A hydrothermal-thermal conversion method for preparing active boehmite and alumina porous microspheres from red mud

A technology of porous microspheres and boehmite, which is applied in the fields of alumina/aluminum hydroxide, alumina/hydroxide preparation, chemical instruments and methods, etc., can solve environmental pollution, does not meet the environmental friendly process green, and is cumbersome to handle. and other problems, to achieve the effect of cheap and easy-to-obtain raw materials, uniform appearance and simple operation

Active Publication Date: 2018-06-12
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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  • A hydrothermal-thermal conversion method for preparing active boehmite and alumina porous microspheres from red mud
  • A hydrothermal-thermal conversion method for preparing active boehmite and alumina porous microspheres from red mud
  • A hydrothermal-thermal conversion method for preparing active boehmite and alumina porous microspheres from red mud

Examples

Experimental program
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Effect test

Embodiment 1

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

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

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

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

[0037] (4) Centrifugal separation of the mixed material and liquid at a speed of 8000 rpm and a centrifugal time of 10 min to obtain supernatant B;

[0038] (5) Add urea to the supernatant B to make the urea concentration in the system 0.71 mol / L, mix well, stir at 300 rpm for 20 minutes to obtain a clear reaction solution;

[0039] (6) Place the reaction solution in a hydrothermal reaction kettle, hea...

Embodiment 2

[0044] A method of preparing alumina (Al 2 O 3 ) Hydrothermal-thermal conversion method of porous microspheres:

[0045] (1)~(6) Same as Example 1;

[0046] (7) The AlOOH porous microspheres prepared by the method of Example 1 were placed in a tube furnace, heated to 650°C at a heating rate of 5°C / min, and kept for 2.0 h, and then naturally cooled to room temperature to obtain multi-stage porous Al 2 O 3 Porous microspheres.

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

[0048] Al prepared in this example 2 O 3 SEM of porous microspheres such as image 3 Shown. From image 3 It can be seen that Al 2 O 3 The surface of the porous microspheres is assembled from nanosheets and has a porous structure with a pore...

Embodiment 3

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

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

[0052] (2) Centrifuge the slurry with a rotation speed of 6000 rpm and a centrifugal time of 15 min to obtain supernatant A;

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

[0054] (4) Centrifugal separation of the mixed material and liquid at a speed of 6000 rpm and a centrifugal time of 15 min to obtain supernatant B;

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

[0056] (6) Put the reaction solution in a hydrothermal reactio...

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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 inorganic chemical material preparation, 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 discharged during the extraction of alumina in the aluminum industry. Generally, for every 1 ton of alumina produced, 1.0 to 1.5 tons of red mud are incidentally produced. As the fourth largest alumina producer in the world, China emits 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 the accumulated stock of red mud will reach 500 million tons by 2020. A large amount of waste red mud is piled up, which not only takes up land, wastes resources, but also easily causes environmental pollution and safety hazards. Exploring the high value-added utilization of waste red m...

Claims

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Application Information

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Patent Type & Authority Patents(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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