Method for preparing nanospherical ferrosilicon red-coated pigment by microwave hydrothermal method

A technology of microwave hydrothermal method and encapsulation of color materials, which is applied in the field of ceramic color materials, can solve the problems of unsuitable for high efficiency and environmental protection, large product particle size, long heat preservation time, etc., achieve low synthesis temperature, simple process, and broad market prospects Effect

Active Publication Date: 2014-12-10
JINGDEZHEN CERAMIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the solid-phase method is used to prepare ferrosilicon red material, but it has defects such as high reaction temperature, long holding time, and large particle size of the obtained product, which is no longer suitable for the current industrial production requirements of energy saving, emission reduction, high efficiency and environmental protection

Method used

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  • Method for preparing nanospherical ferrosilicon red-coated pigment by microwave hydrothermal method
  • Method for preparing nanospherical ferrosilicon red-coated pigment by microwave hydrothermal method
  • Method for preparing nanospherical ferrosilicon red-coated pigment by microwave hydrothermal method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step 1: Measure 30 ml of deionized water into a beaker, add 0.29 g of ferric chloride (FeCl 3 ·6H 2 0), stirring at room temperature with a constant temperature magnetic stirrer makes it dissolve completely;

[0025] Step 2: Add 0.18g of borax to the solution in the previous step, and continue stirring for 10 min;

[0026] Step 3: Mix 5.71 g tetraethyl orthosilicate (as SiO 2 content ≥ 28.4%) was added dropwise to the solution obtained in the previous step, then NaOH solution with a concentration of 3 mol / L was added dropwise to adjust the pH to 9, the temperature of the magnetic stirrer was set to 40 °C, and the stirring was continued for 120 min;

[0027] The fourth step: transfer the obtained mixed solution to a reaction kettle with a volume of 100 ml, add deionized water dropwise, so that the total volume of the solution is 50 ml, put it into a microwave hydrothermal reaction kettle for reaction, and the reaction temperature is 180℃, holding time is 90 minutes; ...

Embodiment 2

[0030] Step 1: Measure 35 ml of deionized water into a beaker, add 0.46 g of ferric chloride (FeCl 3 ·6H 2 0), stirring at room temperature with a constant temperature magnetic stirrer makes it dissolve completely;

[0031] Step 2: Add 0.18 g of borax to the solution in the previous step, and continue stirring for 10 min;

[0032] Step 3: Mix 5.54 g tetraethyl orthosilicate (as SiO 2 content ≥ 28.4%) was added dropwise to the solution obtained in the previous step, then NaOH solution with a concentration of 3 mol / L was added dropwise to adjust the pH to 7, the temperature of the magnetic stirrer was set to 40 °C, and the stirring was continued for 120 min;

[0033] The fourth step: transfer the obtained mixed solution to a reaction kettle with a volume of 100 ml, add deionized water dropwise, so that the total volume of the solution is 50 ml, put it into a microwave hydrothermal reaction kettle for reaction, and the reaction temperature is 200℃, holding time is 90 minutes; ...

Embodiment 3

[0036] Step 1: Measure 33 ml of deionized water into a beaker, add 0.86 g of ferric chloride (FeCl 3 ·6H 2 0), stirring at room temperature with a constant temperature magnetic stirrer makes it dissolve completely;

[0037] Step 2: Add 0.18 g of borax to the solution in the previous step, and continue stirring for 10 min;

[0038] The third step: add 5.14 g tetraethyl orthosilicate (as SiO 2 content ≥ 28.4%) was added dropwise to the solution obtained in the previous step, then NaOH solution with a concentration of 3 mol / L was added dropwise to adjust the pH to 11, the temperature of the magnetic stirrer was set to 40 °C, and stirring was continued for 120 min;

[0039] The fourth step: transfer the obtained mixed solution to a reaction kettle with a volume of 100 ml, add deionized water dropwise, so that the total volume of the solution is 50 ml, put it into a microwave hydrothermal reaction kettle for reaction, and the reaction temperature is 210°C, the holding time is 90...

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Abstract

The invention discloses a method for preparing a nanospherical ferrosilicon red-coated pigment by a microwave hydrothermal method, wherein the method comprises: firstly measuring a certain amount of deionized water into a beaker, adding iron chloride, enabling the iron chloride to be completely dissolved, adding borax into the solution of the previous step, and continuously stirring for 10min; dropping ethyl orthosilicate into the previous solution, then dropping 3mol / L of NaOH solution to regulate a pH value to a needed value, setting the temperature of a magnetic stirrer to be 40 DEG C, and continuously stirring for 120min; and moving the obtained mixed solution into a microwave hydrothermal reaction vessel for reaction at 180-210 DEG C, collecting the products after reaction, washing the products with deionized water until being neutral, and drying with a drying box to prepared the ferrosilicon red-coated pigment with 30-80nm of diameters and pure color. The method has prominent advantages of low preparation temperature, simple technology, and cheap and easily available raw material, so the method has a wide market prospect.

Description

technical field [0001] The invention belongs to the technical field of ceramic pigments, and in particular relates to a method for preparing nano-spherical ferrosilicon red-coated pigments by microwave hydrothermal method. Background technique [0002] Ferrosilicon red material is a kind of ceramic color material with bright color and high temperature stability. It can show bright pink in the blank, and it can show color stably under oxidizing atmosphere at 1250°C. It is widely used in vitrified bricks, etc. It has great application value in the decoration of products. At present, the solid phase method is used to prepare ferrosilicon red material, but it has defects such as high reaction temperature, long holding time, and large particle size of the obtained product, which is no longer suitable for the current industrial production requirements of energy saving, emission reduction, high efficiency and environmental protection. Contents of the invention [0003] The techn...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B41/85
Inventor 曹春娥陈云霞卢希龙吕林琴沈华荣余峰
Owner JINGDEZHEN CERAMIC UNIV
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