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Calcium borate whisker and preparation method thereof

A calcium borate and whisker technology, which is applied in the field of calcium borate whiskers and its preparation, can solve the problems of high cost, random shape, complicated operation, etc., and achieve the effects of significant impact, significant reaction temperature, and low production cost

Active Publication Date: 2020-09-11
CHENGDU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The calcium borate whiskers obtained by this method are fan-shaped or rod-shaped. The shape is random, and the precursor needs to be prepared in advance. The operation is complicated and the cost is high. The thermal stability of the obtained calcium borate whiskers needs to be further improved.

Method used

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  • Calcium borate whisker and preparation method thereof
  • Calcium borate whisker and preparation method thereof
  • Calcium borate whisker and preparation method thereof

Examples

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preparation example Construction

[0033] The preparation method of calcium borate whisker of the present invention, comprises the steps:

[0034] a. Ball milling: Boron source, calcium source and co-solvent are mixed, ball milled for 1-10 minutes, and the ball-milled material is obtained;

[0035] b. Calcination: The ball-milled material is calcined at 800-1000°C for 2-6 hours to obtain the calcined product;

[0036] c. Impregnation: After calcination, the product is cooled, added with water at 70-90°C for impregnation, and then the solid is washed and dried to obtain calcium borate whiskers.

[0037] Through the method of the invention, calcium borate whiskers can be successfully prepared, the operation is simple and the cost is low, and the obtained whiskers have high crystallinity, good thermal stability, high purity and uniform appearance.

[0038] Step a is a ball milling step, in which the boron source, calcium source and co-solvent are mixed and then ball milled. Wherein, the ball milling can adopt co...

Embodiment 1

[0051] A method for preparing calcium borate whiskers, comprising the steps of:

[0052] (1) Ingredients: weigh 1.0153g CaCl 2 , weighed 2.9937g Na 2 B 4 o 7 10H 2 O, take by weighing 5.4301g KCl, mix homogeneously, promptly boron-calcium mol ratio is 3.4:1, and the mol ratio of boron-calcium and potassium chloride is 1:1.8.

[0053] (2) Grinding: transfer the uniformly mixed materials into a vibrating ball mill jar, grind for 2 minutes, and transfer all the powders into a ceramic crucible.

[0054] (3) Calcination: Cover the crucible and place it in a muffle furnace for calcination at 900°C for 4 hours, then cool with the furnace.

[0055] (4) Impregnation: The calcined sample is impregnated at 80°C to remove residual NaCl, KCl and B 2 o 3 .

[0056] (5) Washing: the impregnated sample is washed, filtered, and dried at 105° C. to obtain the calcium borate whisker product with a yield of about 94.8%.

[0057] Gained calcium borate whiskers were characterized, the resu...

Embodiment 2

[0060] A method for preparing calcium borate whiskers, comprising the steps of:

[0061] (1) Ingredients: weigh 1.6794g CaO, weigh 11.4217g Na 2 B 4 o 7 10H 2 O, weigh 11.1632g KCl and mix evenly, that is, the molar ratio of boron to calcium is 4:1, and the molar ratio of boron to calcium to potassium chloride is 1:1.

[0062] (2) Grinding: transfer the uniformly mixed materials into a vibrating ball mill jar, grind for 5 minutes, and transfer all the powders into a ceramic crucible.

[0063] (3) Calcination: Cover the crucible and put it into a muffle furnace for calcination at 950°C for 2 hours, then cool with the furnace.

[0064] (4) Impregnation: The calcined sample is impregnated at 80°C to remove residual NaCl, KCl and B 2 o 3 .

[0065] (5) Washing: the impregnated sample is washed, filtered, and dried at 105°C to obtain calcium borate whiskers with a yield of about 93.1%.

[0066] The SEM spectrum of the calcium borate whiskers is detailed in figure 1 b. Its ...

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Abstract

The invention relates to a calcium borate whisker and a preparation method thereof, and belongs to the technical field of inorganic non-metallic materials. The technical problem to be solved by the invention is to provide the preparation method of the calcium borate whisker, which is simple to operate. The method comprises the following steps of: a, ball-milling: mixing a boron source, a calcium source and a cosolvent, and ball-milling for 1-10 minutes to obtain a ball-milled material; b, calcining: calcining the ball-milled material at 800-1000 DEG C for 2-6 hours to obtain a calcined product; and c, dipping: cooling the calcined product, adding water for dipping at 70-90 DEG C, and then washing the solid and drying to obtain the calcium borate whisker. The calcium borate whiskers are prepared by adopting a new method which has not been reported at home and abroad; the raw materials are easily available, the reaction does not involve high pressure, the preparation cost is low, the safety is high, the operation is simple, the process is easy to control, and the obtained calcium borate whisker has the advantages of good crystallinity, good thermal stability, uniform morphology, highpurity and high yield, and can be applied to the industries of alkali-free glass fibers, flame retardancy, ceramics, reinforcing materials and the like.

Description

technical field [0001] The invention relates to a calcium borate whisker and a preparation method thereof, belonging to the technical field of inorganic non-metallic materials. Background technique [0002] Whiskers refer to a short rod-like fiber-like structure grown in the form of a single crystal under certain reaction conditions, usually with an aspect ratio greater than 10 and a single crystal cross-sectional area less than 5×10 -4 cm -2 . Due to its extremely small diameter, which can usually reach the submicron or nanometer level, it is difficult to have various defects that are common in general crystals. The atoms are arranged uniformly and orderly, and there is a strong bond between each atom. Therefore, Has high mechanical strength. Whiskers are widely used, especially for their excellent potential in strengthening various composite materials. Therefore, all countries in the world attach great importance to the development and utilization of whiskers. [0003]...

Claims

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Application Information

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IPC IPC(8): C30B1/10C30B29/22C30B29/62C01B35/12
CPCC01B35/126C01P2002/72C01P2002/82C01P2004/03C30B1/10C30B29/22C30B29/62
Inventor 曾英黄勇冯珊于旭东彭芸左文章徐攀童翰林
Owner CHENGDU UNIVERSITY OF TECHNOLOGY
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