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A kind of method for preparing low silicon beta zeolite

A beta zeolite and silicon source technology, applied in the field of molecular sieve catalytic material synthesis, can solve the problems of cumbersome synthesis steps and immature synthesis technology of high-silicon beta zeolite, and achieve high catalytic reaction efficiency, high acid density, and inhibition of impurity crystals. produced effect

Active Publication Date: 2017-07-14
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 kind of method for preparing low silicon beta zeolite
  • A kind of method for preparing low silicon 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, 0.1g of sodium aluminate, and 30mL of 25% tetraethylammonium hydroxide in 50mL of distilled water, stir until completely dissolved, then add 8g of white carbon black, stir evenly, and then Under the condition of aging 1.5d.

[0032] (3) Mix the special alumina prepared in step (1) with the silica-alumina gel prepared in step (2), add 0.08g 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 distilled 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: f...

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, 0.3g of aluminum nitrate, and 30mL of 25% tetraethylammonium hydroxide in 50mL of distilled water, stir until completely dissolved, then add 8g of white carbon black, stir evenly, and then Under aging 2d.

[0037] (3) Mix the special alumina prepared in step (1) with the silica-alumina gel prepared in step (2), 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 distilled 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 hours. 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, 0.35g of aluminum sulfate, and 30mL of 25% tetraethylammonium hydroxide in 50 mL of distilled water, stir until completely dissolved, then add 8.5g of silica gel, stir evenly, and then Under aging 1.5d.

[0042] (3) Mix the special alumina prepared in step (1) with the silica-alumina gel prepared in step (2), then add 0.13 g of 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 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 50h. 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 invention discloses a method for preparing low-silicon Beta zeolite. In the synthesis method, firstly, aluminum nitrate is placed in a high-temperature furnace, and then calcined to prepare alumina; Stir to form a silica-alumina gel; then add the alumina obtained above, and dry until the water evaporates completely; finally, put the dry gel into the upper part of the reactor, add a certain amount of water to the bottom of the reactor, and crystallize to synthesize Beta zeolite. The Beta zeolite synthesized by the method of the invention is a zeolite with a low silicon-aluminum ratio and high crystallinity, which not only effectively avoids the generation of miscellaneous crystals but also is simple and easy to operate.

Description

technical field [0001] The invention relates to a synthesis method of Beta zeolite, in particular to a synthesis method of Beta zeolite with a low silicon-aluminum ratio, and 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 per...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 范峰凌凤香王少军张会成陈晓刚杨春雁
Owner CHINA PETROLEUM & CHEM CORP