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Method for preparing MCM-22/Beta composite molecular sieve

A technology of MCM-22 and composite molecular sieves, which is applied in molecular sieves and base exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of inappropriate large-scale production, and achieve the effect of easy large-scale production and simple operation

Pending Publication Date: 2019-10-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN105565335B and CN109046445A have successively disclosed that by adding surface-modified Beta molecular sieves to the synthesis system of MWW molecular sieves, a composite molecular sieve with a core-shell structure is obtained, but in this process, complex plasma surface modification or cationic modification of Beta molecular sieves is required first. Sexual treatment, not suitable for large-scale production

Method used

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  • Method for preparing MCM-22/Beta composite molecular sieve
  • Method for preparing MCM-22/Beta composite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The raw materials used are as follows:

[0017] (1) Silica sol (30.19wt.% SiO 2 , 0.29 wt.% Na 2 O, 0.23wt.% Al 2 o 3 , 69.29 wt.% H 2 O);

[0018] (2) Sodium metaaluminate (NaAlO 2 , 16.80wt.% Al 2 o 3 , 19.38 wt.% Na 2 O, 63.82 wt.% H 2 O);

[0019] (3) Sodium hydroxide (content ≥ 96%);

[0020] (4) deionized water;

[0021] (5) piperidine;

[0022] (6) Beta molecular sieve.

[0023] According to the molar ratio: 0.2Na 2 O: 0.03Al 2 o 3 : 1.0 SiO 2 : 20H 2 O: 0.4R: 30% Beta molecular sieve, stir and mix 198.7g silica sol, 15.5g sodium metaaluminate, 11.5g sodium hydroxide, 212.4g deionized water and 34.1g piperidine in a certain order, then add 18.9g Mix the Beta molecular sieves evenly, add them into the synthesis kettle and seal it, and make it dynamically crystallize at 150° C. for 48 hours. Wash the solid product with deionized water until the washing liquid is neutral, then centrifuge and dry overnight at 120°C to obtain a molecular sieve prod...

Embodiment 2

[0025] The raw materials used are as follows:

[0026] (1) White carbon black (dry basis 86.6%);

[0027] (2) Sodium metaaluminate (NaAlO 2 , 16.80wt.% Al 2 o 3 , 19.38 wt.% Na 2 O, 63.82 wt.% H 2 O);

[0028] (3) Sodium hydroxide (content ≥ 96%);

[0029] (4) deionized water;

[0030] (5) Hexamethyleneimine;

[0031] (6) Beta molecular sieve.

[0032] According to the molar ratio: 0.1Na 2 O: 0.01Al 2 o 3 : 1.0 SiO 2 : 30H 2 O: 0.3R: 20% Beta molecular sieve, mix 69.28g white carbon black, 6.07g sodium metaaluminate, 6.75g sodium hydroxide, 526.8g deionized water and 29.8g hexamethyleneimine in a certain order and mix evenly , and then add 12.2g of Beta molecular sieves and mix evenly, add it into the synthesis kettle and seal it, and make it dynamically crystallize at 160°C for 24h. Wash the solid product with deionized water until the washing liquid is neutral, centrifuge and dry overnight at 120°C to obtain a molecular sieve product, and its X-ray diffraction...

Embodiment 3

[0034] The raw materials used are as follows:

[0035] (1) Silica gel (dry basis 92.7%);

[0036] (2) Sodium metaaluminate (NaAlO 2 , 16.80wt.% Al 2 o 3 , 19.38 wt.% Na 2 O, 63.82 wt.% H 2 O);

[0037] (3) Sodium hydroxide (content ≥ 96%);

[0038] (4) deionized water;

[0039] (5) piperidine;

[0040] (6) Beta molecular sieve.

[0041] According to the molar ratio: 0.5Na 2 O: 0.04Al 2 o 3 : 1.0 SiO 2 : 15H2 O: 0.5R: 15% Beta molecular sieve, stir and mix 64.7g silica gel, 24.3g sodium metaaluminate, 35.3g sodium hydroxide, 249.8g deionized water and 42.6g piperidine in a certain order, and then add 9.15g Beta Molecular sieves were mixed evenly, added to the synthesis kettle and then sealed for dynamic crystallization at 140°C for 56 hours. Wash the solid product with deionized water until the washing liquid is neutral, centrifuge and dry overnight at 120°C to obtain a molecular sieve product, and its X-ray diffraction (XRD) spectrum is consistent with figure 1 ...

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Abstract

The invention provides a method for preparing an MCM-22 / Beta composite molecular sieve. The synthetic method comprises the following steps: directly adding a Beta molecular sieve into mixed gel of analuminum source, a silicon source, an alkali source, a template agent and deionized water, performing full and uniform stirring, crystallizing at a temperature of 130-160 DEG C for 24-72 hours, and performing washing separation and drying, thereby obtaining the MCM-22 / Beta composite molecular sieve. According to the method disclosed by the invention, the Beta molecular sieve is directly added intothe synthesis system without any treatment, and by changing the addition amount of the Beta molecular sieve and reasonably matching synthesis conditions, the MCM-22 / Beta composite molecular sieve having the mass fraction of the Beta molecular sieve of 3-47% is prepared so as to meet requirements in different application fields. The preparation method provided by the invention is simple in operation and easy for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis of inorganic materials, and in particular relates to a preparation method of an MCM-22 / Beta composite molecular sieve. Background technique [0002] Beta molecular sieve is a molecular sieve with three-dimensional twelve-membered ring straight channels. MCM-22 contains two relatively independent channel systems: ten-membered ring sinusoidal channels in the layer and twelve-membered ring supercages between layers. There are also openings on the surface. Semi-supercages of twelve-membered rings. These two molecular sieves have good reactivity for the alkylation of benzene and ethylene, but because of their different topological structures, they show their own advantages. Beta molecular sieve has high low-temperature reactivity, but its ethylbenzene selectivity is low; MCM-22 molecular sieve has lower low-temperature reactivity than Beta molecular sieve, but it has high ethylbenzene selec...

Claims

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Application Information

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IPC IPC(8): C01B39/48
CPCC01B39/48C01P2002/72C01P2004/82
Inventor 谢素娟王亚男徐龙伢朱向学曲令多高扬郭英杰陈福存李秀杰崔倩
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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