Bismuth oxychloride crystal and preparation method thereof

A technology of bismuth oxychloride and crystal, applied in the field of bismuth oxychloride crystal and its preparation, can solve the problems of limited application, influence on brightness, complicated preparation process, etc., and achieve the effect of ensuring speed and good brightness

Inactive Publication Date: 2014-03-26
MINJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the shape of these bismuth oxychloride crystals is irregular, which affects its own brightness and limits its application in the application field.
The patent application number is 201010301274.6, and the patent publication number is CN101935022 introduces the method of preparing BiOCl with bismuth oxide as raw material, but it needs to dissolve bismuth oxide in nitric acid solution first, and this process takes a long time, and the preparation of this solution will also affect the final product. affect the product and complicate the preparation process

Method used

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  • Bismuth oxychloride crystal and preparation method thereof
  • Bismuth oxychloride crystal and preparation method thereof

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preparation example Construction

[0030] The preparation method of a kind of bismuth oxychloride crystal disclosed by the present invention is as follows:

[0031] The growth of described bismuth oxychloride crystal is carried out by following reaction:

[0032] Bi(NO 3 ) 3 + HCl + H 2 O → BiOCl(crystal) + 3HNO 3

[0033] The mixture of described bismuth nitrate and hydrochloric acid is bismuth salt, and wherein, the ratio of bismuth nitrate and hydrochloric acid is 1: 0.8~1.2, by adjusting the consumption of described bismuth salt solution, the size of bismuth oxychloride crystal is controlled, at pH≤1 The hydrolysis reaction is carried out under acidic conditions, and the directional growth of the crystal is controlled by AEO9, thereby preparing a regular tetragonal sheet-like bismuth oxychloride crystal.

[0034] In some embodiments, the preparation method also uses NaOH solution as an adjustment solution to adjust the pH of the solution, thereby preparing the bismuth oxychloride crystals. The specifi...

Embodiment 1

[0044] Add 25 mL of concentrated hydrochloric acid to 1.2 L of deionized water, stir and heat to 65 °C, then start to add 0.38 g of surfactant AEO9 dropwise, and at the same time add bismuth salt solution (bismuth nitrate The ratio of hydrochloric acid and hydrochloric acid is 1:1.0) and NaOH solution with a concentration of 20% is added to the system. After adding for 30 minutes, increase the dropping rate to 0.2 mL / min. After dropping for 120 minutes, stop adding the bismuth salt solution dropwise, continue adding NaOH until the pH is 10, and stop heating and stirring. After cooling to room temperature, the solution was allowed to stand until the layers were separated, and then the supernatant was removed. The resulting solid was washed with deionized water to obtain BiOCl crystals. Observation by microscope shows that the obtained product presents regular tetragonal flaky crystals with a particle size of 12-14 μm.

Embodiment 2

[0046] Add 25 mL of concentrated hydrochloric acid into 1.2 L of deionized water, stir and heat to 70 °C, then start to add 0.38 g of surfactant AEO9 dropwise, and at the same time add bismuth salt solution (bismuth nitrate The ratio of hydrochloric acid and hydrochloric acid is 1:0.6) and NaOH solution with a concentration of 20% is added to the system. After adding for 30 minutes, increase the dropping rate to 0.3 mL / min. After dropping for 120 minutes, stop adding the bismuth salt solution dropwise, continue adding NaOH until the pH is 10, and stop heating and stirring. After cooling to room temperature, the solution was allowed to stand until the layers were separated, and then the supernatant was removed. The resulting solid was washed with deionized water to obtain BiOCl crystals. Observation by microscope shows that the crystal size of the obtained product is uneven, and the particle diameter is 10-16 μm.

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Abstract

The invention discloses a bismuth oxychloride crystal and a preparation method thereof, and belongs to the technical field of chemical industry. The bismuth oxychloride crystal is a lamellar crystal which is controllable in size and is in a regular square quadrilateral shape, and the size ranges from 8 micrometers to 20 micrometers. The preparation method comprises the following steps: neutralizing redundant acid in a reaction process by adopting bismuth nitrate as a raw material, providing chloride ions which form bismuth oxychloride through hydrochloric acid and adding a sodium hydroxide solution with a proper concentration to keep the proper acidity of the growth of the bismuth oxychloride crystal; carrying out hydrolysis reaction under the acidic condition that the pH is less than or equal to 1; and controlling the orientated growth of the crystal through a surface active agent to prepare the lamellar bismuth oxychloride crystal in the square quadrilateral shape. The bismuth oxychloride crystal synthesized by the method disclosed by the invention has very good brightness, metal luster and hiding power and can be widely applied to the fields of cosmetics, plastics, printing ink, automobile baking paint, and the like by being prepared into pearly slurry.

Description

【Technical field】 [0001] The invention relates to a bismuth oxychloride crystal and a preparation method thereof, belonging to the technical field of chemical industry. 【Background technique】 [0002] Pearlescent pigments are also called non-metallic pigments with metallic luster, usually referring to pigments with pearl luster and metallic luster. Due to its good chemical stability, non-toxicity, strong hiding power, high refractive index and colorful features, pearlescent pigments have been widely used in coatings, plastics, cosmetics, leather, printing, ceramics and other products. In the 1960s, the first generation of pearlescent materials - mica titanium pearlescent materials were developed abroad. However, due to the limitations of natural mica's own structure (usually with a large thickness and a wide range of thickness distribution), this will lead to poor stability of the coating, making the prepared pearlescent pigments have color difference and color is not unifo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B11/00
Inventor 王莉玮袁占辉林棋谢秉坤
Owner MINJIANG UNIV
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