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A method for synthesizing aluminum-rich beta zeolite

A beta zeolite and aluminum-rich technology, which is applied in the field of molecular sieve catalytic material synthesis, can solve the problems of cumbersome synthesis steps and immature high-silicon Beta zeolite synthesis technology, and achieve high catalytic reaction efficiency, high acid density, and suppression of impurity crystals the effect produced

Active Publication Date: 2017-08-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although the prior art discloses several synthesis methods of Beta zeolite with low silicon-to-aluminum ratio, the synthesis technology of high-silicon Beta zeolite is not yet mature, and its synthesis steps are relatively cumbersome.

Method used

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  • A method for synthesizing aluminum-rich beta zeolite
  • A method for synthesizing aluminum-rich beta zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) First, put 16g of aluminum nitrate in a high-temperature furnace and bake it at 500°C for 3h.

[0031] (2) Take 0.27g of sodium hydroxide and 0.1g of sodium aluminate in 50mL of distilled water, stir until they are completely dissolved, then add 8g of white carbon black, and stir evenly.

[0032] (3) Mix the special alumina synthesized in step (1) with the silica-alumina gel synthesized in step (2), add 0.08g of Beta zeolite seed crystals, and dry in an oven at 110°C for 12 hours.

[0033] (4) Then put the dry glue obtained in step (3) into the upper part of the reactor, add 10 mL of 25% ammonia water to the bottom of the reactor, put it into a closed reaction kettle, and crystallize it in an oven at 140 ° C for 48 hours. The obtained product was washed 4 times with distilled water to neutrality, and dried at 120°C for 12 hours. The obtained sample number was CL1, and the obtained sample was as follows: figure 1 As shown, it is pure beta zeolite without other impur...

Embodiment 2

[0035] (1) First, put 10g of aluminum nitrate in a high-temperature furnace and bake it at 600°C for 2h.

[0036] (2) Take 0.27g of potassium hydroxide and 0.3g of aluminum nitrate in 50mL of distilled water, stir until they are completely dissolved, then add 8g of white carbon black, stir evenly, and then age at 8°C for 2 days.

[0037] (3) Mix the special alumina synthesized in step (1) with the silica-alumina gel synthesized in step (2), then add 0.1 g of Beta zeolite seed crystals, and dry in an oven at 120°C for 12 hours.

[0038] (4) Then put the dry glue obtained in step (3) into the upper part of the reactor, add 12 mL of 20% ammonia water to the bottom of the reactor, put it into a closed reaction kettle, and crystallize it in an oven at 140 ° C for 40 h. The obtained product was washed 4 times with distilled water until neutral, and dried at 120°C for 12 hours. The obtained sample was beta zeolite, coded as CL2.

Embodiment 3

[0040] (1) First, put 12g of aluminum nitrate in a high-temperature furnace and bake it at 700°C for 2h.

[0041] (2) Take 0.3g of sodium hydroxide and 0.35g of aluminum sulfate in 50 mL of distilled water, stir until they are completely dissolved, then add 8.5g of silica gel, and stir evenly.

[0042] (3) Mix the special alumina synthesized in step (1) with the silica-alumina gel synthesized in step (2), then add 0.13g Beta zeolite seed crystals, and dry in an oven at 130°C for 12 hours.

[0043] (4) Then put the dry glue obtained in step (3) into the upper part of the reactor, add 15 mL of 15% ammonia distilled water to the bottom of the reactor, put it into a closed reaction kettle, and crystallize it in an oven at 150 ° C for 50 h. The obtained product was washed 4 times with distilled water to neutrality, and dried at 120°C for 12 hours. The obtained sample was beta zeolite, coded as CL3.

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Abstract

The present invention discloses an aluminum-rich Beta zeolite synthesis method, which comprises: placing aluminum nitrate in a high temperature furnace, and calcining to synthesize alumina; mixing an inorganic base, an aluminum source, a silicon source and water, and stirring to obtain a silicon aluminum gel; adding the obtained alumina, and drying until the water is completely evaporated; and finally loading the dried gel into the upper portion of the reactor, adding a fixed amount of ammonia water to the bottom portion of the reactor, and carrying out crystallization synthesis to obtain the Beta zeolite. According to the present invention, the synthesized Beta zeolite is low silica-alumina ratio zeolite, and has high crystallinity, and the generation of miscellaneous crystals is effectively avoided and the operation is simple and easy to perform.

Description

technical field [0001] The invention relates to a synthesis method of Beta zeolite, in particular to a synthesis method of aluminum-rich Beta zeolite, which belongs to the field of synthesis of molecular sieve catalytic materials. Background technique [0002] Beta zeolite was synthesized for the first time by Mobil Corporation in 1967. Due to the long-term failure to solve the problem of its structure determination, it has not attracted enough attention for a long time. Until 1988, when its characteristic three-dimensional structure was revealed, Beta zeolite attracted people's interest again. Beta zeolite has good thermal and hydrothermal stability, moderate acidity and thermal stability and hydrophobicity, and is the only large-pore high-silica molecular sieve with a crossed twelve-membered ring channel system, which exhibits hydrocarbon reactions in the catalytic process It is not easy to coke and has a long service life. It has excellent catalytic performance in hydroc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02
Inventor 范峰凌凤香王少军张会成陈晓刚杨春雁
Owner CHINA PETROLEUM & CHEM CORP
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