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Process for preparing spherical nanometer spinel zaffre by hydrothermal method

A nano-spinel and spinel-type technology is applied in the field of preparing spherical nano-spinel-type cobalt blue materials by a hydrothermal method, which can solve the problems of limited use range, complex synthesis process, high price, etc. Single, simple process, no pollution to the environment

Inactive Publication Date: 2013-07-10
JINGDEZHEN CERAMIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High-performance spherical nano-cobalt blue material still needs to be imported, but due to its complex synthesis process and high energy consumption, it is expensive, which limits its application range

Method used

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  • Process for preparing spherical nanometer spinel zaffre by hydrothermal method
  • Process for preparing spherical nanometer spinel zaffre by hydrothermal method
  • Process for preparing spherical nanometer spinel zaffre by hydrothermal method

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) With cobalt chloride and aluminum chloride as raw materials, 0.15mol Co 2+ , 0.3mol Al 3+ Weigh it into a beaker, add deionized water, and then put the beaker on a magnetic stirrer and stir evenly;

[0033] (2) Slowly drop 3 mol / L NaOH solution into the uniformly stirred mixed solution, and continue stirring at a constant temperature of 20°C for 30 minutes until the pH of the solution is 13;

[0034] (3) Take a small amount of the supernatant of the above solution and add dropwise a few drops of 3mol / L NaOH solution to observe whether there is precipitation or not. If there is no precipitation, the reaction is complete;

[0035] (4) In the above-mentioned fully reacted solution, add a triethanolamine liquid with a volume fraction of 4% and a glycerol liquid with a volume fraction of 2%, and continue stirring for 30 minutes;

[0036] (5) Put the above-mentioned uniformly stirred mixed solution into a 100mL reactor with a filling degree of 70%, and incubate it under...

Embodiment 2

[0039] (1) With cobalt chloride and aluminum chloride as raw materials, 0.12mol Co 2+ , 0.24mol Al 3+ Add to the beaker, add deionized water, then put the beaker on a magnetic stirrer and stir evenly;

[0040] (2) Slowly drop 3 mol / L NaOH solution into the uniformly stirred mixed solution, and continue stirring at a constant temperature of 20°C for 30 minutes until the pH of the solution is 13;

[0041] (3) Take a small amount of the supernatant of the above solution and add dropwise a few drops of 3mol / L NaOH solution to observe whether precipitation is generated, if there is no precipitation, the reaction is complete;

[0042] (4) In the above-mentioned fully reacted solution, add a triethanolamine liquid with a volume fraction of 8% and a glycerol liquid with a volume fraction of 4%, and continue stirring for 30 min;

[0043] (5) Put the above-mentioned uniformly stirred mixed solution into a 100mL reactor at a filling degree of 70%, and incubate it under hydrothermal hea...

Embodiment 3

[0046] (1) With cobalt chloride and aluminum chloride as raw materials, 0.18mol Co 2+ , 0.36mol Al 3+ Add to the beaker, add deionized water, then put the beaker on a magnetic stirrer and stir evenly;

[0047] (2) Slowly drop 3 mol / L NaOH solution into the uniformly stirred mixed solution, and continue stirring at a constant temperature of 20°C for 30 minutes until the pH of the solution is 13;

[0048] (3) Take a small amount of the supernatant of the above solution and add dropwise a few drops of 3mol / L NaOH solution to observe whether there is precipitation or not. If there is no precipitation, the reaction is complete;

[0049] (4) In the above-mentioned fully reacted solution, add a triethanolamine liquid with a volume fraction of 12% and a glycerol liquid with a volume fraction of 6%, and continue stirring for 30 min;

[0050] (5) Put the above-mentioned uniformly stirred mixed solution into a 100mL reactor with a filling degree of 70%, and incubate it with hydrotherma...

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Abstract

The invention discloses a process for preparing spherical nanometer spinel zaffre by the hydrothermal method. The process comprises the following steps: weighing and putting cobalt chloride and aluminum chloride according to a mol ratio of Co<2+> : Al <3+> = 1:2, putting the materials into a beaker, adding a proper amount of deionized water and carrying out uniform stirring on a magnetic stirrer;adding a sodium hydroxide solution drop by drop until the pH value of the mixture in the beaker is 13 and continuing stirring; adding mixed liquor of triethanolamine and glycerol with a volume fraction of 6 to 18% and resuming stirring; carrying out hydrothermal cultivation on the mixed solution at a temperature of 245 DEG C for 20 to 40 hours and taking the mixed solution out for natural coolingat room temperature; repeatedly rinsing the hydrothermal cultivation resultant material in liquid phase until the pH value equals 7 and putting the resultant material into a baking oven for drying attemperature of 60 DEG C so as to obtain spherical products with particle size less than 100 nm. The advantages of the invention are as follows: liquid phase hydrothermal cultivation is employed and composite organic matters are added; therefore, nanometer spherical powder is formed directly without calcining, energy consumption is relatively low, and no environmental pollution is generated.

Description

technical field [0001] The invention belongs to the field of inorganic non-metallic materials (ceramics), and in particular relates to a method for preparing spherical nano-spinel-type cobalt blue material by a hydrothermal method. Background technique [0002] Blue is one of the three primary colors of red, green and blue, and many colors are indispensable. In the decoration of ceramics, cobalt blue is an important spinel-type colored inorganic pigment, which is a composite oxide with a spinel structure. In a broad sense, the spinel-type composite oxide is the sum of the positive oxidation values ​​of the cations in its simplest formula is +8, while the negative oxidation value -8 is provided by four -2 oxygens. A class of composite oxides. For example, cobalt blue with the simplest chemical formula can be expressed by the following formula: CoAl 2 o 4 , also known as cobalt aluminate blue. [0003] Compared with other blue pigments, spinel-type cobalt blue pigment has...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B41/85
Inventor 曹春娥胡琪陈云霞卢希龙余峰沈华荣洪琛
Owner JINGDEZHEN CERAMIC UNIV
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