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Synthetic method of ZSM-5/mordenite composite molecular sieve

A technology of ZSM-5 and composite molecular sieves, which is applied in the direction of mercerized crystalline aluminum silicate zeolite, molecular sieve catalysts, chemical instruments and methods, etc., can solve problems such as environmental pollution, high proportion, and health hazards, and achieve green and environmental protection in the preparation process. The effect of reducing production cost and simple and easy operation

Active Publication Date: 2013-01-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is well known that organic templates account for the highest proportion in the preparation cost of zeolite molecular sieves. The use of templates also increases the operation steps of removing templates from composite molecular sieves, which not only increases costs, but also pollutes the environment.
And operators will cause great harm to their health when they come into contact with organic templates. For these reasons, many zeolite molecular sieve materials with excellent performance cannot be applied on a large scale in industry

Method used

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  • Synthetic method of ZSM-5/mordenite composite molecular sieve
  • Synthetic method of ZSM-5/mordenite composite molecular sieve
  • Synthetic method of ZSM-5/mordenite composite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Take 40g of mordenite 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.

[0043] Take 14 g of sodium hydroxide and 10 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 20 mL of the structure-directing agent prepared in the previous step, and stir vigorously for 20 min; then add 30 g ZSM-5 molecular sieve and 8 g NaCl, stir vigorously for 30 min, put it into a closed reactor, and crystallize at 170 °C for 28 h. The obtained product was washed 4 times with distilled water until neutral, and dried at 120°C for 4 hours. The obtained sample was a core-shell structure ZSM-5 / mordenite composite molecular sieve, and the sample number was CL1.

[0044] Fr...

Embodiment 2

[0047] Take 45g of mordenite and 900mL of 1.8mol / L NaOH solution in a beaker, stir at room temperature for 250min, transfer to a closed reaction kettle, and treat in an oven at 140°C for 4h. The resulting suspension is the structure-directing agent and is ready for use.

[0048] Take 22 g of sodium hydroxide and 12 g of aluminum sulfate in 200 mL of distilled water, and stir vigorously until they are completely dissolved. Slowly add 100 mL of water glass and stir vigorously for 30 min. Then add 40mL of the structure-directing agent prepared in the previous step, and stir vigorously for 30 min; then add 25 g ZSM-5 molecular sieve and 10 g NaCl, stir vigorously for 30 min, put it into a closed reactor, and crystallize at 180°C for 30 h. The obtained product was washed 4 times with distilled water until neutral, and dried at 120°C for 4 hours. The obtained sample was a core-shell structure ZSM-5 / mordenite composite molecular sieve, and the sample number was CL2.

[0049]

Embodiment 3

[0051] Take 35g of mordenite and 800mL of 0.8 mol / L KOH 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 3h. The resulting suspension is the structure-directing agent and is ready for use.

[0052] Take 14 g of sodium hydroxide and 8.5 g of sodium aluminate in 400 mL of distilled water, and stir vigorously until they are completely dissolved. Add 120 mL of silica sol slowly and stir vigorously for 30 min. Then add 30 mL of the structure-directing agent prepared in the previous step, and stir vigorously for 30 min; then add 25 g of ZSM-5 molecular sieve and 9 g of NaCl, stir vigorously for 20 min, put it into a closed reactor, and crystallize at 165 °C for 25 h. The obtained product was washed 4 times with distilled water to neutrality, and dried at 120°C for 4 hours. The obtained sample was a core-shell structure ZSM-5 / mordenite composite molecular sieve, and the sample number was CL3.

[0053] ...

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Abstract

The invention discloses a synthetic method of a ZSM-5 / mordenite composite molecular sieve, comprising the following steps of: firstly carrying out alkali treatment on mordenite under an enclosed condition so as to prepare a structure-directing agent; mixing inorganic base, an aluminium source, a silicon source and water with stirring according to a certain mole ratio, adding the structure-directing agent, ZSM-5 zeolite and chloride, and crystallizing at the temperature of 160-180 DEG C for 15-45 hours so as to obtain the product. According to the method, the structure-directing agent is used to greatly raise directing efficiency of mordenite, greatly reduce the amount of mordenite and simultaneously increase crystallization degree of mordenite in the composite molecular sieve. During the synthetic process, addition of the chloride is beneficial to synthesis of the core-shell structured molecular sieve with high degree of complexation. The method provided by the invention is simple and easy to operate. Raw materials are cheap, easily available and nontoxic and harmless such that the use of expensive and toxic organic template raw materials is avoided. Therefore, production cost is reduced, and the whole preparation process is green and environmental friendly.

Description

[0001] technical field [0002] The invention relates to a method for synthesizing a ZSM-5 / mordenite composite molecular sieve, which belongs to the field of synthesizing molecular sieve catalytic materials. [0003] Background technique [0004] ZSM-5 molecular sieve and mordenite are widely used in petrochemical and other fields due to their good shape-selective catalytic performance and good thermal stability. However, because the pore size of these two molecular sieves is uniform and single, it is not conducive to the treatment of raw materials with complex components. Composite molecular sieve is a kind of molecular sieve material with a composite structure of various compositions. Its pores and acid properties are the organic combination of the pores and acid properties of its constituent molecular sieves. It has better multi-level pores and reasonable acid distribution than individual molecular sieves. When complex reactants with different molecular diameters are us...

Claims

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Application Information

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IPC IPC(8): C01B39/38C01B39/26B01J29/40
Inventor 范峰凌凤香王少军杨春雁
Owner CHINA PETROLEUM & CHEM CORP
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