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A kind of preparation method of novel fluorinated bismuth oxychloride

A technology of fluorinated bismuth oxychloride and bismuth oxychloride, which is applied in chemical instruments and methods, single crystal growth, polycrystalline material growth and other directions, can solve the problems of affecting brightness, high price, limited application fields, etc., and achieves improved coverage. The effect of strength, easy operation and strong weather resistance

Active Publication Date: 2017-01-18
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the bismuth oxychloride crystals obtained by such inventions and preparations are all irregular crystal shapes, which affect their own brightness, and are more expensive, which limits their application fields.

Method used

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  • A kind of preparation method of novel fluorinated bismuth oxychloride
  • A kind of preparation method of novel fluorinated bismuth oxychloride
  • A kind of preparation method of novel fluorinated bismuth oxychloride

Examples

Experimental program
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Effect test

Embodiment 1

[0035]a. Add 90 mL of 37.5 wt% concentrated hydrochloric acid and 4.2 g of octadecyltrimethylammonium chloride surfactant to 12 L of deionized water, mechanically stir at 600 rpm, and control the temperature of the reaction system within the range of 70 °C;

[0036] b. The ratio between bismuth chloride, bismuth nitrate and bismuth fluoride with a concentration of 0.7 moL / L is 0.4 : 0.5 : 0.1 and the concentration is 20 wt% sodium hydroxide solution respectively at a speed of 3.0 mL / min and a speed of 2.5mL / min were added to the reaction system at the same time;

[0037] c. After adding for 30 min, the ratio of 0.4: 0.5: 0.1 between bismuth chloride, bismuth nitrate and bismuth fluoride with a concentration of 0.7 moL / L was increased to 4.5 mL / min, Control the addition rate of 20 wt% sodium hydroxide solution to be 4.0 mL / min to maintain the pH value of the solution;

[0038] d. After adding the bismuth salt solution, quickly add 20 wt% sodium hydroxide solution to make t...

Embodiment 2

[0040] a. Add 200 mL of 37 wt% concentrated hydrochloric acid and 4.8 g of octadecyl dimethyl amine oxide surfactant to 12 L of deionized water, mechanically stir at 300 rpm, and control the temperature of the reaction system within the range of 80 °C;

[0041] b. The ratio between bismuth chloride, bismuth nitrate and bismuth fluoride with a concentration of 0.8 moL / L is 0.3 : 0.5 : 0.2 and the concentration is 20 wt% sodium hydroxide solution respectively at a speed of 3.0 mL / min and a speed of 2.5mL / min were added to the reaction system at the same time;

[0042] c. After adding for 30 min, the ratio of bismuth chloride, bismuth nitrate and bismuth fluoride with a concentration of 0.8 moL / L is 0.3: 0.5: 0.2. Control the addition rate of 20 wt% sodium hydroxide solution to be 4.0 mL / min to maintain the pH value of the solution;

[0043] d. After the bismuth salt solution is added, quickly add sodium hydroxide to make the pH value of the solution 10, remove the supernata...

Embodiment 3

[0045] a. Add 150 mL of 36 wt% concentrated hydrochloric acid and 6.0 g of tetradecyl dimethyl amine oxide surfactant to 12 L of deionized water, mechanically stir at 400 rpm, and control the temperature of the reaction system within the range of 75 °C;

[0046] b. The ratio between the bismuth chloride, bismuth nitrate and bismuth fluoride with a concentration of 0.8 moL / L is 0.1 : 0.5 : 0.4, and the concentration is 20 wt% sodium hydroxide solution respectively at a speed of 3.0 mL / min and a speed of 2.5mL / min were added to the reaction system at the same time;

[0047] c. After adding 30 min, the ratio between bismuth chloride, bismuth nitrate and bismuth fluoride of 0.8 mol / L is 0.1:0.5:0.4. The adding rate of wt% sodium hydroxide solution is 4.9 mL / min to keep the pH value of the solution;

[0048] d. After the bismuth salt solution has been added, quickly add sodium hydroxide to make the pH of the solution 10, remove the supernatant after standing for stratification...

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Abstract

The invention provides a novel preparation method of fluoro-bismuth oxychloride. The method comprises the following steps: adding a saline solution containing fluorine, chlorine and bismuth as well as a sodium hydroxide solution into a reaction system consisting of concentrated hydrochloric acid and a surfactant; after the saline solution containing the fluorine, the chlorine and the bismuth is added into the reaction system, rapidly adding the sodium hydroxide solution in order that the pH value of the solution of the reaction system is 10; standing the solution for delaminating, and removing a supernatant; and washing an obtained solid through deionized water to obtain a fluoro-bismuth oxychloride sheet crystal. The fluoro-bismuth oxychloride sheet crytal has regular squares and regular octagons which are arranged orderly, and has excellent chemical stability as well as superior weather resistance and temperature resistance; and the effects of shielding force, brightness and the like of the crystal are improved effectively, and a fluoro-substitution proportion can be controlled according to different demands. The fluoro-bismuth oxychloride sheet crystal is low in the preparation cost and has high pearl performance, and the preparation method is easy and convenient to operate.

Description

technical field [0001] The invention relates to a fluorobismuth oxychloride flake crystal and a preparation method thereof, in particular to a fluorobismuth oxychloride crystal with weather resistance, temperature resistance and good pearlescent performance and its preparation. Background technique [0002] Pearlescent pigment is a kind of effect pigment, which is named for its unique luster and charming brilliance. It has been loved by people for a long time and is very popular. Although natural pearl has a good pearlescent effect and has no toxins, as a natural substance, its resources are limited, its price is expensive, and its preparation process is complicated, resulting in limited application range; early artificially synthesized pearlescent pigments such as: 2, 30 High mercury chloride crystals and different types of arsenic and lead crystals prepared in the 1940s, lead thiosulfate platelets and lead phosphate platelets appeared in the 1940s, and basic lead carbonate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/64C30B29/16C30B7/14
Inventor 黄宝铨周为明钱庆荣柯梅珍陈庆华肖荔人刘欣萍许兢薛珲罗永晋
Owner FUJIAN NORMAL UNIV
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