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Method for synthesizing morphology-controllable SSZ-13 molecular sieves

A synthetic method and technology of molecular sieves, applied in the field of molecular sieves

Active Publication Date: 2019-04-23
CHIA TAI ENERGY MATERIALS DALIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on the preparation of SSZ-13 molecular sieves with different morphologies.

Method used

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  • Method for synthesizing morphology-controllable SSZ-13 molecular sieves
  • Method for synthesizing morphology-controllable SSZ-13 molecular sieves
  • Method for synthesizing morphology-controllable SSZ-13 molecular sieves

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Experimental program
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Effect test

Embodiment 1

[0032] Such as figure 1 , Figure 5 Shown, a kind of synthetic method of controllable shape SSZ-13 molecular sieve, according to alkaline solution (with Na 2 O): Raw material aluminum (as Al 2 o 3 Calculated): Accelerator: Raw silicon (as SiO 2 Count): H 2 The molar ratio of O: template agent is 12:3:3:110:4500:20 to prepare the reaction liquid. Take a certain amount of 3%wt NaOH solution, 25%wt N,N,N-trimethyl-1-adamantyl ammonium hydroxide and water into the beaker, stir evenly; then add pseudo-boehmite and triethanolamine , stirred for 3 hours; then added silica sol, stirred for 1 hour; the reaction solution was put into a high-pressure reactor, and hydrothermally crystallized at 160° C. for 4 days. Then filter and wash until the filtrate is neutral, dry at 140°C for 4 hours, and roast at 550°C for 6 hours to obtain SSZ-13 molecular sieve. XRD shows SSZ-13 molecular sieve (see figure 1 ), SEM showed regular cubic morphology crystals (see Figure 5 , A).

Embodiment 2

[0034] Such as figure 2 , Figure 5 Shown, a kind of synthetic method of controllable shape SSZ-13 molecular sieve, according to alkaline solution (with Na 2 O): Raw material aluminum (as Al 2 o 3 Calculated): Accelerator: Raw silicon (as SiO 2 Count): H 2 The molar ratio of O: template agent is 15:2:4:100:3500:15 to prepare the reaction solution. Take a certain amount of 20%wt NaOH solution, 25% N,N,N-trimethyl-1-adamantyl ammonium hydroxide and water into the beaker, stir evenly; then add pseudo-boehmite and tetraethylene penta Amine, stirred for 3 hours; white carbon black was added, stirred for 2 hours; the reaction solution was put into a high-pressure reactor, and hydrothermally crystallized at 180°C for 4 days. Then filter and wash until the filtrate is neutral, dry at 140°C for 4 hours, and roast at 550°C for 6 hours to obtain SSZ-13 molecular sieve. XRD shows SSZ-13 molecular sieve (see figure 2 ), SEM showed multi-folded cubic-like crystals (see Figure 5 ...

Embodiment 3

[0036] Such as image 3 , Figure 5 Shown, a kind of synthetic method of controllable shape SSZ-13 molecular sieve, according to alkaline solution (with Na 2 O): Raw material aluminum (as Al 2 o 3 Calculated): Accelerator: Raw silicon (as SiO 2 Count): H 2 The molar ratio of O: template agent is 10:3:3:110:4500:20 to prepare the reaction liquid. Take a certain amount of 3%wt NaOH solution, 25% N,N,N-trimethyl-1-adamantyl ammonium hydroxide and water into the beaker, stir evenly; then add sodium metaaluminate and cysteine acid, and stirred for 1 hour; then added white carbon black, and stirred for 2 hours; the reaction liquid was put into a high-pressure reactor, and hydrothermally crystallized at 160° C. for 4 days. Then filter and wash until the filtrate is neutral, dry at 140°C for 4 hours, and roast at 550°C for 6 hours to obtain SSZ-13 molecular sieve. XRD shows SSZ-13 molecular sieve (see image 3 ), SEM showed spherical crystals (see Figure 5 , C).

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Abstract

The invention discloses a method for synthesizing morphology-controllable SSZ-13 molecular sieves. The method includes steps of S01, mixing alkali solution with certain concentration, template agentsand water with one another, and uniformly stirring the alkali solution, the template agents and the water; S02, adding a raw material aluminum and accelerators into solution obtained at the step S01,and stirring the raw material aluminum, the accelerators and the solution at the room temperature for a certain time; S03, adding a raw material silicon into solution obtained at the step S02 and stirring the raw material silicon and the solution for a certain time; S04, filling reaction kettles with solution obtained at the step S03, and hydrothermally crystallizing the solution at certain temperatures for a certain time; S05, carrying out filtration washing, drying and calcination on hydrothermally crystallized reaction products to obtain the morphology-controllable SSZ-13 molecular sieves.The method has the advantages that combinations of synthesis raw materials and the accelerators are controlled, so that the SSZ-13 molecular sieves with different types of morphology can be prepared by the aid of the method, and the method includes simple processes.

Description

technical field [0001] The invention relates to a method for synthesizing SSZ-13 molecular sieves with controllable morphology, belonging to the technical field of molecular sieves. Background technique [0002] In the 1980s, Zones synthesized the molecular sieve SSZ-13 for the first time by hydrothermal method. The SSZ-13 molecular sieve has a chabazite (CHA) structure and is composed of SiO 4 and AlO 4 The tetrahedra are joined end to end by oxygen atoms. The regular arrangement is eight-membered ring channel and three-dimensional cross channel structure. The pore size is 0.38nm×0.38nm, which belongs to small and medium pore molecular sieves classified as zeolite molecular sieves. The structural characteristics of SSZ-13 endow it with good acidity tunability and ion exchange properties, as well as excellent hydrothermal stability. Therefore, it is widely used in aromatics structure reaction, methanol to low carbon olefins (MTO), automobile exhaust absorption and CO 2 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48
CPCC01B39/48C01P2002/72
Inventor 程鸿魁周彤郝伟李元东王闯袁龙姜叶葳
Owner CHIA TAI ENERGY MATERIALS DALIAN