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A kind of preparation method of high crystallinity sapo-11 molecular sieve

A technology of SAPO-11 and molecular sieves, applied in the field of synthesis of SAPO-11 molecular sieves

Active Publication Date: 2018-06-29
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the current literature reports, almost all industrially produced boehmite with large particles and high crystallinity is used as the aluminum source, and very few use nano-flaky boehmite as the aluminum source.

Method used

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  • A kind of preparation method of high crystallinity sapo-11 molecular sieve
  • A kind of preparation method of high crystallinity sapo-11 molecular sieve
  • A kind of preparation method of high crystallinity sapo-11 molecular sieve

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Embodiment 1

[0023] 1. Preparation of silicon-containing pseudo-boehmite: Weigh 22.56g of sodium hydroxide, 9.78g of gibbsite, and 67.66g of deionized water, stir evenly, and react at 120°C for 5h to prepare a sodium metaaluminate solution with Na / Al=4.5 . Weigh 233.24 g of aluminum sulfate octadecahydrate, add deionized water to dissolve, and prepare an aluminum sulfate solution with a concentration of 0.7 mol / L. Under room temperature and stirring conditions, weigh 25g of aluminum sulfate solution, and add sodium metaaluminate solution dropwise until pH = 10.0, using this as the base solution, and add sodium metaaluminate solution and aluminum sulfate dropwise to it at the same time Solution and water glass, keep system pH=9.5 in this process, add dropwise 75g aluminum sulfate solution in total at last, 4.68g water glass (Catalyst Changling branch company, silicon oxide 27.426%, sodium oxide 8.76%), obtain after dropping complete white suspension. The obtained homogeneous white suspens...

Embodiment 2

[0026] Implementation process except the following difference, all the other are the same as embodiment 1: in the formed gel, silicon-containing pseudo-boehmite is replaced by SiO 2 In terms of phosphoric acid in P 2 o 5 Calculated, the molar ratio to template agent di-n-propylamine and water is 0.14:1:1.75:55. Get the spectrogram and the XRD of product SAPO-11 molecular sieve figure 1 Similar to a in middle, it can be seen from SEM that its shape is a rectangular plate with a size of 10 μm.

Embodiment 3

[0028] Implementation process except the following difference, all the other are the same as embodiment 1: in the formed gel, silicon-containing pseudo-boehmite is replaced by SiO 2 In terms of phosphoric acid in P 2 o 5 The molar ratio of template agent di-n-propylamine and water is 0.14:1:2:55. Get the spectrogram and the XRD of product SAPO-11 molecular sieve figure 1 Similar to a in middle, it can be seen from SEM that its shape is hemispherical with a hole in the middle.

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Abstract

The invention discloses a method for preparing an SAPO-11 molecular sieve with high crystallinity. The method comprises the following steps: mixing nano lamelliform silicon-containing pseudo-boehmite with large specific surface area and large pore volume, phosphoric acid, an organic template agent and water so as to obtain a mixture, transferring the mixture into a polytetrafluoroethylene reaction kettle, implementing hydrothermal reaction, filtering, washing, drying and roasting, and obtaining the SAPO-11 molecular sieve with large specific surface area and high crystallinity. According to the method, the nano lamelliform silicon-containing pseudo-boehmite with the large specific surface area and the large pore volume is taken as an aluminum source, the lamella thickness is only 8, and relatively rich aluminum hydroxyl is accumulated on the surface, so that relatively rich active sites can be generated to promote generation of Al-O-P, and the reaction can be implemented under relatively gentle conditions; as silicon is introduced into the aluminum source to form framework silicon, the problem that the crystallinity of the molecular sieve is affected by amorphous phase of free silicon which is hard to enter framework can be solved.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve synthesis, in particular to a method for synthesizing SAPO-11 molecular sieves. Background technique [0002] SAPO-11 molecular sieve is a mesoporous silicoaluminophosphate molecular sieve with AEL topological structure. It has one-dimensional straight channels and ten-membered ring elliptical channels. The channel size is 0.39nm×0.64nm. It belongs to the orthorhombic crystal system. The unit cell parameters A = 1.34nm, b = 1.87nm, c = 0.84nm, SAPO-11 molecular sieve is suitable for catalytic hydrocracking, isomerization, alkylation and light olefins due to its suitable pore structure and size and relatively mild acidity. It has broad application prospects in various oil refining and chemical industries such as polymerization. [0003] Since SAPO-11 is an aluminum-rich molecular sieve, the type of aluminum source has an important influence on the synthesis of the molecular sieve. The ear...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/08
CPCC01B37/08C01B39/54C01P2002/72C01P2004/03C01P2006/12C01P2006/90
Inventor 宋家庆邬勇焦琨徐向宇吕志
Owner BEIJING UNIV OF CHEM TECH
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