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MCM-22 molecular sieve with controlled pore channel structure and preparation method thereof

A technology of MCM-22 and pore structure is applied in the field of preparation of MCM-22 molecular sieve, and achieves the effects of good technical effect, flexible crystallization method and stable process.

Inactive Publication Date: 2017-12-01
TIANJIN UNIVERSITY OF TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to prepare MCM-22 molecular sieve with controllable pore structure by using piperidine as a single template agent and by controlling the synthesis conditions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] According to the molar ratio of reaction materials: SiO 2 :0.025Al 2 o 3 :0.2Na 2 O:1.0PI:25H 2 O, configure the reaction mixture, then add 2% MCM-22 molecular sieve active seed crystals of the dry weight of the mixture, and the active crystal seeds are commercially available active crystal seeds. Wherein, the silicon source is ethyl orthosilicate, the aluminum source is sodium metaaluminate, the alkali source is sodium hydroxide, and the template agent is analytically pure piperidine. The mixture was vigorously stirred and treated in ultrasonic for 1 hour, then statically crystallized at 145°C for 48 hours, and the mother liquor was subjected to solid-liquid separation, washing, drying and roasting to obtain MCM-22 molecular sieve. The X-ray diffractometer determines that the crystal is MCM-22 molecular sieve, and the molecular sieve micropore part is 600m through the physical adsorption specific surface area measurement method. 2 / g, the mesopore part is 116m 2 ...

Embodiment 2

[0018] According to the molar ratio of reaction materials: SiO 2 :0.025Al 2 o 3 :0.5Na 2 O:0.5PI:25H 2 O, configure the reaction mixture, then add 2% MCM-22 molecular sieve active seed crystals of the dry weight of the mixture, and the active crystal seeds are commercially available active crystal seeds. Wherein, the silicon source is ethyl orthosilicate, the aluminum source is aluminum sulfate, the alkali source is sodium hydroxide, and the template agent is analytically pure piperidine. The mixture was vigorously stirred and treated in ultrasonic for 3 hours, then dynamically crystallized at 145°C for 33 hours. After crystallization, the mother liquor was subjected to solid-liquid separation, washing, drying and roasting to obtain MCM-22 molecular sieve. The X-ray diffractometer determines that the crystal is MCM-22 molecular sieve, and the molecular sieve micropore part is 514m according to the physical adsorption specific surface area measurement method. 2 / g, the mes...

Embodiment 3

[0020] According to the molar ratio of reaction materials: SiO 2 :0.033Al 2 o 3 :1.5Na 2 O:0.5PI:35H 2 O, configure the reaction mixture, then add 3% MCM-22 molecular sieve active seed crystals of the dry weight of the mixture, and the active crystal seeds are commercially available active crystal seeds. Wherein, the silicon source is silica sol, the aluminum source is sodium metaaluminate, the alkali source is sodium hydroxide, and the template agent is analytically pure piperidine. The mixture was vigorously stirred and treated in ultrasonic for 2 hours, then statically crystallized at 145°C for 50 hours. After crystallization, the mother liquor was subjected to solid-liquid separation, washing, drying and roasting to obtain MCM-22 molecular sieve. The X-ray diffractometer determines that the crystal is MCM-22 molecular sieve, and the molecular sieve micropore part is 368m according to the physical adsorption specific surface area measurement method. 2 / g, the mesopore ...

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Abstract

The invention relates to an MCM-22 molecular sieve with a controlled pore channel structure and a preparation method thereof, and mainly solves the problems that an MCM-22 molecular sieve pore channel cannot be controlled and the toxicity of a template agent is high in the prior art. According to the preparation method of the MCM-22 molecular sieve with the controlled pore channel structure disclosed by the invention, a silicon source, an aluminum source, the template agent and water are mixed to obtain a mixture, then a molecular sieve crystal seed is added into the mixture to carry out ultrasonic treatment, crystallization on the mixture is carried out for 1 hour to 120 hours at temperature of 110 DEG C to 190 DEG C in a static or dynamic method; after crystallization, mother liquid is subjected to solid-liquid separation, washing, drying and roasting to obtain the MCM-22 molecular sieve with the controlled pore channel structure; the shape of the molecular sieve is of a platy crystal, a micro-pore range is between 50m<2> / g and 800m<2> / g, the mesopore range is between 0m<2> / g and 500m<2> / g, and the total specific surface area range is between 50m<2> / g and 1100m<2> / g. By adopting the technical scheme, the problems are solved well, and the MCM-22 molecular sieve can be used in industrial production of relevant molecular sieves.

Description

technical field [0001] The invention relates to a preparation method of MCM-22 molecular sieve, in particular to a preparation method of MCM-22 molecular sieve with controllable pore structure. technical background [0002] MCM-22 molecular sieve is a layered molecular sieve with MWW topology. It was first synthesized by Mobil under the hexamethyleneimine template system in 1990. According to the analysis, the skeleton topology of MCM-22 consists of three sets of independent The composition of the pore system: one is a pore system in which a supercage with a pore size of 0.71nm×0.71nm×1.82nm is connected with an interlayer ten-membered ring of 0.40nm×0.54nm, and the other is a layer with a pore size of 0.40nm×0.59nm The two-dimensional intersecting sinusoidal network channel system of the inner ten-membered ring, and the 12-membered ring hole located on the outer surface of the crystal with a depth of 0.70nm, the size of which is 0.70×0.71×0.71nm. The unique pore structure ...

Claims

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Application Information

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IPC IPC(8): C01B39/04
CPCC01B39/04C01P2006/12C01P2006/14C01P2006/17
Inventor 张舜光甄彬王华伟王雷
Owner TIANJIN UNIVERSITY OF TECHNOLOGY