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Method for preparing SrCuSi4O10 and BaCuSi4O10 blue pigments through hydrothermal technique

A blue pigment, technology of technology, applied in chemical instruments and methods, luminescent materials, alkaline earth metal silicates, etc.

Inactive Publication Date: 2014-02-26
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] So far, there is no SrCuSi that can prepare a pure phase, has an adjustable multi-level structure, has good dispersion, and is suitable for large-scale production. 4 o 10 and BaCuSi 4 o 10 The synthetic method of Chinese blue pigment

Method used

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  • Method for preparing SrCuSi4O10 and BaCuSi4O10 blue pigments through hydrothermal technique
  • Method for preparing SrCuSi4O10 and BaCuSi4O10 blue pigments through hydrothermal technique
  • Method for preparing SrCuSi4O10 and BaCuSi4O10 blue pigments through hydrothermal technique

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1: SrCuSi 4 o 10 preparation (1)

[0041] Weigh 5.7g Na 2 SiO 3 9H 2 O (20mmol) and 40mL distilled water were mixed to form solution A, and concentrated hydrochloric acid was added to adjust the pH value to 8; weigh 1.334g SrCl 2 ·6H 2 O (5mmol) and 15mL of distilled water were mixed to form solution B. After solution A and solution B are mixed, add 0.4g CuO (5mmol) powder and stir (30 minutes), then use concentrated ammonia water to adjust the pH value of the solution to 11.5, then put it into a high-pressure reactor with a volume of 80mL, so that the filling degree reaches 80 %, react at 250°C for 24 hours after sealing. After the reactor was cooled, the blue powdery product was collected.

[0042] Figure 6 It is a comparison chart of the X-ray diffraction pattern of the reaction product in this example and the fitting data of the single crystal X-ray diffraction. From Figure 6 It can be seen from the figure that the X-ray diffraction pattern of t...

Embodiment 2

[0044] Example 2: SrCuSi 4 o 10 Preparation (2)

[0045] Weigh 1.14g Na 2 SiO 3 9H 2 O (4mmol) and 10mL distilled water were mixed to make solution A, and dilute hydrochloric acid was added to adjust the pH value to 7, and 0.212g Sr(NO 3 ) 2 (1mmol) and 10mL distilled water were mixed to form solution B. 0.17g CuCl 2 2H 2 O (1mmol) was mixed with 10mL distilled water and stirred (60 minutes), then mixed with 10mL 2mol / L NaOH solution to form suspension C, solution A, solution B and suspension C were mixed. The pH of the solution was adjusted to 11 using concentrated ammonia water. Put it into a high-pressure reactor with a volume of 22.4mL to make the filling degree reach 60%, and react at 250°C for 24 hours after sealing. After the reactor was cooled, the solid phase product was collected. Rinse three times with distilled water and dry. The product is analyzed by a scanning electron microscope to be multi-layered microparticles self-assembled by microsheets. XRD ...

Embodiment 3

[0047] Example 3: SrCuSi 4 o 10 Preparation (3)

[0048] Weigh 1.14g Na 2 SiO 3 ·5H 2 O (4mmol) and 10mL distilled water were mixed to form solution A, and dilute hydrochloric acid was added to adjust the pH value to 9, and 0.2666g SrCl was weighed 2 ·6H 2 O (1mmol) and 5mL distilled water were mixed to form solution B. After solution A and solution B were mixed, 0.08 g of CuO (1 mmol) powder was added and stirred thoroughly (30 minutes), and the pH value of the solution was adjusted to 12.5 with concentrated ammonia water. Put it into a high-pressure reactor with a volume of 22.4mL to make the filling degree reach 80%, and react at 250°C for 12 hours after sealing. After the reactor was cooled, the solid phase product was collected. The product is mixed powder. It was found that the product had some unreacted CuO. After adding 0.5 mol / L HCl solution and soaking for 12 hours, the blue solid phase product was collected, rinsed with distilled water three times, and drie...

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Abstract

The invention provides a method for preparing SrCuSi4O10 and BaCuSi4O10 blue pigments through a hydrothermal technique, and belongs to the technical field of hydrothermal chemistry. The method uses copper oxide powder or copper salt, barium salt or strontium salt, and silicate as raw materials, and NH4OH as a mineralizing agent and comprises the following hydrothermal reaction processes: mixing a reactant with distilled water according to a stoichiometric ratio of an objective product, adjusting the pH value of a solution to be greater than 10 and less than 14, putting in a high-pressure reactor so as to enable the filling degree to reach 40%-90%, sealing and reacting for 5-72 hours at the temperature of 230-300 DEG C; and cooling and filtering so as to obtain products. The invention provides a new reaction route and a green preparation method for SrCuSi4O10 and BaCuSi4O10 difficult to prepare. The products are multi-level structure microparticles, have high purity, regular morphology and good dispersity and are uniform in particle size. The preparation method is simple, efficient and high in yield; waste liquid generated in a hydrothermal reaction process can be recycled.

Description

technical field [0001] The invention belongs to the technical field of hydrothermal chemistry. Particularly related to green, high-yield preparation of SrCuSi exhibiting near-infrared fluorescence properties 4 o 10 Blue Pigment and BaCuSi 4 o 10 Soft chemical synthesis method of Chinese blue pigment. Background technique [0002] Functional inorganic pigments are pigments with certain special properties composed of inorganic substances, which play an important role in the material industry and material science research. Functional inorganic pigments also have the advantages of light fastness, heat resistance, weather resistance, good solvent resistance, strong hiding power, etc., and have a wide range of applications as pigments. At the same time, because of its specific functional properties, the added value of the material is greatly increased. Such as the widely used TiO 2 , ZnO and other pigments are also used in catalysis, photovoltaic cells, semiconductors and o...

Claims

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Application Information

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IPC IPC(8): C01B33/24C09K11/59
Inventor 陈岩冯守华
Owner JILIN UNIV
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