Hydrated calcium borate microsphere and anhydrous calcium borate microsphere, and preparation methods thereof

A calcium borate hydrate, calcium borate technology, applied in borates, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of product particle stability deviation, insufficient pore structure, wide diameter distribution, etc., to achieve mild conditions, Low cost and good thermal stability

Inactive Publication Date: 2016-11-09
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Zhu, W.C. et al reported a hierarchical calcium borate hydrate (Ca 4 B 10 o 19 ·7H 2 O) Superstructures (Zhu, W.C.; Wang, X.L. et al. Hierarchical laminar superstructures of rhombic priceite (Ca 4 B 10 o 19 ·7H 2 O): Facile hydrothermal synthesis,shape evolution,optical,and thermal decomposition properties.Cryst.Growth Des.2011,11:2935-2941.), but the size of the product is large, and due to the interaction force between diamond-shaped sheets and sheets Weak, resulting in product particle stability deviation, easy to disassemble, can not be roasted to obtain anhydrous calcium borate; publication number is CN104817094A Chinese patent also discloses a preparation of hydration and anhydrous multi-level porous by hydrothermal-thermal conversion The method of calcium borate microspheres, but the particle shape uniformity of the above products is poor, the surface of the microspheres is relatively smooth and dense, the pore structure is not rich enough, and the size of the microspheres is uneven, and the diameter distribution is broad

Method used

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  • Hydrated calcium borate microsphere and anhydrous calcium borate microsphere, and preparation methods thereof
  • Hydrated calcium borate microsphere and anhydrous calcium borate microsphere, and preparation methods thereof
  • Hydrated calcium borate microsphere and anhydrous calcium borate microsphere, and preparation methods thereof

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preparation example Construction

[0026] The invention provides a preparation method of calcium borate hydrate microspheres, comprising the following steps:

[0027] (1) mixing calcium salt, alkali source and water to obtain a mixed slurry;

[0028] (2) mixing the mixed slurry obtained in the step (1) with a surfactant to obtain a mixed solution;

[0029] (3) The mixed solution obtained in the step (2) is mixed with a boron source, and hydrothermally reacted to obtain hydrated calcium borate microspheres.

[0030] The present invention mixes calcium salt, alkali source and water to obtain mixed slurry. In the present invention, there is no special limitation on the mixing operation, and the method for preparing the mixed slurry well known to those skilled in the art can be used. In the present invention, the calcium salt is preferably mixed with water to obtain a calcium salt solution; then the calcium salt solution is mixed with alkali to obtain a mixed slurry. In the present invention, the mixing is prefe...

Embodiment 1

[0046] (1) Add 10 mL of deionized water into a beaker filled with 5 mmol of calcium nitrate solid, and stir magnetically at a speed of 400 rpm / min for 10 min to obtain a mixed solution;

[0047] (2) Dilute 10mL of 1mol·L -1 Add the KOH solution dropwise to the mixed solution at a rate of 3mL / min, and continue to stir at a speed of 400rpm / min for 10min to obtain a mixed slurry;

[0048] (3) Add 0.3125mmol EDTA-2Na solid into the mixed solution obtained in (2), and stir at 400rpm / min for 5min;

[0049] (4) 30mL containing 20mmol of H 3 BO 3 The solution was dripped into the mixed solution obtained in (3) at a rate of 3 mL / min, and continued to stir at a speed of 400 rpm / min for 15 min to obtain a hydrothermal precursor;

[0050] (5) Transfer the hydrothermal precursor to the hydrothermal reaction kettle, raise the temperature to 210°C at a heating rate of 10°C / min, keep the temperature for 1.0h, and then naturally cool to room temperature to obtain the hydrothermal product; ...

Embodiment 2

[0055] The hydrated calcium borate (Ca 4 B 10 o 19 ·7H 2 O) The microspheres are placed in a tube furnace, heated to 750°C at a heating rate of 10°C / min, calcined for 1.0h, and then naturally cooled to room temperature to obtain Ca(BO 2 ) 2 Microspheres.

[0056] The Ca(BO) prepared in this embodiment 2 ) 2 Microsphere XRD patterns such as image 3 shown. It can be seen from the figure that Ca(BO 2 ) 2 The XRD patterns of the microspheres match well with the XRD standard card JCPDS No.78-1277, and have very good crystallinity.

[0057] The Ca(BO) prepared in this embodiment 2 ) 2 The microsphere has a multi-level porous structure, the particle size is 9-14 μm, and the particle size distribution is uniform.

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Abstract

The invention provides a hydrated calcium borate microsphere and an anhydrous calcium borate microsphere, and preparation methods thereof. The preparation method of the hydrated calcium borate microsphere is characterized in that a hydrothermal-thermal conversion technology is adopted, a calcium salt, a boron source and an alkali source are adopted as raw materials, a surfactant is added to an aqueous solution in order to effectively regulate the composition and the morphology of products, and a hydrothermal reaction is carried out to obtain the hydrated calcium borate microsphere with uniform dimension. The preparation method of the anhydrous calcium borate microsphere is characterized in that the hydrated calcium borate microsphere is roasted to improve the crystallization degree in order to obtain the anhydrous calcium borate microsphere with uniform dimension. The hydrated calcium borate microsphere and the anhydrous calcium borate microsphere are hopeful to be widely applied to the fields of treatment of wastewater containing heavy metal ions or dyes, supported catalysis and flame retardation. The preparation methods have the advantages of simplicity in operation, mild conditions, low energy consumption, low cost, easy control of the process, and suitableness for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of inorganic chemical industry, in particular to hydrated calcium borate microspheres, anhydrous calcium borate microspheres and a preparation method thereof. Background technique [0002] In recent years, three-dimensional hierarchical nanomaterials have attracted much attention due to their excellent performance, unique structure, high specific surface area, and good mechanical strength, and have been widely used in energy storage, sensors, water treatment, catalyst supports, and other fields. Due to the variable composition of borates and their unique properties and potential applications in many fields, more and more attention has been paid to them. Among them, calcium borate can be widely used as a flame retardant, and can also be used in industries such as white pigments, ceramics, glass, papermaking, rubber and plastics. The cost of synthesizing calcium borate is equivalent to 1.3 times the price of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/12
CPCC01B35/126C01P2002/72C01P2004/03C01P2004/32C01P2004/61
Inventor 朱万诚陈秀平李杰翟配艳张恒张兆顺张强
Owner QUFU NORMAL UNIV
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