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Sandwich type solvent thermal synthesis method of boehmite powder

A solvothermal synthesis method, the technology of boehmite powder, applied in the direction of alumina/aluminum hydroxide, etc., can solve the problems of inability to completely isolate water, difficult to achieve separation and purification, etc., to achieve simple recovery, regular powder morphology, Eliminates the effect of hard agglomerations

Active Publication Date: 2015-07-01
TAISHAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the traditional solvothermal method, the solvent after the reaction is mixed and mixed with water-soluble products. Even after recovery, it is difficult to separate and purify
In addition, the traditional solvothermal method only partially replaces water with non-aqueous solvents, and there is still water in the mixed solvent. Although the existence of these waters is helpful for the dissolution of aluminum salts, the water cannot be completely isolated during the growth of the powder. , the powder still has the opportunity to come into contact with water molecules, and the agglomeration phenomenon can only be alleviated, but it cannot be eliminated more completely

Method used

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  • Sandwich type solvent thermal synthesis method of boehmite powder
  • Sandwich type solvent thermal synthesis method of boehmite powder
  • Sandwich type solvent thermal synthesis method of boehmite powder

Examples

Experimental program
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Effect test

Embodiment 1

[0028] First, pure AlCl will be analyzed 3 9H 2 O was added to deionized water and stirred on a magnetic stirrer to dissolve it to obtain Al3+ Concentration is the transparent solution A of 0.2mol / L; Secondly, add a certain amount of analytically pure urea as precipitating agent, the addition amount of urea is to precipitate all Al 3+ 125% of the required theoretical demand, continue to stir for half an hour to obtain a transparent solution B; then, add 15ml of phthalic acid di Methyl ester constitutes the bottom layer, slowly add 10ml of solution B along the inner wall of the liner to the upper part of the dimethyl phthalate layer as the water layer; then, carefully add 15ml of n-hexanol along the inner wall of the liner, slowly Add to the upper part of the water layer as the top layer, the total filling degree is controlled at 80%, seal the hydrothermal reaction kettle, put it into an electric heating constant temperature blast drying oven, control the solvent heat temperat...

Embodiment 2

[0031] First, pure AlCl will be analyzed 3 9H 2 O was added to deionized water and stirred on a magnetic stirrer to dissolve it to obtain Al 3+ Concentration is the transparent solution A of 0.4mol / L; Secondly, add a certain amount of analytically pure urea as precipitating agent, the addition amount of urea is to precipitate all Al 3+ 150% of the required theoretical demand, continue to stir for half an hour to obtain a transparent solution B; then, add 15ml of phthalic acid di Butyl ester constitutes the bottom layer. Slowly add 10ml of solution B along the inner wall of the inner container to the upper part of the dibutyl phthalate layer as the water layer; then, carefully add 10ml of n-amyl alcohol along the inner wall of the inner container, Slowly add to the upper part of the water layer as the top layer, the total filling degree is controlled at 70%, seal the hydrothermal reaction kettle, put it into an electric heating constant temperature blast drying oven, control ...

Embodiment 3

[0034] First, pure Al(NO 3 ) 3 9H 2 O was added to deionized water and stirred on a magnetic stirrer to dissolve it to obtain Al 3+ A transparent solution A with a concentration of 0.1mol / L; secondly, add a certain amount of analytically pure urea as a precipitant, and the amount of urea added is to precipitate all Al 3+ 125% of the required theoretical demand, continue to stir for half an hour to obtain a transparent solution B; then, add 15ml of phthalic acid di Methyl ester constitutes the bottom layer, slowly add 10ml of solution B along the inner wall of the liner to the upper part of the dimethyl phthalate layer as the water layer; then, carefully add 11ml of n-hexanol along the inner wall of the liner, slowly Add to the upper part of the water layer as the top layer, the total filling degree is controlled at 72%, seal the hydrothermal reaction kettle, put it into an electric heating constant temperature blast drying oven, control the solvent heat temperature at 160 °...

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Abstract

The invention relates to a sandwich type solvent thermal synthesis method of boehmite powder. The method includes the steps of: dissolving an analytically pure aluminum salt to prepare a transparent solution A with an Al<3+> concentration of 0.1-0.4mol / L, adding a certain amount of a precipitation agent, conducting stirring for half an hour to obtain a transparent solution B, adding a certain amount of phthalate ester into a hydrothermal reaction kettle liner made of polytetrafluoroethylene to form a bottom layer, adding a certain amount of solution B to the upper part of the phthalate ester layer slowly and carefully along the inner wall of the liner to serve as a water layer; adding a certain amount of non-water soluble alcohol to the upper part of the water layer slowly and carefully along the inner wall of the liner so as to form a three-layer sandwich type solvent thermal synthesis system; controlling the solvent thermal temperature at 150-200DEG C, letting the reaction last 12-24h, at the end of the reaction, carrying out natural cooling to room temperature, and finally, opening the hydrothermal reaction kettle, firstly taking out the upper layer alcohol, then employing pumping filtration separation to separate the precipitate from the bottom liquid part, washing the filter cake, then putting it in a vacuum drying box at 80-100DEG C and drying it for 4-8h, thus obtaining the boehmite powder.

Description

technical field [0001] The invention relates to a method for preparing boehmite superfine powder, in particular to a method for preparing boehmite powder with different shapes by a sandwich type solvothermal method with recyclable solvent. Background technique [0002] Boehmite (boehmite), also known as boehmite, appears as a white powder with a molecular formula of γ-AlOOH. Boehmite itself can be used as a flame retardant, and its most important use is to prepare alumina powder after calcination, so it is called the precursor of alumina. The macroscopic properties of inorganic powder materials represented by boehmite and alumina not only depend on their chemical composition, but also are largely affected by their particle size and shape. Therefore, the preparation of boehmite with different shapes Stone powder has always been a research hotspot in the field of inorganic material synthesis. [0003] In the process of preparing boehmite powder by hydrothermal method with wa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/02
Inventor 吴秀勇
Owner TAISHAN MEDICAL UNIV