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Method for synthesizing BETA molecular sieve

A synthesis method and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of low crystallinity, low crystallinity and health hazards of BETA molecular sieves, achieve green and environmental protection in the preparation process, avoid impurity crystals, and cheap and easy raw materials. the effect

Active Publication Date: 2015-02-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it has been verified by experiments that the crystallinity of the BETA molecular sieve obtained by this method is relatively low, and miscellaneous crystals are easily produced, which cannot meet the requirements of industrial production.
[0008] The existing technology reduces the synthesis cost of BETA molecular sieves by different means, especially reducing the consumption of organic templates, but the cost pressure from templates is still very high, and the use of templates still has environmental pollution problems, and operators are It can also cause great health hazards when exposed to templating agents
Although CN101249968A develops no-template agent synthesis technology, the obtained product has a low ratio of miscellaneous crystals and low crystallinity, which cannot meet industrial requirements

Method used

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  • Method for synthesizing BETA molecular sieve
  • Method for synthesizing BETA molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029]Take 40g of BETA molecular sieve and 1000mL of 1mol / L NaOH solution in a beaker, stir at room temperature for 30min, transfer to a closed reaction kettle, and treat in an oven at 120°C for 4h. The resulting suspension is the structure-directing agent and is ready for use.

[0030] Take 25.2 g of sodium hydroxide and 5.8 g of sodium aluminate in 500 mL of distilled water, and stir vigorously until they are completely dissolved. Add 70 g of white carbon black slowly and stir vigorously for 30 min. Then add 25mL of the structure directing agent prepared in the previous step and stir vigorously for 30 min. Then it was stirred in a water bath at 40°C for 5h, then put into a closed reaction kettle, and crystallized in an oven at 140°C for 30h. 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 molecular siev...

Embodiment 2

[0032] Take 30g of BETA molecular sieve and 1000mL of 0.8mol / L NaOH solution in a beaker, stir at room temperature for 30min, transfer to a closed reaction kettle, and treat in an oven at 125°C for 4h. The resulting suspension is the structure-directing agent and is ready for use.

[0033] Take 28.5 g of sodium hydroxide and 7.0 g of sodium aluminate in 550 mL of distilled water, and stir vigorously until they are completely dissolved. Add 80 g of white carbon black slowly and stir vigorously for 20 min. Then add 30mL of the structure directing agent prepared in the previous step and stir vigorously for 30 min. Then it was stirred in a water bath at 30°C for 4h, then put into a closed reaction kettle, and crystallized in an oven at 140°C for 24h. The obtained product was washed 4 times with distilled water to neutrality, and dried at 120°C for 12 hours. The sample number obtained was CL2, which was a pure BETA molecular sieve.

Embodiment 3

[0035] Take 30g of BETA molecular sieve and 1000mL of 0.8mol / L NaOH solution in a beaker, stir at room temperature for 30min, transfer to a closed reaction kettle, and treat in an oven at 125°C for 4h. The resulting suspension is the structure-directing agent and is ready for use.

[0036] Take 26.5 g of sodium hydroxide and 7.0 g of sodium aluminate in 400 mL of distilled water, and stir vigorously until they are completely dissolved. Add 100 mL of water glass slowly and stir vigorously for 40 min. Then add 35mL of the structure directing agent prepared in the previous step and stir vigorously for 30 min. Then it was stirred in a water bath at 35°C for 4h, then put into a closed reaction kettle, and crystallized in an oven at 130°C for 24h. 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 CL3, which was a pure BETA molecular sieve.

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Abstract

The invention discloses a method for synthesizing a BETA molecular sieve. The method comprises the steps of firstly processing the BETA molecular sieve with an alkaline solution to prepare a structure-directing agent, stirring inorganic alkali, aluminium sources, silicon sources and water to synthesize silicon-aluminium gel, then adding the structure-directing agent and obtaining the BETA molecular sieve after hydrothermal crystallization. The method has the advantages that the BETA molecular sieve synthesized by the method has a high degree of crystallinity and effectively avoids mixed crystals; and the method is simple and easy to operate, is cheap and available in raw materials and avoids using toxic and harmful organic template agents.

Description

technical field [0001] The invention relates to a method for synthesizing BETA molecular sieves, in particular to a green and low-cost method for synthesizing BETA molecular sieves, and belongs to the field of synthesis of molecular sieve catalytic materials. Background technique [0002] BETA molecular sieve was first synthesized by Mobil Company 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 unique three-dimensional structural characteristics were revealed, BETA molecular sieves aroused people's interest again. BETA molecular sieve has good thermal and hydrothermal stability, moderate acidity and thermal stability and hydrophobicity, and is the only large-pore high-silicon molecular sieve with crossed twelve-membered ring channel system, which shows hydrocarbon reaction in the catalytic process It is not easy to coke and has a long service life. It has e...

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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