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Method for synthesis of MCM-22 molecular sieve

A molecular sieve and aniline technology, applied in the field of synthesizing MCM-22 molecular sieve, can solve the problem of irreplaceable role of composite template agent, and achieve the effect of reducing synthesis cost and dosage

Active Publication Date: 2014-05-07
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, hexamethyleneimine 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

[0034] This example illustrates the synthetic method provided by the present invention.

[0035] A certain amount of sodium metaaluminate (Sinopharm Group, analytically pure) and sodium hydroxide (Beijing Reagent Company, analytically pure) were dissolved in deionized water, stirred until completely dissolved, and solid silica gel (Qingdao Ocean Chemical Factory, dry basis 97 %) was added to the above solution, and then hexamethyleneimine (TCI, Japan, analytically pure) and aniline (Beijing Chemical Plant, analytically pure) were added. The colloidal molar ratio of the mixture is: 0.18NaOH:SiO 2 :0.033Al 2 o 3 : 0.10 hexamethyleneimine: 0.20 aniline: 15H 2 O, the crystallization temperature is 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 roast at 550°C for 10 hours to obtain a sample.

[0036] The XRD diffraction pattern of the test sample, the 2θ angle is 0 to 35°, ...

Embodiment 2

[0049] This example illustrates the synthetic method provided by the present invention.

[0050] The silicon source, aluminum source, alkali source, and deionized water used in Example 1 are the same as in Example 1. The difference from Example 1 is that the ratio of hexamethyleneimine to aniline is different in Example 2. The colloidal molar ratio of the mixture is 0.18NaOH:SiO 2 :0.033Al 2 o 3 :0.05 hexamethyleneimine: 0.25 aniline: 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 roast at 550°C for 10 hours to obtain a sample.

[0051] Test its XRD diffraction pattern, the 2θ angle is 0 to 35°, the product is MCM-22 molecular sieve, the specific surface is 496m 2 / g, the relative crystallinity is 95%. , The saturated adsorption capacity of mesitylene is 7.01mg / g.

[0052] The amount of hexamethyleneimine used in this example is o...

Embodiment 3

[0058] This example illustrates the synthetic method provided by the present invention.

[0059] The silicon source, aluminum source, alkali source, deionized water and templating agent used in this embodiment and the operation steps are the same as in embodiment 1, the difference is that the aniline used in this embodiment is after the crystallization of embodiment 1 and embodiment 2. The templating agent is separated from the mother liquor, and after liquid separation, the upper aniline phase is taken as the source of aniline in this embodiment.

[0060] The colloidal molar ratio of the mixture is: 0.18NaOH:SiO 2 :0.033Al 2 o 3 : 0.10 hexamethyleneimine: 0.20 aniline: 15H 2 O, the crystallization temperature is 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 roast at 550°C for 10 hours to obtain a sample.

[0061] Test its XRD diffraction pattern, the 2θ angle is 0 to...

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Abstract

The invention discloses a method for synthesis of an MCM-22 molecular sieve. The method is characterized in that a molecular sieve is synthesized under hydrothermal crystallization conditions; a used template agent contains hexamethylene imine and aniline; and a mole ratio of the hexamethylene imine to the aniline is less than 1.2. The method reduces a hexamethylene imine use amount, reduces a cost, inhibits conversion of the MCM-22 molecular sieve into a ZSM-35 molecular sieve, realizes obvious improvement of a product specific surface area and obviously promotes improvement of a mesitylene saturated adsorption capacity.

Description

technical field [0001] The invention relates to a method for synthesizing molecular sieves, in particular, a method for synthesizing MCM-22 molecular sieves. 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 shows the characteristics of twelve-membered rings, and also...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
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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