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Method for synthesizing integrated SSZ-13 molecular sieve from mixed template agent and dry glue

A hybrid template agent, dry glue synthesis technology, applied in the direction of molecular sieve catalysts, including molecular sieve catalysts, molecular sieves and alkali exchange compounds, etc., can solve the problems of reduced catalytic efficiency, dust pollution, blocked pores, etc., to reduce the use of solvent water, The effect of less water consumption and reduced raw material waste

Inactive Publication Date: 2019-02-12
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the handling and processing of powder samples can easily cause dust pollution and product waste, and the addition of binders during molding may block the pores or cover the active sites of molecular sieves, resulting in a decrease in catalytic efficiency. The monolithic crystallized SSZ-13 molecular sieve has so far No patent report

Method used

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  • Method for synthesizing integrated SSZ-13 molecular sieve from mixed template agent and dry glue
  • Method for synthesizing integrated SSZ-13 molecular sieve from mixed template agent and dry glue
  • Method for synthesizing integrated SSZ-13 molecular sieve from mixed template agent and dry glue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) 188g of white carbon black and 25g of sodium metaaluminate were mixed and fully ground at room temperature;

[0033] (2) At room temperature, in a small beaker, successively add 263g of water, 150g of N,N,N-trimethyladamantane ammonium (content is 25%) and 50g of choline chloride, stir until choline chloride The base is completely dissolved in the N,N,N-trimethyladamantyl ammonium solution;

[0034] (3) Add the completely dissolved and transparent solution into the uniformly ground solid raw material, fully knead for 2 hours with a kneader, and shape it with a cylindrical extruded slat;

[0035] (4) Put the molded raw material dry glue strip into a polytetrafluoroethylene tray, and place it in a polytetrafluoroethylene-lined high-pressure reactor with a small amount of water. After sealing, crystallize at 160 ° C for 2 days to obtain Na-SSZ-13 molecular sieve;

[0036] (5) After the reactor is cooled to room temperature, it is washed and dried with deionized water...

Embodiment 2

[0051] (1) 188g of white carbon black, 18g of anhydrous aluminum sulfate and 23g of sodium metaaluminate are mixed and fully ground at room temperature;

[0052] (2) At room temperature, in a small beaker, successively add 263g of water, 150g of N,N,N-trimethyladamantane ammonium (content is 25%) and 50g of choline chloride, stir until choline chloride The base is completely dissolved in the N,N,N-trimethyladamantyl ammonium solution;

[0053] (3) Add the completely dissolved and transparent solution into the uniformly ground solid raw material, fully knead for 2 hours with a kneader, and shape it with a cylindrical extruded slat;

[0054] (4) Put the molded raw material dry glue strip into a polytetrafluoroethylene tray, and place it in a polytetrafluoroethylene-lined high-pressure reactor with a small amount of water. After sealing, crystallize at 160 ° C for 2 days to obtain Na-SSZ-13 molecular sieve;

[0055] (5) After the reactor is cooled to room temperature, it is was...

Embodiment 3

[0060] (1) 188g of white carbon black, 50g of anhydrous aluminum sulfate and 23g of sodium metaaluminate are mixed and fully ground at room temperature;

[0061] (2) At room temperature, in a small beaker, successively add 263g of water, 150g of N,N,N-trimethyladamantane ammonium (content is 25%) and 50g of choline chloride, stir until choline chloride The base is completely dissolved in the N,N,N-trimethyladamantyl ammonium solution;

[0062] (3) Add the completely dissolved and transparent solution into the uniformly ground solid raw material, fully knead for 2 hours with a kneader, and shape it with a cylindrical extruded slat;

[0063] (4) Put the molded raw material dry glue strip into a polytetrafluoroethylene tray, and place it in a polytetrafluoroethylene-lined high-pressure reactor with a small amount of water. After sealing, crystallize at 160 ° C for 2 days to obtain Na-SSZ-13 molecular sieve;

[0064] (5) After the reactor is cooled to room temperature, it is was...

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Abstract

The invention discloses a method for synthesizing an integrated SSZ-13 molecular sieve from a mixed template agent and dry glue. According to the method disclosed by the invention, the mixed templateagent mainly adopts choline chloride and N,N,N-trimethyl adamantine ammonium, the mixed template agents and raw materials are kneaded, extruded and preformed according to the proportion, and then dryglue stripes are crystallized under the certain temperature in a high pressure kettle; the prepared SSZ-13 molecular sieve has the advantages of high purity, pure crystal phase, even grain size, moreconcentrated accumulation bore diameter, larger specific surface area and appropriate acid sites. The SSZ-13 molecular sieve synthesized by the method disclosed by the invention has high heat stability, has more concentrated accumulation holes near 4 nm and has a very excellent catalyzing effect in catalytic reaction of MTO methanol to olefin. Compared with hydrothermal synthesis and a traditionaldry glue and solid phase grinding method, an integrated type dry glue synthesizing process has the characteristics that dust pollution and raw material waste in cost powder processing are reduced, the cost is low, the water use amount is small, a preparation process is simple and easy to operate, no adhesive is added, active sites are exposed, a catalytic effect is strong and the like.

Description

technical field [0001] The invention belongs to the field of catalyst carrier preparation, and in particular relates to a synthesis method of monolithic SSZ-13 molecular sieves. Background technique [0002] SSZ-13 molecular sieve is a CHA structure with small pores and large cages of chabazite, composed of AlO 4 and SiO 4 The tetrahedrons are connected end to end through oxygen atoms, arranged in an orderly manner into an ellipsoid (0.73nm×1.2nm) crystal with an eight-membered ring structure, and all three-dimensional intersecting channels are small-pore molecular sieves with a size of 0.38nm×0.38nm. The molecular sieve has excellent catalytic performance for the reaction of producing low-carbon olefins (MTO) from methanol due to its regular pore structure and medium-strength acidity. [0003] In the 1980s and 1990s, Zones successfully synthesized high-purity SSZ-13 molecular sieves (US No. 4,544,538) using the hydrothermal method for the first time, using N,N,N-trimethyl...

Claims

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Application Information

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IPC IPC(8): C01B39/48B01J29/70C07C11/04C07C11/06C07C1/20
CPCB01J29/7015C01B39/026C01B39/48C01P2002/72C01P2004/03C01P2004/38C01P2004/62C07C1/20C07C2529/70C07C11/04C07C11/06Y02P20/52Y02P30/20Y02P30/40
Inventor 冯晴于海斌孙彦民曾贤君张利杰李荣军李贺裴仁彦
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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