis. There are many kinds and compositions of borates, which play an increasingly prominent role in high-tech, and have attracted people's attention in recent years. Affected by it, the research and application of borate inorganic nanomaterials have de...

Claims

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Application Information

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IPC IPC(8): C30B29/10C30B29/62C30B7/10B82Y40/00
CPCB82Y40/00C30B7/10C30B29/10C30B29/62
Inventor 朱万诚张照强翟奎露朱林张强
Owner QUFU NORMAL UNIV
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