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Synthesis method of MCM (Mobil Composition of Matter)-22 molecular sieve

A synthesis method and molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of irreplaceable effect of composite templates

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

[0039] This example illustrates the synthetic method provided by the present invention.

[0040] The colloidal molar ratio of mixture A is: 0.18NaOH:SiO 2 :0.033Al 2 o 3 :0.30HMI: 15H 2 O, the crystallization temperature is 145°C, under autogenous pressure, after hydrothermal crystallization at a stirring speed of 300 rpm for 24 hours, the directing agent is obtained by cooling to room temperature, and the XRD spectrum of the obtained sample does not have any MCM-22 characteristic diffraction peaks.

[0041] Continue to add silicon source, aluminum source, alkali source, aniline and deionized water to it, obtain molar ratio and be:

[0042] 0.18NaOH:SiO 2 :0.033Al 2 o 3 :0.075HMI:0.225AN:15H 2 O mixture B and stir well to SiO 2 On a molar basis, the silicon source of the directing agent / total silicon source=1:4, at a crystallization temperature of 145°C and an autogenous pressure, the hydrothermal crystallization was continued for 96 hours at a stirring speed of 250 rp...

Embodiment 2

[0045] This example illustrates the synthetic method provided by the present invention.

[0046] The colloidal molar ratio of mixture A is: 0.18NaOH:SiO 2 :0.033Al 2 o 3 :0.10HMI:0.20AN:

[0047] 15H 2 O, the crystallization temperature is 145°C, the product is cooled to room temperature after hydrothermal crystallization under stirring for 24 hours to obtain the directing agent. The XRD spectrum of the obtained sample does not have any MCM-22 characteristic diffraction peaks.

[0048] Continue to add silicon source, aluminum source, alkali source, aniline and deionized water to it, obtain molar ratio and be 0.18NaOH:SiO 2 :0.033Al 2 o 3 :0.05HMI:0.25AN:15H 2 O mixture B and stir well to SiO 2 On a molar basis, silicon source of the directing agent / total silicon source=1:2, at a crystallization temperature of 145°C and autogenous pressure, continue hydrothermal crystallization at a stirring speed of 250 rpm for 96 hours, take out the product after cooling, and filter ...

Embodiment 3

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

[0052] The colloidal molar ratio of mixture A is 0.18NaOH:SiO 2 :0.033Al 2 o 3 :0.05HMI:0.25AN:15H 2 O, the crystallization temperature is 155°C, the product is cooled to room temperature after hydrothermal crystallization under stirring for 32 hours to obtain the directing agent. The XRD spectrum of the obtained sample does not have any MCM-22 characteristic diffraction peaks.

[0053] Continue to add silicon source, aluminum source, alkali source, aniline and deionized water to it to obtain molar ratio: 0.18NaOH: SiO 2 :0.033Al 2 o 3 :0.025HMI:0.275AN:15H 2 O mixture B and stir well to SiO 2 On a molar basis, the silicon source of the directing agent / total silicon source=1:2, at a crystallization temperature of 155°C, under autogenous pressure, continue the hydrothermal crystallization at a stirring speed of 250 rpm for 120 hours, take out the product after cooling, and filter ...

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Abstract

The invention discloses a synthesis method of an MCM (Mobil Composition of Matter)-22 molecular sieve. The synthesis method is characterized by comprising the steps of mixing raw materials to obtain a mixture A, wherein the raw materials include a silicon source, an aluminum source, an alkaline source, a template agent and deionized water; treating the obtained mixture A under a hydrothermal crystallization condition to obtain a guiding agent; mixing the guiding agent, the silicon source, the aluminum source, the alkaline source, phenylamine and the deionized water to obtain a mixture B; crystallizing the obtained mixture B under a hydrothermal condition and recovering a product, wherein the template agent is hexamethyleneimine or a hexamethyleneimine and phenylamine mixture containing hexamethyleneimine and phenylamine which are in the molar ratio of at least 0.05:1, and the weight ratio (measured by SiO2) of the silicon source from the guiding agent in the mixture B to the total silicon source in the mixture B is (0.05-1):1. The method can be used for effectively reducing the consumption of hexamethyleneimine, improving the stability of the MCM-22 molecular sieve and inhibiting the crystal transformation of the molecular sieve.

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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