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Hydrothermal-thermal conversion method for preparing active boehmite and alumina porous microsphere with red mud as raw material

A technology of porous microspheres and boehmite, which is applied in the fields of alumina/aluminum hydroxide, preparation of alumina/hydroxide, chemical instruments and methods, etc., can solve the problems of environmentally friendly processes such as green, cumbersome processing, and environmental pollution and other problems, to achieve the effect of uniform appearance, simple operation, and cheap and easy-to-obtain raw materials

Active Publication Date: 2017-06-13
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the currently reported synthesis of three-dimensional alumina processes, the raw materials are all analytically pure aluminates, but the waste red mud is used as the raw material, and the aluminum in it is extracted as the aluminum source to synthesize active boehmite (AlOOH) with a porous structure. ) and alumina (Al 2 o 3 ) Functional materials have not been reported publicly
In addition, the processes involved in the existing patents or literatures often require polymer surfactants, and the follow-up process is cumbersome and easy to cause environmental pollution, which does not meet the requirements of environmentally friendly processes and green

Method used

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  • Hydrothermal-thermal conversion method for preparing active boehmite and alumina porous microsphere with red mud as raw material
  • Hydrothermal-thermal conversion method for preparing active boehmite and alumina porous microsphere with red mud as raw material
  • Hydrothermal-thermal conversion method for preparing active boehmite and alumina porous microsphere with red mud as raw material

Examples

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Embodiment 1

[0033] A hydrothermal-thermal conversion method for preparing active boehmite (AlOOH) porous microspheres from red mud, the steps are:

[0034] (1) Mix red mud with 3 mol / L dilute hydrochloric acid at a solid-to-liquid ratio of 1:10 g / mL, heat to 100°C and keep it warm for 2.0 h to obtain a slurry, and cool to room temperature;

[0035] (2) Centrifuge the slurry at a speed of 8000 rpm for 10 min to obtain supernatant A;

[0036] (3) Add 2 mol / L NaOH aqueous solution dropwise to the supernatant A to adjust the pH to 13.0 to obtain a mixed material liquid;

[0037] (4) Centrifuge the mixture liquid at a speed of 8000 rpm for 10 min to obtain the supernatant B;

[0038] (5) In the supernatant B, add urea so that the urea concentration in the system is 0.71mol / L, mix well, stir at 300 rpm for 20min, and obtain a clear reaction solution;

[0039] (6) Put the reaction liquid in a hydrothermal reaction kettle, raise the temperature to 150°C at a heating rate of 5°C / min, react at a ...

Embodiment 2

[0044] A kind of red mud is used as raw material to prepare alumina (Al 2 o 3 ) Hydrothermal-thermal conversion method of porous microspheres:

[0045] (1)~(6) are with embodiment 1;

[0046] (7) Put the AlOOH porous microspheres prepared by the method in Example 1 into a tube furnace, raise the temperature to 650°C at a heating rate of 5°C / min, keep it warm for 2.0 h, and then cool naturally to room temperature to obtain a multi-level porous Al 2 o 3 porous microspheres.

[0047] The Al prepared in this embodiment 2 o 3 The XRD patterns of porous microspheres are as follows figure 1 shown. From figure 1 It can be seen in Al 2 o 3 The XRD pattern of the porous microspheres matches well with the XRD standard card number JCPDS No. 10-0425, indicating that the composition of the product is relatively pure.

[0048] The Al prepared in this embodiment 2 o 3 SEM of porous microspheres as image 3 shown. From image 3 It can be seen in Al 2 o 3 The surface of porou...

Embodiment 3

[0050] A hydrothermal-thermal conversion method for preparing active boehmite (AlOOH) porous microspheres from red mud, the steps are:

[0051] (1) Mix red mud and 4mol / L dilute nitric acid at a solid-to-liquid ratio of 1:20g / mL, heat to 90°C and keep it warm for 2.0 h to obtain a slurry, and cool to room temperature;

[0052] (2) Centrifuge the slurry at a speed of 6000 rpm for 15 min to obtain supernatant A;

[0053] (3) Add dropwise 3 mol / L NaOH aqueous solution to the supernatant A to adjust the pH to 12.9 to obtain the mixed material liquid;

[0054] (4) Centrifuge the mixture liquid at a speed of 6000 rpm for 15 min to obtain the supernatant B;

[0055] (5) Add urea to the supernatant B so that the urea concentration in the system is 1.67mol / L, mix well, stir at 400 rpm for 30 min, and obtain a clear reaction solution;

[0056] (6) Put the reaction solution in a hydrothermal reaction kettle, raise the temperature to 180°C at a heating rate of 10°C / min, react at a const...

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Abstract

The invention relates to a hydrothermal-thermal conversion method for preparing active boehmite and alumina porous microsphere with red mud as a raw material. The aluminium element extracted from red mud is used as a basic aluminium source and undergoes hydrothermal treatment at 120-210 DEG C in the presence of a proper amount of urea for 1.0-12.0 h so as to prepare AlOOH porous microspheres (diameter is 2.0-10.0 microns and pore diameter is 2-80 nm); and through medium temperature roasting, Al2O3 porous microspheres with morphology maintained greatly are obtained (diameter is 1.5-8.5 microns and pore diameter is 4-120 nm). By using aluminium in waste red mud as the raw material, the AlOOH / Al2O3 porous microsphere structure which has excellent properties and has a wide application prospect in fields of water treatment, industrial catalysis and the like is synthesized by the method. The raw materials are cheap and easily available; equipment is simple; the technological condition is mild; and the method is environment-friendly and is easy for enlarge production.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic chemical materials, and relates to a hydrothermal-thermal conversion method for preparing active boehmite and alumina porous microspheres from red mud. Background technique [0002] Red mud is the polluting waste slag discharged when the aluminum industry extracts alumina. Generally, for every ton of alumina produced, 1.0 to 1.5 tons of red mud is incidentally produced. As the fourth largest producer of alumina in the world, China discharges tens of millions of tons of waste red mud every year. At present, the comprehensive utilization rate of red mud in my country is only 5%, and it is estimated that by 2020, the accumulated stock of red mud will reach 500 million tons. A large amount of waste red mud is piled up, which not only occupies land, wastes resources, but also easily causes environmental pollution and potential safety hazards. Exploring the high value-added utilizatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/02C01F7/30
CPCC01F7/02C01F7/306C01P2002/72C01P2004/03C01P2004/32C01P2004/61C01P2006/17
Inventor 朱万诚李杰翟配艳陈秀平张恒张兆顺
Owner QUFU NORMAL UNIV
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