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A kind of γ-alumina and preparation method thereof

A technology of alumina and aluminum salts, applied in the preparation of aluminum hydroxide, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as wide pore size distribution, achieve uniform microscopic supersaturation, high mixing efficiency, and improve mass transfer efficiency Effect

Active Publication Date: 2017-11-07
TSINGHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN1247773 discloses a preparation method of γ-alumina. By controlling the swing of the pH value of the precipitation reaction, pseudo-boehmite is prepared, and then γ-alumina can be obtained by roasting. However, the γ-alumina prepared by this method Aluminum also has a broad pore size distribution

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  • A kind of γ-alumina and preparation method thereof
  • A kind of γ-alumina and preparation method thereof
  • A kind of γ-alumina and preparation method thereof

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preparation example Construction

[0029] The invention provides a preparation method of γ-alumina, comprising the following steps:

[0030] (1) the aluminum salt solution is vertically dispersed into the flowing metaaluminate solution through the microporous membrane, and the precipitation reaction obtains a pseudo-boehmite suspension;

[0031] (2) aging the pseudo-boehmite suspension obtained in the step (1) to obtain a γ-alumina precursor;

[0032] (3) calcining the γ-alumina precursor obtained in the step (2) to obtain γ-alumina.

[0033] In the invention, the aluminum salt solution is vertically dispersed into the flowing metaaluminate solution through the microporous membrane, and the pseudo-boehmite suspension is obtained by precipitation reaction. The present invention does not have a special limitation on the dispersing device, and a device known to those skilled in the art that can disperse the solution on a micron-scale mixing scale can be used. The present invention preferably disperses the alumin...

Embodiment 1

[0046] 1) Prepare a sodium metaaluminate solution with a concentration of 0.6mol / L, and make it flow at a flow rate of 30mL / min.

[0047] 2) Prepare an aluminum sulfate solution with a concentration of 0.3mol / L, and make it flow at a flow rate of 10mL / min, pass through the microporous membrane and disperse into the sodium metaaluminate solution from the vertical direction.

[0048] 3) The membrane dispersion microreactor was placed in a water bath at 80°C, and the two phases reacted in the microreactor to form a pseudo-boehmite gel, and the pH at the end of the reaction was 9.

[0049] 4) Aging in a stirred tank reactor for 2 hours, then filtering, washing, drying, and roasting at 650°C to obtain γ-alumina.

[0050] The γ-alumina prepared in this example has a pore volume of 1.07mL / g and a specific surface area of ​​284.4m 2 / g, the average pore diameter is 14.0nm; the microscopic appearance is short fiber-like, the fiber length is 26.4nm, and the fiber diameter is 5.3nm.

...

Embodiment 2

[0053] 1) Prepare a sodium metaaluminate solution with a concentration of 1mol / L, and make it flow at a flow rate of 18mL / min.

[0054] 2) Prepare an aluminum sulfate solution with a concentration of 0.8mol / L, and make it flow at a flow rate of 5mL / min, pass through the microporous membrane and disperse into the sodium metaaluminate solution from the vertical direction.

[0055] 3) The membrane dispersion microreactor was placed in a water bath at 60°C, and the two phases reacted in the microreactor to form a pseudo-boehmite gel, and the pH at the end of the reaction was 8.5.

[0056] 4) Aged in a stirred tank reactor for 1 hour, then filtered, washed, dried, and calcined at 650°C to obtain γ-alumina.

[0057] The γ-alumina prepared in this example has a pore volume of 0.92mL / g and a specific surface area of ​​249.6m 2 / g, the average pore diameter is 13.5nm; the microscopic appearance is short fiber-like, the fiber length is 26.1nm, and the fiber diameter is 5.0nm.

[0058]...

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Abstract

The invention provides gamma-alumina and a preparation method thereof. The preparation method comprises the following steps: vertically dispersing an aluminum salt solution into a flowing meta-aluminate solution through a microporous membrane, and performing a precipitation reaction to obtain a pseudo-boehmite suspension; and performing aging to obtain a gamma-alumina precursor, and performing calcination to obtain the gamma-alumina. According to the invention, rapid mixing of reaction materials is achieved by using fluid cross-flow sheared microporous dispersion, the mass transfer efficiency of the system is improved, the mixing efficiency is high, and a uniform microcosmic degree of super-saturation is achieved, so that short crude fiber-shaped gamma-alumina can be obtained easily, and meanwhile, the gamma-alumina is ensured to have a relatively large pore volume and relatively narrow pore size distribution. An experimental result shows that the pore volume of the gamma-alumina provided by the invention can reach 1.25mL / g, the pore size distribution is centralized between 5nm and 30nm, and the standard deviation of the pore size distribution is as low as 0.2127.

Description

technical field [0001] The invention relates to the technical field of functional materials, in particular to a γ-alumina and a preparation method thereof. Background technique [0002] γ-Alumina is a nanomaterial obtained by calcining aluminum hydroxide at a high temperature between 550 and 800 ° C. It is also called activated alumina in industry, and its molecular formula is γ-Al. 2 O 3 , is a white powdery solid with the advantages of porosity, high specific surface area, good thermal stability, moderate surface acidity and alkalinity, and low cost, and is often used as a hydrogenation catalyst carrier. In recent years, due to the rapid growth of the market demand for hydrogenation catalysts, and residue hydrogenation is the mainstay in China, γ-alumina is required to have a larger pore volume to achieve higher catalytic activity. In addition, the study found that it is not the total pore volume but the pore size distribution that has a greater impact on the catalytic p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/34C01F7/44B82Y40/00
CPCC01F7/34C01F7/441C01P2004/04C01P2004/16C01P2006/12C01P2006/14C01P2006/17
Inventor 王玉军万艳春骆广生
Owner TSINGHUA UNIV