Method for preparing mordenite/ Zeolite Socony Mobil (ZSM)-5 composite molecular sieve

A technology of ZSM-5 and composite molecular sieve, which is applied in the direction of mercerized crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of high conversion rate of C4 hydrocarbons, low Catalytic activity etc.

Active Publication Date: 2012-05-23
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The results show that compared with ZSM-5, MOR has very low catalytic activity, but the ZSM-5/MOR composite molecular sieve shows highe

Method used

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  • Method for preparing mordenite/ Zeolite Socony Mobil (ZSM)-5 composite molecular sieve
  • Method for preparing mordenite/ Zeolite Socony Mobil (ZSM)-5 composite molecular sieve
  • Method for preparing mordenite/ Zeolite Socony Mobil (ZSM)-5 composite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Mix 0.42g of solid sodium hydroxide, 1.5g of tetraethylammonium bromide (TEABr, 99%, analytically pure), and 15g of deionized water evenly, add 0.4g of ZSM-5 seed crystals, and oscillate ultrasonically for 30 minutes to disperse the crystal seeds evenly . After that, 5.0 g of kaolin microspheres and 2.0 g of white carbon black were added, and stirred for 20 min to form a uniform gel. The gel was transferred to a polytetrafluoroethylene self-pressurized reactor, sealed and aged at room temperature for 30 hours, and then moved into an oven for crystallization at 150°C for 48 hours. After the reaction, the solid product was isolated, washed with deionized water until neutral, dried overnight at 120°C, and calcined at 550°C to obtain a sodium-type mordenite / ZSM-5 composite molecular sieve product.

[0025] The molar ratio of raw materials in the reaction system is: SiO 2 / Al 2 o 3 =30,Na 2 O / SiO 2 =0.1, TEA+ / SiO 2 =0.15,H 2 O / SiO 2 =17. Comparing the XRD diffracti...

Embodiment 2

[0027] Mix 0.30 g of solid sodium hydroxide, 1.5 g of tetraethylammonium bromide (TEABr, 99%, analytically pure), and 15 g of deionized water evenly, add 0.4 g of ZSM-5 seed crystals, and oscillate ultrasonically for 30 minutes to disperse the crystal seeds evenly . After that, 5.0 g of kaolin microspheres and 2.0 g of white carbon black were added, and stirred for 20 min to form a uniform gel. The gel was transferred to a polytetrafluoroethylene self-pressurized reactor, sealed and aged at room temperature for 30 hours, and then moved into an oven for crystallization at 150°C for 48 hours. After the reaction, the solid product was isolated, washed with deionized water until neutral, dried overnight at 120°C, and calcined at 550°C to obtain a sodium-type mordenite / ZSM-5 composite molecular sieve product.

[0028] The molar ratio of raw materials in the reaction system is: SiO 2 / Al 2 o 3 =30,Na 2 O / SiO 2 =0.075, TEA+ / SiO 2 =0.15,H 2 O / SiO 2 =17. Comparing the XRD dif...

Embodiment 3

[0030] Mix 0.42 g of solid sodium hydroxide, 1.5 g of tetraethylammonium bromide (TEABr, 99%, analytically pure), and 15 g of deionized water evenly, add 0.4 g of mordenite seed crystals, and oscillate ultrasonically for 30 minutes to disperse the crystal seeds evenly. After that, 5.0 g of kaolin microspheres and 2.0 g of white carbon black were added, and stirred for 20 min to form a uniform gel. The gel was transferred to a polytetrafluoroethylene self-pressurized reactor, sealed and aged at room temperature for 30 hours, and then moved into an oven for crystallization at 150°C for 48 hours. After the reaction, the solid product was isolated, washed with deionized water until neutral, dried overnight at 120°C, and calcined at 550°C to obtain a sodium-type mordenite / ZSM-5 composite molecular sieve product.

[0031] The molar ratio of raw materials in the reaction system is: SiO 2 / Al 2 o 3 =30,Na 2 O / SiO 2 =0.1, TEA+ / SiO 2 =0.15,H 2 O / SiO 2 =17. Comparing the XRD diffr...

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Abstract

The invention relates to a method for preparing a mordenite/Zeolite Socony Mobil (ZSM)-5 composite molecular sieve, which comprises the following steps: evenly mixing sodium hydroxide, tetraethylammonium bromide and deionized water; adding mordenite or ZSM-5 seed crystal, wherein the seed crystal addition volume is 5wt% of total feeding material SiO2; carrying out ultrasonic vibration for 30min to evenly disperse the seed crystal; then, adding kaolin microspheres and white carbon black; stirring for half an hour, and transferring gel into a polytetrafluoroethylene reaction kettle; and then transferring the gel into an oven after ageing at the room temperature for 10-40h and crystallizing at the temperature of 110-170DEG C for 14-70h. A reaction system is formed at the following molar ratio: SiO2/Al2O3 is equal to 10-60, Na2O/SiO2 is equal to 0.029-0.31, tetraethylammonium (TEA)+/SiO2 is more than or equal to 0.02, and H2O/SiO2 is equal to 5.0-30.0. In the method, only the single seedcrystal needs to be added to obtain a product which can be directly used for fluid catalytic cracking (FCC) reaction after being slightly modified.

Description

technical field [0001] The invention relates to a method for preparing mordenite / ZSM-5 composite molecular sieves with kaolin microspheres as raw materials and an in-situ crystallization process. Background technique [0002] ZSM-5 and Mordenite (MOR) are two molecular sieves widely used in oil refining and petrochemical industries. ZSM-5 has an MFI structure, and its unique ten-membered ring channel structure prevents the formation of ring-shaped condensed ring aromatic hydrocarbon condensation products and enters the channel, thereby inhibiting the formation of coke. Its excellent thermal and hydrothermal stability makes it have good aromatization activity and low-carbon olefin selectivity. Mordenite has a large one-dimensional twelve-membered ring straight channel and excellent heat resistance, acid resistance and isomerization performance, but because the one-dimensional channel of mordenite is easy to coke and deactivate, and its hydrothermal stability is poor, it is d...

Claims

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Application Information

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IPC IPC(8): C01B39/26C01B39/38
Inventor 郭士岭潘晖华陈宜俍朴佳锐禹子洋庞新梅高林波陈新兴卫冬燕阎立军
Owner PETROCHINA CO LTD
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