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Synthetic method for MCM-22 molecular sieve

A technology of MCM-22 and synthesis method, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of irreplaceable effect of composite template agent, and achieve the reduction of synthesis cost, dosage and harm Effect

Active Publication Date: 2014-01-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this patent significantly expands the scope of templates used in MCM-22 molecular sieves, HMI is still the most commonly used template for the synthesis of MCM-22 series molecular sieves, and its role in composite templates is irreplaceable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] This example illustrates the synthetic method provided by the present invention.

[0042] The preparation process of MCM-22 as the seed crystal: the raw materials and steps of Comparative Example 1 are exactly the same, the difference is that the colloidal molar ratio of the mixture is: 0.18NaOH:SiO 2 :0.033Al 2 o 3 :0.30HMI: 15H 2 O, crystallization temperature 145°C, under autogenous pressure, crystallize at a stirring speed of 300 rpm for 72 hours, take out the product after cooling, filter, wash and dry, and use it as uncalcined MCM-22 seed crystal A.

[0043] Dissolve aluminum source and sodium hydroxide in deionized water, stir until completely dissolved, add unroasted MCM-22 seed crystal A, silicon source and aniline, and continue to stir evenly. The colloidal molar ratio of the resulting mixture is: 0.18NaOH:SiO 2 (total): 0.033Al 2 o 3 :0.33MCM-22 (SiO 2 Gauge): 0.20AN: 15H 2 O. Then transfer the resulting mixture to a closed crystallization tank, stir...

Embodiment 2

[0046] This example illustrates the synthetic method provided by the present invention.

[0047] The preparation process of MCM-22 as the seed crystal: silicon source, aluminum source, alkali source, and deionized water are used. The operation steps are the same as in Example 1, except that HMI and AN are used as composite templates. The colloidal molar ratio of the mixture is: 0.18NaOH:SiO 2 :0.033Al 2 o 3 :0.10HMI:0.20AN:15H 2 O, crystallization temperature 145°C, under autogenous pressure, crystallize at a stirring speed of 300 rpm for 72 hours, take out the product after cooling, filter, wash and dry, and use it as uncalcined MCM-22 seed crystal B.

[0048] Dissolve aluminum source and sodium hydroxide in deionized water, stir until completely dissolved, add unroasted MCM-22 seed crystal B, silicon source and aniline, and continue to stir evenly. The colloidal molar ratio of the resulting mixture is: 0.18NaOH:SiO 2 (total): 0.033Al 2 o 3 :0.33MCM-22 (SiO 2 Gauge): ...

Embodiment 3

[0051] This example illustrates the synthetic method provided by the present invention.

[0052] The preparation process of MCM-22 as the seed crystal: silicon source, aluminum source, alkali source, and deionized water are used. The operation steps are the same as in Example 2, except that the ratio of HMI and AN in Example 2 is different. The colloidal molar ratio of the mixture is 0.18NaOH:SiO 2 :0.033Al 2 o 3 :0.05HMI:0.25AN:15H 2 O, crystallization temperature 155°C, under autogenous pressure, crystallize at a stirring speed of 400 rpm for 96 hours, take out the product after cooling, filter, wash and dry, and use it as uncalcined MCM-22 seed crystal C.

[0053] Dissolve aluminum source and sodium hydroxide in deionized water, stir until completely dissolved, then add unroasted MCM-22 seed crystal C, silicon source and aniline, and continue to stir evenly. The colloidal molar ratio of the resulting mixture is: 0.18NaOH:SiO 2 (total): 0.033Al 2 o 3 :0.50MCM-22 (SiO 2...

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Abstract

The invention discloses a synthetic method for an MCM-22 molecular sieve, which is characterized by comprising the following steps of: mixing an unroasted MCM-22 molecular sieve, a silicon source, an aluminum source, aniline and deionized water, and uniformly stirring the substances to obtain a mixture colloid; and carrying out hydrothermal crystallization on the mixture colloid in a closed reaction kettle under self-generated pressure conditions, and recycling a resulting substance to obtain the MCM-22 molecular sieve, wherein the ratio of the silicon in the unroasted MCM-22 molecular sieve to the total silicon in the mixture colloid is (0.05-1) to 1 based on SiO2 mole, and the ratio of the aniline to the total silicon in the mixture colloid is (0.1-1) to 1 based on SiO2 mole.

Description

technical field [0001] The present invention relates to a method for synthesizing molecular sieves, in particular to a method for synthesizing molecular sieves with an MCM-22 molecular sieve crystal phase structure. Background technique [0002] MCM-22 molecular sieve is a representative molecular sieve of the MWW family of molecular sieves. MCM-22 molecular sieve has two sets of independent pore systems that are not directly connected to each other: a ten-membered ring channel with a pore diameter of 0.40×0.59 nm in the layer; a twelve-membered ring supercage with a 0.40 nm diameter between layers. The opening of the ten-membered ring of ×0.54nm communicates with the outside world. On the crystal surface of MCM-22 molecular sieve, there are some twelve-membered ring holes, which are half of the supercage, and the depth is about 0.71nm (Science, 1994, 264:1910). Therefore, in some catalytic reactions, it not only shows the characteristics of ten-membered rings, but also sh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04B01J29/06
Inventor 邢恩会谢文华刘强慕旭宏罗一斌舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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