A dual-functional template for the synthesis of hierarchically porous zsm-12 zeolite molecular sieves and its preparation and molecular sieves based on it

A ZSM-12, zeolite molecular sieve technology, applied in the field of molecular sieves, to achieve the effects of high hydrothermal stability, high thermal stability and good application value

A ZSM-12, zeolite molecular sieve technology, applied in the field of molecular sieves, to achieve the effects of high hydrothermal stability, high thermal stability and good application value

CN106966408BActive Publication Date: 2019-01-29SOUTH CHINA UNIV OF TECH
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  • A dual-functional template for the synthesis of hierarchically porous zsm-12 zeolite molecular sieves and its preparation and molecular sieves based on it
  • A dual-functional template for the synthesis of hierarchically porous zsm-12 zeolite molecular sieves and its preparation and molecular sieves based on it
  • A dual-functional template for the synthesis of hierarchically porous zsm-12 zeolite molecular sieves and its preparation and molecular sieves based on it

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Embodiment 1: the preparation of bifunctional templating agent

[0052] (1) Dissolve 3.5gα,α'-dibromo-p-xylene and 6.88g N,N,N',N'-tetramethyl-1,6-hexanediamine in 100mL acetonitrile solvent, under nitrogen protection conditions , heated to 70°C and held for 24 hours;

[0053] (2) Add a sufficient amount of diethyl ether to the solution obtained in step (1), specifically add the solution to diethyl ether at a volume ratio of 1:3, seal and put it into the refrigerator for 12 hours to cool and precipitate;

[0054] (3) Suction filter the precipitate obtained in step (2) with ether, and wash repeatedly. Put it into a vacuum oven at 60°C for 12 hours to ensure that the organic matter is completely volatilized to obtain the bifunctional template agent BSDA, the template agent of Example 1 13 C NMR spectrum see figure 1 .

Embodiment 2

[0055] Embodiment 2: the preparation of bifunctional templating agent

[0056] (1) Dissolve 1.7g of 1,4-benzenediol and 5.8g of N,N,N',N'-tetramethyl-1,3-butanediamine in 100mL of acetonitrile solvent, and heat the to 75°C and hold for 16 hours;

[0057] (2) Add a sufficient amount of diethyl ether to the solution obtained in step (1), specifically add the solution to diethyl ether at a volume ratio of 1:3, seal and put it into the refrigerator for 12 hours to cool and precipitate;

[0058] (3) Suction filter the precipitate obtained in step (2) with ether, and wash repeatedly. Dry in a vacuum oven at 60°C for 12 hours to ensure complete volatilization of organic matter to obtain the bifunctional template agent BSDA.

Embodiment 3

[0059] Embodiment 3: the preparation of bifunctional templating agent

[0060] (1) Dissolve 3.5gα,α'-dibromo-p-xylene and 6.88g N,N,N',N'-tetramethyl-1,6-hexanediamine in 100mL acetonitrile solvent, under nitrogen protection conditions , heated to 65°C and held for 36 hours;

[0061] (2) Add a sufficient amount of diethyl ether to the solution obtained in step (1), specifically add the solution to diethyl ether at a volume ratio of 1:3, seal and put it into the refrigerator for 12 hours to cool and precipitate;

[0062] (3) Suction filter the precipitate obtained in step (2) with ether, and wash repeatedly. Dry in a vacuum oven at 60°C for 12 hours to ensure complete volatilization of organic matter to obtain the bifunctional template agent BSDA.

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Abstract

The invention belongs to the technical field of molecular sieve catalytic material synthesis and discloses a difunctional template agent for oriented synthesis of a hierarchical-pore ZSM-12 type zeolite molecular sieve, a preparation method of such difunctional template agent and a molecular sieve based on such difunctional template agent. The preparation method includes the steps of dissolving at least one of alpha,alpha'-dichloro-p-xylene, alpha,alpha'-dibromo-p-xylene and hydroquinone and at least one of N,N,N',N'-tetramethyl-1,3-butanediamine, N,N,N',N'-tetramethyl-1,5-pentanediamine, N,N-dimethylhexylamine, N,N,N',N'-tetramethyl-1,6-hexanediamine and homologs thereof into a solvent prior to heating and holding so as to obtain the difunctional template agent. A micro / mesoporous hierarchical-pore ZSM-12 type molecular sieve can be obtained through the difunctional template agent according to a one-step hydrothermal method, and is of a crystallized mesoporous wall structure so as to avoid the defects of traditional single porous structure effectively.

Description

technical field [0001] The invention belongs to the technical field of synthesis of molecular sieve catalytic materials, and in particular relates to a dual-functional template agent for guiding the synthesis of hierarchically porous ZSM-12 type zeolite molecular sieves, a preparation method thereof and a molecular sieve based thereon. Background technique [0002] Since the 1950s, traditional microporous zeolite molecular sieves have been widely used in catalysis and adsorption separation in petrochemical and related industries. , zeolite materials are helpless in the catalysis and separation of organic molecules with large diameters. Ordered mesoporous (2-50nm) and macroporous (>50nm) molecular sieve materials are also difficult to be widely used in the field of catalysis due to their low framework acid activity and hydrothermal stability. Therefore, hierarchically porous molecular sieve materials (also known as mesoporous zeolites) with both micropores and mesoporous ...

Claims

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Application Information

Patent Timeline
29 Jan 2019
Publication
CN106966408B
IPC
C07C209/12; C01B39/42; C07C211/63
CPC
C01B39/42; C01P2002/72; C01P2004/03; C01P2004/04; C01P2006/12; C01P2006/17; C07C209/12; C07C211/63
Inventors
张凯; 奚红霞