MWW molecular sieve, preparation method thereof and application of alkaloid in preparation of MWW molecular sieve

A technology of molecular sieves and alkaloids, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as industrial application restrictions, environmental health hazards, etc., achieve low cost, inhibit crystal transformation, and simple process Effect

Active Publication Date: 2022-03-25
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, in view of the fact that hexamethyleneimine, piperidine and other easily toxic or highly polluting chemicals must be used as templates and additives in the process of preparing MWW series molecular sieves in the prior art, it is necessary to stabilize the structure of synthetic MWW series molecular sieves. However, the process of preparing molecular sieves will cause great harm to the environment and people's health in the process of industrial application, and its industrial application is currently subject to great restrictions.

Method used

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  • MWW molecular sieve, preparation method thereof and application of alkaloid in preparation of MWW molecular sieve
  • MWW molecular sieve, preparation method thereof and application of alkaloid in preparation of MWW molecular sieve
  • MWW molecular sieve, preparation method thereof and application of alkaloid in preparation of MWW molecular sieve

Examples

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Effect test

Embodiment 1

[0085] The present invention provides a kind of preparation method of MCM-56 molecular sieve, wherein, the method comprises:

[0086] Silica gel (3g, pore size 2.5-4nm), NaAlO 2 , NaOH, (CH 3 ) 3 N + CH 2 CH 2 OH and H 2 O is 1SiO in molar ratio 2 :1 / 30Al 2 o 3 :0.1OH - :20H 2 O:0.1 template ((CH 3 ) 3 N + CH 2 CH 2 OH) mixed to form a mixture;

[0087] Add ITQ-1 molecular sieve active crystal seed to the mixture, obtain mixed glue; Wherein, the mass ratio of ITQ-1 molecular sieve active crystal seed and silica gel is, ITQ-1 molecular sieve active crystal seed:SiO 2 =0.05;

[0088] The mixed gum was hydrothermally crystallized at 150° C. for 48 hours, and the product obtained by hydrothermal crystallization was centrifuged, washed and dried to obtain MCM-56 molecular sieve.

[0089] Obtain the XRD figure of the MCM-56 molecular sieve prepared by the present embodiment, the result is as follows figure 1 As shown in the b spectrum in figure 1 It can be seen f...

Embodiment 2

[0092] The present invention provides a kind of preparation method of MCM-56 molecular sieve, wherein, the method comprises:

[0093] Coarse-porous silica gel (3g, pore size 5-10nm), aluminum chloride, KOH, (CH 3 ) 3 N + CH 2 COO - and H 2 O is 1SiO in molar ratio 2 :0.04Al 2 o 3 :0.12OH - :25H 2 O:0.15 template ((CH 3 ) 3 N + CH 2 COO - ) mixed to form a mixture;

[0094] Add MCM-22 molecular sieve active crystal seed to the mixture to obtain mixed glue; wherein, the mass ratio of MCM-22 molecular sieve active crystal seed to silica gel is, MCM-22 molecular sieve active crystal seed: SiO 2 =0.02;

[0095] The mixed gum was hydrothermally crystallized at 150° C. for 72 hours, and the product obtained by hydrothermal crystallization was centrifuged, washed and dried to obtain MCM-56 molecular sieve.

[0096] Obtain the XRD figure of the MCM-56 molecular sieve prepared by the present embodiment, the result is as follows figure 1 As shown in the c spectrum in f...

Embodiment 3

[0099] The present invention provides a kind of preparation method of MCM-56 molecular sieve, wherein, the method comprises:

[0100] Sodium silicate (6.1g), aluminum nitrate, KOH, CH 3 COOCH 2 CH 2 N(CH 3 ) 3 and H 2 O is 1SiO in molar ratio 2 :0.05Al 2 o 3 :0.13OH - :20H 2 O:0.18 template (CH 3 COOCH 2 CH 2 N(CH 3 ) 3 ) mixed to form a mixture;

[0101] Add SMC-1 crystal seed (prepared by the synthetic example of above-mentioned seed crystal SCM-1) in the mixture, obtain mixed glue; Wherein, the mass ratio of SMC-1 crystal seed and silica gel is, SMC-1 crystal seed: SiO 2 =0.02;

[0102] The mixed gum was hydrothermally crystallized at 150° C. for 96 hours, and the product obtained by hydrothermal crystallization was centrifuged, washed and dried to obtain MCM-56 molecular sieve.

[0103] Obtain the XRD pattern of the MCM-56 molecular sieve prepared by the present embodiment, the results are as follows figure 1 As shown in the d diagram in figure 1It can b...

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Abstract

The invention provides an MWW molecular sieve, a preparation method thereof and application of alkaloid in preparation of the MWW molecular sieve. The alkaloid is applied as a template agent in preparation of the MWW molecular sieve. The preparation method of the MWW molecular sieve comprises the following steps: mixing a silicon source, an aluminum source, an alkali source, a template agent and water according to a molar ratio of 1SiO2: 0.001-0.1 Al2O3: 0.005-0.6 OH <->: 5-50 H2O: 0.01-1 template agent to form a mixture; wherein alkaloid is selected as the template agent; adding an active seed crystal into the mixture to obtain mixed glue; wherein the mass ratio of the active seed crystal to the silicon source is that the mass ratio of the active seed crystal to SiO2 is (0.001-0.2): 1; and carrying out hydrothermal crystallization on the mixed glue at 100-180 DEG C for 24-240 hours to obtain the MWW molecular sieve.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a MWW molecular sieve, a preparation method thereof and the application of alkaloids in the preparation of the MWW molecular sieve. Background technique [0002] As we all know, molecular sieves such as MCM-22, MCM-49 and MCM-56 are important family members of MWW series molecular sieve structures. The structure of the MWW molecular sieve consists of a ten-membered ring sinusoidal channel (0.40nm×0.59nm) and a semi-supercage (0.70nm×0.71nm×0.71nm) located on the outer surface of the crystal, and also contains a part of the supercage (0.71nm×0.71nm×1.82 nm) composition. Unlike MCM-22 and MCM-49 molecular sieves, the layers of MCM-56 molecular sieves lack supercage connections, and the layers are stacked face to face. MCM-56 molecular sieve is recognized as the intermediate transition state in the synthesis process of MCM-49 molecular sieve, so the synthesi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48
CPCC01B39/48C01P2002/72
Inventor 巩雁军曹世伟
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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