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Preparation method of pseudo-boehmite with high purity and high crystallization degree

A pseudo-boehmite, high crystallinity technology, applied in the preparation of alkali metal aluminate/alumina/aluminum hydroxide, alumina/aluminum hydroxide, etc., can solve the problem of amorphous pseudo-boehmite, sol Aggregation into gel, uneven particle size distribution, etc., to achieve the effect of complete crystal grains, improved purity, and high purity

Active Publication Date: 2016-05-18
SINOPEC DALIAN RES INST OF PETROLEUM & PETROCHEMICALS CO LTD +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 the sol to quickly aggregate into a gel, resulting in the formation of amorphous pseudo-boehmite. Formation, and its particle size distribution is uneven, low crystallinity, high impurity content and other shortcomings

Method used

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  • Preparation method of pseudo-boehmite with high purity and high crystallization degree
  • Preparation method of pseudo-boehmite with high purity and high crystallization degree

Examples

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Effect test

Embodiment 1

[0040] 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. Adjust the feeding speed of the two feeding pipes on the reactor, and the NaAlO with a concentration of 10g / 100ml 2 The solution has a flow rate of 20ml / min and a concentration of 30g / 100ml of Al 2 (SO 4 ) 3 The solution flows into the reactor in parallel at a flow rate of 15ml / min. 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 to keep the pressure difference △P at 0.5-2.0 Between MPa, keep the sol concentration between 5 and 15g / 100ml, and continue to react for 1.0h. After the reaction is over, start the stirring paddle, adjust the rotation speed to 1200r / min, adjust the pH value of the reactor to 9.5 and set the temperature at 15°C / min. The reaction temperature was raised to 80°C in the high-temperature section, aged for 1.0 ...

Embodiment 2

[0042] 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 two feeding pipes on the reactor, the NaAlO that concentration is 15g / 100ml 2 The solution has a flow rate of 25ml / min and a concentration of 35g / 100ml of Al 2 (SO 4 ) 3 The solution flows into the reactor in parallel at a flow rate of 20ml / min, and after forming a gel for 30 minutes, after the aluminum hydroxide sol reaches 10g / 100ml, apply a specific pressure in the pressure zones on both sides to keep the pressure difference △P at 0.5-4.0MPa In between, keep the sol concentration between 5 and 15g / 100ml, and continue the reaction for 0.5h. After the reaction is over, start the stirring paddle, adjust the rotation speed to 1000r / min, adjust the pH value of the reactor to 9.0 and react at a rate of 10°C / min. The temperature was raised to 90°C in the high temperature section, aged for 1.5 hours, filtered, washed and dried t...

Embodiment 3

[0044] 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. Adjust the feed rate of the two feeding pipes on the reactor, and the NH concentration of 10g / 100ml 4 OH solution ml / min flow rate and Al concentration of 35g / 100ml 2 (SO 4 ) 3 The solution flows into the reactor in parallel at a flow rate of 20ml / min. After forming a gel for 20 minutes, after the aluminum hydroxide sol reaches 7.4g / 100ml, apply a specific pressure in the pressure zones on both sides to keep the pressure difference △P at 0.7~ Between 2.0MPa, maintain the sol concentration between 5 ~ 15g / 100ml, continue to react for 1.0h, after the end of the reaction, start the stirring paddle, adjust the rotation speed to 1500r / min, adjust the pH value of the reactor to 9.5 and the rate of 15℃ / min Raise the reaction temperature to 75°C in the high temperature section, perform aging for 2.0 hours, filter, wash and dry to obtain p...

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Abstract

The invention discloses a preparation method of pseudo-boehmite with high purity and high crystallization degree. The method comprises the following steps: (1) bottom water is added into a pressure zone and a reaction zone of a reactor, and a stabilizing agent is added into water in the reaction zone; (2) an aqueous solution of aluminium salts and an alkaline solution are respectively injected into a feed inlet I and a feed inlet II at the upper part of the reaction zone of the reactor, a sol forming reaction is carried out, during the sol forming reaction process, when aluminium hydroxide sol reaches a certain concentration, a pressure pump pumps water in the pressure zone into a reaction zone through a semi-permeable membrane, the sol is kept in a concentration range, and the reaction is continuously carried out for a period of time; (3) after the reaction ends, a stirring paddle at the bottom of the reactor is started, pH value of the reactor is adjusted, temperature is rapidly raised to an 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 and catalysts of hydrotreatment 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 kind of " carbonic acid process (CO 2 method) to produce pseudo-boehmite, which uses the intermediate product-industrial sodium aluminate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/02C01F7/14
Inventor 薛冬吕振辉
Owner SINOPEC DALIAN RES INST OF PETROLEUM & PETROCHEMICALS CO LTD
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