TWI465526B - A means for the synthesis of ultramarine from mica powder - Google Patents

Description

Method for synthesizing ultramarine powder of mica powder

This creation belongs to the technical field of synthesizing high economic value products with natural mineral resources.

Ultramarine is a mineral pigment with stable properties, weathering resistance, alkali resistance and high temperature resistance, with lapis lazuli as the main component. The chemical formula of lapis lazuli is Na ₈ Al ₆ Si ₆ O ₂₄ (S ₂ , S ₃ ), which is a mineral of equiaxed crystal system. The crystal is rhombohedral dodecahedron with {011} incomplete cleavage plane, and the fracture is staggered. Mismatched, Mo type hardness is 5~5.5, specific gravity is 2.4-2.45, glass luster, translucent, blue-green, strong yellow light will be emitted in the flame test, which is the spectrum emitted by Na ⁺ . The crystal structure of lapis lazuli is a ^sodalite β cage composed of cations such as Si ⁴⁺ , Al ³⁺ , Na ^{+ ,} etc., containing S _x ^- (x=2-4) anion groups to maintain charge balance, and Blue and yellow chromophore. Industrial greens are synthesized by artificial means, and the quality is purer than natural ones.

The raw materials used for synthesizing ultramarine at home and abroad include kaolin, Helestone, natural zeolite, fly ash, cerium/aluminum/sodium oxide, etc., and there is no mica powder (including sericite and pyrophyllite) used in the present invention. ) as raw materials.

The invention is characterized in that the mica powder is ground and mixed with sodium carbonate (Na ₂ CO ₃ ), sulfur (S) and activated carbon (C), in an air atmosphere, before the temperature of 700 ° C to 1000 ° C, and then at 300 ° C. The temperature of 500 ° C, respectively, calcined for 1 to 16 hours, you can synthesize ultramarine, the main content is as follows: grinding mica powder below 10 μm (median diameter d ₅₀ 0.6 μm, specific surface area 50 m ² /g), mixed with sodium carbonate (Na ₂ CO ₃ ), sulfur (S), activated carbon (C), the mass ratio of the four raw materials is 1: (0.33~3): (0.5~2): ( 0.05~0.5), the mixture is heated to a temperature range of 700 ° C to 1000 ° C under an air atmosphere, and maintained at this temperature for 1 hour to 16 hours, and then cooled to a temperature range of 300 ° C to 500 ° C, and The temperature is maintained for 1 hour to 16 hours. After the reaction is completed, the solid product is washed with water and filtered, and the solid portion is further processed and ground to obtain ultramarine blue.

The first figure is a flow chart of the "method of synthesizing ultramarine in mica" of the present invention.

Annex I The invention uses an X-ray diffraction pattern of the raw material.

Annex II X-ray diffraction pattern of the product by the method of the invention.

Annex III Raman absorption spectra of the product by the method of the invention.

Annex IV According to the method of the present invention, the mica grinding sample is the starting material, the color of the product under the influence of the Na ₂ CO ₃ /S ratio and the calcination temperature.

Annex V is a graph of the crystalline region of nepheline and lapis lazuli under the influence of the Na ₂ CO ₃ /S ratio and the calcination temperature by the method of the present invention.

Annex VI Electron micrograph of the product by the method of the invention.

The method for carrying out the invention is shown in the first figure, and the mica powder is ground to below 10 μm (median particle diameter d ₅₀ 0.6 μm, specific surface area 50 m ² /g), this -10 μm solid "11", mixed with sodium carbonate (Na ₂ CO ₃ ) "12", sulfur (S) "13", activated carbon (C) "14""2" The mass ratio of the four raw materials is 1: (0.33~3): (0.5~2): (0.05~0.5), and the mixture is heated to a temperature range of 700 ° C to 1000 ° C under an atmospheric atmosphere, and at the temperature Maintaining for 1 hour to 16 hours, then cooling to a temperature range of 300 ° C to 500 ° C, and maintaining the temperature for 1 hour to 16 hours "3". After the reaction is completed, the exhaust gas "32" is recovered and the solid product "31" is washed. And filter "4", the filtrate "42" is recycled, the solid "41" is dried "5", and the polishing "6" is the ultramarine "61".

11‧‧‧mica powder (-10 μm)

12‧‧‧Sodium carbonate (Na ₂ CO ₃ )

16‧‧‧Sulphur (S)

14‧‧‧Active carbon (C)

2‧‧‧Mixed solid materials

21‧‧‧Reactive raw materials

3‧‧‧Reaction

31‧‧‧Reaction products

4‧‧‧Washing filtration

41‧‧‧ filtrate

42‧‧‧ Solid

5‧‧‧Drying

6‧‧‧ grinding

61‧‧‧Qingqing

Claims (1)

A method for synthesizing ultramarine blue with mica powder (including sericite and pyrophyllite), the method is to grind mica powder to below 10 μm (median diameter d ₅₀ 0.6μm, specific surface area 50m ² /g), mixed with sodium carbonate (Na ₂ CO ₃ ), sulfur (S), activated carbon (C), the mass ratio of the four raw materials is 1: (0.33~3): (0.5~2): (0.05 ~0.5), the mixture is heated to a temperature range of 700 ° C to 1000 ° C in an air atmosphere, and maintained at this temperature for 1 hour to 16 hours, and then cooled to a temperature range of 300 ° C to 500 ° C, and The temperature is maintained for 1 hour to 16 hours. After the reaction is completed, the solid product is washed with water and filtered, and the solid is dried and ground to be ultramarine.