Preparation method of high-purity boehmite

A pseudo-boehmite, high-purity technology, applied in the field of metal-organic compound synthesis, can solve the problem that the crystal phase purity of pseudo-boehmite is only 97%, the price is expensive, and the production cost of high-purity pseudo-boehmite increases, etc. problems, to achieve the effect of saving equipment investment, easy filtration, and energy consumption

Inactive Publication Date: 2011-07-13
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY +1
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  • Abstract
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  • Application Information

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Problems solved by technology

Compared with using high-purity 99.9999% aluminum wire and water to prepare high-purity pseudo-boehmite (such as CN1974390A) at high temperature and pressure, the shortcoming of this method is to use expensive high-purity aluminum wire, and the second is to carry out the process under high temperature and high pressure conditions. , leading to an increase in the production cost of high-purity pseudo-boehmite, and the crystal phase purity of pseudo-boehmite is only 97%

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0015] Put 27g of aluminum ingots, 1.33g of anhydrous aluminum trichloride and 50g of n-butanol (water content less than 0.2%) in a 1L four-necked flask with a condenser, and after reflux for 1 hour, add 260g of n-octanol and 24g of n-butanol Mix alcohol with alcohol, reflux for 1h, and filter while hot. Put the filtrate into a 2L four-neck flask with a reflux condenser and a water separator. After the temperature reaches 80°C, add 400g of deionized water at a temperature of 80°C, hydrolyze for 4 hours, separate the alcohol, and then add 500g of deionized water. Raise the temperature to 95°C, reflux and age for 14 hours, distill off the remaining alcohol and part of the water, and dry at 120°C for 6 hours to obtain 60g of white pseudo-boehmite. After XRD, differential thermal and ICP-MS analysis, it is proved that it is a high-purity pseudo-boehmite with a crystal phase purity of 100% and an impurity content of less than 0.01%. The calculated n and m values ​​are listed in Tab...

Embodiment 2

[0017] Put 27g of aluminum ingot, 1.33g of anhydrous aluminum trichloride and 50g of n-butanol (water content is less than 0.2%) in the 1L four-neck flask with condenser tube, after reflux reaction for 0.5h, add 234g of n-octanol and 24g of n-butanol Butanol mixed with alcohol, refluxed for 1h, the following operations were the same as in Example 1.

Embodiment 3

[0019] Put 27g of aluminum wire, 1.33g of anhydrous aluminum trichloride and 50g of n-butanol in a 2L four-neck flask, and after reacting for 0.5h, add 260g of n-octanol and 24g of n-butanol mixed alcohol, and reflux for 2h. The following operations are the same as in the example 1. The hydrolysis temperature is 80°C for 4 hours, the aging temperature is 100°C for 12 hours, and the drying temperature is 120°C for 6 hours.

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Abstract

The invention provides a preparation method of high-purity boehmite, belonging to the technical field of synthesis of metallic organic compounds. The preparation method comprises the following steps of: preparing alkoxyl aluminum by adopting metallic aluminum with the purity more than 99.5 percent and mixed alcohol of C5-C8 and n-butyl alcohol under the existence of aluminum choride and alkylbenzene solvents; and hydrolyzing, aging and drying the alkylbenzene to obtain the high-purity boehmite. The invention overcomes the defects that the purification is difficult when the alkoxyl aluminum is prepared with low-carbon alcohol and the reaction efficiency is low when the alkoxyl aluminum is prepared with high-carbon alcohol and can obtain the boehmite with the purity up to 99.9 percent by controlling the proportion of the mixed alcohol and the metallic aluminum and the hydrolysis condition. The method provided by the invention ensures that the preparation process of the high-purity boehmite is simplified, the preparation efficiency is high, and the preparation cost is low.

Description

technical field [0001] A method for preparing high-purity pseudo-boehmite belongs to the technical field of metal organic compound synthesis. More specifically, it relates to a high-purity pseudo-boehmite and a preparation method thereof. Background technique [0002] High-purity pseudo-boehmite is the precursor material of catalyst carrier alumina. The grain size, crystal phase purity and morphology of pseudo-boehmite have important effects on the properties of alumina such as pore volume, pore distribution, specific surface area and stability. Pseudo-boehmite mainly has three preparation methods: acid method, alkali method and aluminum alcohol method. At present, an alkaline method, that is, the carbonization method, is often used to produce pseudo-boehmite. The impurity phases such as bayerite, nodelite, and gibbsite produced during the preparation process are not easy to remove, and it is difficult to obtain pseudo-boehmite with high crystal phase purity. Boehmite. H...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/42
Inventor 辛秀兰徐培力徐培全高玉李徐宝财
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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