Unlock instant, AI-driven research and patent intelligence for your innovation.

A method for synthesizing silicalite-2 all-silicon molecular sieves

A technology of all-silicon molecular sieve and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of molecular sieves prone to mixed crystal state, high temperature in gelation process, and long crystallization time, so as to shorten the gel and crystallization time. Time-saving, easy to operate, and low-cost effects

Active Publication Date: 2018-02-09
CHINA PETROLEUM & CHEM CORP +1
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires a narrow range of synthetic pH, high temperature in the gelation process, and long crystallization time, so the obtained molecular sieve is prone to mixed crystal state

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A method for synthesizing silicalite-2 all-silicon molecular sieves
  • A method for synthesizing silicalite-2 all-silicon molecular sieves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Configure ZSM-5 seed crystal solution: mix ethanol: water according to the volume ratio of 40: 100 to obtain an alcohol solution, add the material to the alcohol solution according to the ratio of 2.0KBr: 1.2PEG400: 100 water and stir for 1 h, then ZSM-5 molecular sieves were ground to below 300 mesh, and ZSM-5 seed crystals were added to the above solution according to the mass ratio of 10 ZSM-5:100 water to prepare a ZSM-5 seed crystal solution.

[0032] Prepare the mixed solution of tetrabutylammonium hydroxide and sodium hydroxide that the pH value is 13.15, then add white carbon black and ZSM-5 seed crystal solution in the material (the amount of seed crystal takes ZSM-5 to account for the SiO used 2 The mass percentage is calculated as 2.5%), sealed and uniformly stirred for 1.0 hours to obtain a mixture gel system, the molar ratio of each material in the gel is 3.2NaOH: 6.0TBAOH: 100SiO 2 : 5350H 2 O, the final mixture gel system was crystallized at 140°C for 2 ...

Embodiment 2

[0034] Configure the ZSM-5 seed crystal solution: mix ethanol: water according to the volume ratio of 10: 100 to obtain an alcohol solution, add the material to the alcohol solution according to the ratio of 0.5Cl: 0.5PEG400: 100 water and stir for 1 h, and then Grinding ZSM-5 molecular sieves to below 300 mesh, adding ZSM-5 seed crystals to the above solution according to the mass ratio of 5 ZSM-5:100 water, to prepare ZSM-5 seed crystal solution.

[0035] Prepare the mixed solution of tetrabutylammonium hydroxide and sodium hydroxide that the pH value is 13.15, then add white carbon black and ZSM-5 seed crystal solution in the material (the amount of seed crystal takes ZSM-5 to account for the SiO used 2 The mass percentage is calculated as 2.5%), sealed and uniformly stirred for 1.0 hours to obtain a mixture gel system, the molar ratio of each material in the gel is 3.2NaOH: 6.0TBAOH: 100SiO 2 : 5350H 2 O, the final mixture gel system was crystallized at 140°C for 2 days, ...

Embodiment 3

[0037] Configure ZSM-5 seed crystal solution: mix ethanol: water according to the volume ratio of 80: 100 to obtain an alcohol solution, according to the mass ratio of 15KBr: 15PEG400: 100 water, add the material to the alcohol solution and stir for 1 h, then ZSM -5 molecular sieves are ground to below 300 mesh, and ZSM-5 seed crystals are added to the above solution according to the mass ratio of 20 ZSM-5: 100 water to prepare a ZSM-5 seed crystal solution.

[0038] Prepare the mixed solution of tetrabutylammonium hydroxide and sodium hydroxide that the pH value is 12.2, then add white carbon black and ZSM-5 seed crystal solution in the material (the amount of seed crystal takes ZSM-5 to account for the SiO used 2 The mass percentage is calculated as 4.3%), sealed and uniformly stirred for 2.5 hours to obtain a mixture gel system, the molar ratio of each material in the gel is 2.6NaOH: 15.0TBAOH: 100SiO 2 : 2800H 2 O, the final mixture gel system was crystallized at 120°C fo...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
specific surface areaaaaaaaaaaa
specific surface areaaaaaaaaaaa
specific surface areaaaaaaaaaaa
Login to View More

Abstract

The invention provides a method for synthesizing Silicalite‑2 all-silicon molecular sieve, which belongs to the field of molecular sieve synthesis. The synthesis method includes the following steps: (1) configuring ZSM‑5 seed crystal solution: firstly mix alcohol and water to obtain an alcohol solution, then add solvent A and solvent B, stir until completely dissolved, then add ZSM‑5 seed crystal, and stir evenly Finally, the ZSM-5 seed solution is obtained; (2) prepare a mixed solution containing a template agent and an alkali source, and the pH value of the mixed solution is 9.00 to 14.0; (3) add a silicon source and the obtained in step (1) to the mixed solution ZSM-5 seed crystal solution, and then mix the mixed solution uniformly under airtight conditions to obtain a gel; then the gel is crystallized at 100°C-170°C for 10-120h, and then separated, washed, dried, and roasted. Silicalite‑2 all silicon molecular sieve. The method of the invention has simple preparation process and low cost, and the prepared all-silicon molecular sieve has high crystallinity and is suitable for industrial application.

Description

technical field [0001] The invention relates to a method for synthesizing all-silicon molecular sieves, in particular to a method for rapidly synthesizing all-silicon molecular sieves Silicalite-2 induced by crystal seeds. Background technique [0002] Silicalite-2 is a molecular sieve with a MEL-type framework structure, and is the all-silicon form of ZSM-11. It can be used as an inert carrier for shape-selective catalysts and a separation membrane material for organic aqueous phases, and has received extensive attention. [0003] In early 1973, Chu P (USP3709979) used Bu 4 N + As a template agent, the ZSM-11 molecular sieve was successfully synthesized. In 1978, Flanigen E M of U.C.C. Company successfully synthesized the last member of the Pentasil family, all-silicon ZSM-11-Silicalite-2, which in turn promoted the rapid development of the field of silicon-rich molecular sieve synthesis. develop. In 1990, McWilliam (USP4894212) used octylamine as a template and crystall...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08
Inventor 耿晨晨秦波张喜文凌凤香王诗语
Owner CHINA PETROLEUM & CHEM CORP