Preparation method of pseudo-boehmite

A pseudo-boehmite and bottom water technology, applied in the preparation of alkali metal aluminate/alumina/hydroxide, reagents, educts, etc., can solve the problem of amorphous pseudo-boehmite and sol aggregation into gel Glue, uneven particle size distribution and other problems, to achieve the effect of complete crystal grains, improved purity, and high purity

Active Publication Date: 2017-05-17
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, pseudo-boehmite is mostly prepared by neutralization and gelation. During the preparation process, the concentration of pseudo-boehmite sol is constantly increasing, which can easily cause th...

Method used

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  • Preparation method of pseudo-boehmite
  • Preparation method of pseudo-boehmite
  • Preparation method of pseudo-boehmite

Examples

Experimental program
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Effect test

Embodiment 1

[0042] 1 L of bottom water and 8.7 g of ethylene glycol were added to the bottom of Reactor 1, and the reaction temperature was adjusted to 30°C. Regulate the feed rate of feed pipe on the reactor, the NaAlO that concentration is 10g / 100ml 2 The flow rate of the solution is 20ml / min and CO is injected at a flow rate of 2.5L / min through the semi-permeable membrane from the bottom. 2 After forming a gel for 20 minutes, after the aluminum hydroxide sol reaches 7.6g / 100ml, apply a specific pressure in the pressure zones on both sides, keep the pressure difference △P between 1.0-2.0MPa, and maintain the sol concentration at 5-15g / 100ml In between, continue to react for 1.0h. After the reaction, start ultrasonic oscillation, adjust the pH value of the reactor to 5.0 and increase the reaction temperature to 80°C in the high temperature section at a rate of 10°C / min, and perform aging for 1.0h. The aging pH value is 5.0 . After aging, pressurize the top of the reactor to pass water ...

Embodiment 2

[0045] Add 2L of bottom water and 10g of glycerol to the bottom of reactor 1, and adjust the reaction temperature to 40°C. Regulate the feeding speed of feed pipe on the reactor, the NaAlO that concentration is 15g / 100ml 2 The flow rate of the solution is 25ml / min and CO is injected at a flow rate of 3.5L / min through the semi-permeable membrane from the bottom. 2 After forming a gel for 30 minutes, after the aluminum hydroxide sol reaches 10g / 100ml, apply a specific pressure in the pressure zone on both sides, keep the pressure difference △P between 2.0-4.0MPa, and maintain the sol concentration between 5-15g / 100ml During the reaction, continue to react for 0.5h. After the reaction, start ultrasonic oscillation, adjust the pH value of the reactor to 5.5 and increase the reaction temperature to 90°C in the high temperature section at a rate of 20°C / min, and perform aging for 1.5h, and the aging pH value is 6.0. After aging, pressurize the top of the reactor to pass water throu...

Embodiment 3

[0048] 1.5L of bottom water and 8.7g of ethylene glycol were added to the bottom of reactor 1, and the reaction temperature was adjusted to 25°C. Regulate the feed rate on the reactor, and the NH concentration of 10g / 100ml 4 OH solution ml / min flow and inject CO at 4.5L / min flow through the semi-permeable membrane from the bottom 2 ,, After 20 minutes of gelling, after the aluminum hydroxide sol reaches 7.4g / 100ml, apply a specific pressure in the pressure zone on both sides, keep the pressure difference △P between 1.5-2.0MPa, and maintain the sol concentration at 5-15g Between / 100ml, continue to react for 1.0h. After the reaction is over, start the stirring paddle, adjust the rotation speed to 1500r / min, adjust the pH value of the reactor to 6.0 and raise the reaction temperature to 75°C in the high temperature section at a rate of 15°C / min. Aging for 2.0h, the aging pH value is 5.0. After aging, pressurize the top of the reactor to pass water through the semi-permeable me...

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Abstract

The invention discloses a preparation method of pseudo-boehmite. The method comprises the following steps: (1) bottom water is added into a pressure zone and a reaction zone of a reactor, a stabilizing agent is added into bottom water in the reaction zone, and gelling temperature is adjusted; (2) an aqueous solution of alkaline aluminate is added into the reactor from the upper part of the reaction zone, at the same time CO2 permeates from a semi-permeable membrane at the lower part of the reaction zone into the reaction zone, CO2 and the aqueous solution of alkaline aluminate are neutralized for carrying out a sol forming reaction, when the concentration of the aluminium hydroxide sol to be generated reaches 5-15g/100ml, a pressure pump pumps water in the pressure zone into a reaction zone through a semi-permeable membrane, the sol concentration is kept in a concentration range, and the reaction is continuously carried out for a period of time; (3) after the reaction ends, ultrasonic vibration at the bottom is started, pH value of the reactor is adjusted, temperature is rapidly raised to a aging temperature, after aging, filtering, washing and drying are carried out, the pseudo-boehmite is obtained. The pseudo-boehmite is prepared by a semi-permeable membrane penetration mode, and the obtained pseudo-boehmite has the advantages of high purity, high crystallization degree, and uniform particle size distribution; and the pseudo-boehmite is suitable for preparing carriers of hydrotreatment catalysts and catalysts for wax oil, heavy oil and other inferior raw materials.

Description

technical field [0001] The invention relates to a method for preparing pseudo-boehmite, in particular to a method for preparing pseudo-boehmite with high purity and high crystallinity. Background technique [0002] At present, industrial aluminum hydroxide is mainly prepared by industrial routes such as acid dissolution and reprecipitation with ammonia water or other alkalis. This method has complex production process, requires anti-corrosion equipment and consumes expensive chemical raw materials. In China, the cost of hydrolysis of organoaluminum compounds produced by other industrial by-products is much lower. Moreover, the pseudo-boehmite currently prepared in China has the disadvantages of high impurity content, uneven particle size distribution, low crystallinity, and unsatisfactory pore structure. [0003] CN85100161A discloses a carbonation process (CO 2 method) to produce pseudo-boehmite, which uses the intermediate product-industrial sodium aluminate solution as...

Claims

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Application Information

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IPC IPC(8): C01F7/14
CPCY02P20/141
Inventor 吕振辉彭绍忠张学辉高玉兰佟佳徐黎明
Owner CHINA PETROLEUM & CHEM CORP
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