Preparation method of aluminum oxide carrier

An alumina carrier, ionic liquid technology, applied in catalyst carriers, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of amorphous pseudo-boehmite, sol aggregation into gel, uneven particle size distribution, etc. , to achieve the effect of large pore size and pore volume, improving comprehensive performance and high specific surface area

Active Publication Date: 2017-05-17
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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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 aluminum oxide carrier
  • Preparation method of aluminum oxide carrier
  • Preparation method of aluminum oxide carrier

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preparation example Construction

[0040] The preparation method of alumina carrier of the present invention comprises the following steps:

[0041] (a) The concentration and preparation method of the working solution are well known to those skilled in the art. For example, the concentration of an acidic aluminum salt solution is Al 2 o 3 It is calculated as 3g / 100mL~15g / 100mL; the concentration of alkali metal aluminum salt solution is expressed as Al 2 o 3 Calculated as 8g / 100mL~35g / 100mL, the alkali metal aluminum salt aqueous solution is selected from NaAlO 2 , KAlO 2 One or more in aqueous solution, preferably NaAlO 2 aqueous solution;

[0042] (b) by M 1 respectively and M 2 , M 3 Made into ionic liquids I and II;

[0043] (c) Add bottom water and a certain amount of ionic liquid I to the bottom of reactor 1, and heat to 25-45°C;

[0044] (d) Adjust the feeding speed of the feeding pipe on the reactor, and flow a certain concentration of alkaline metal salt solution into the reactor at a flow r...

Embodiment 1

[0052] 400g of triethylammonium chloride, 220g of sodium hexafluorophosphate, and 450g of pure water were mixed, heated to 90°C under stirring, kept at a constant temperature for 3 hours, clarified, naturally cooled to about 30°C, and centrifuged to filter out the solid to obtain 450g of ionic liquid I. The water content is about 3.5wt%, and the yield is 72wt%.

[0053] Trimethylphenylammonium chloride 500g, sodium hexafluorophosphate 260g, pure water 450g, mix, heat to 90°C under stirring, keep the temperature for 3 hours, clarify, naturally cool to about 30°C, centrifuge and filter out the solid to obtain the ionic liquid II 550g, water content about 3.5wt%, yield 74wt%.

[0054] 1L of bottom water and 40g of ionic liquid I 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 f...

Embodiment 2

[0057] Triethylammonium chloride 300g, sodium hexafluorophosphate 160g, pure water 350g, mixed, heated to 100°C under stirring, kept at constant temperature for 2.5h, clarified, naturally cooled to about 30°C, centrifuged to filter out the solid to obtain 420g of ionic liquid I , the water content is about 3.7wt%, and the yield is 72wt%.

[0058] Dimethylphenylammonium chloride 600g, sodium tetrafluoroborate 300g, pure water 550g, mix, heat to 70°C under stirring, keep the temperature for 3 hours, clarify, naturally cool to about 30°C, centrifuge and filter out the solid to obtain the ionic liquid II 550g, water content about 4.0wt%, yield 74wt%.

[0059] Add 2L of bottom water and 35g of ionic liquid I 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 sem...

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Abstract

The invention discloses a preparation method of an aluminum oxide carrier. The method comprises the following steps: (1) bottom water is added into a pressure zone and a reaction zone of a reactor, ionic liquid I is added, and gelling temperature is adjusted; (2) an aqueous solution of alkaline aluminate is added into the reactor, at the same time CO2 enters the reaction zone from the lower part of the reaction zone, CO2 and the aqueous solution of alkaline aluminate are neutralized for carrying out a sol forming reaction, when water in the pressure zone enters the reaction zone through a semi-permeable membrane, the sol concentration is kept in a concentration range, and the reaction is continuously carried out; (3) after the reaction ends, ultrasonic vibration at the bottom is started, and after aging, washing and drying are carried out, pseudo-boehmite is obtained. (4) mixing and kneading, moulding, drying and calcination of the pseudo-boehmite prepared in the step (3), an adhesive and ionic liquid II are carried out, and the aluminum oxide carrier is obtained. The aluminum oxide carrier has the advantages of high specific surface area, large aperture and pore volume, high lateral compressive strength, and low abrasion; and the product is adapted to be the carrier of boiling bed wax oil, residual oil hydrogenation catalysts.

Description

technical field [0001] The invention relates to a method for preparing an alumina carrier, in particular to a method for preparing an alumina carrier with a large pore size and a double pore distribution. 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 a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J32/00B01J21/04B01J35/10B01J19/10B01J19/00
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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