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Method for synthesizing SAPO-34 molecular sieve by using hectorite

A technology of SAPO-34 and laponite, which is applied in the production of molecular sieves and alkali-exchanged phosphates, molecular sieve-specific silicoaluminophosphates, and bulk chemicals, can solve problems such as crystal structure damage, achieve short synthesis cycles, and improve production efficiency effect

Active Publication Date: 2019-11-15
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above method, high-temperature calcination, alkali fusion, and acid-base activation are used to treat clay minerals. The crystal structure of clay minerals is destroyed, and only part of the silicon source is used. In addition, high-temperature calcination and acid-base treatment produce a large amount of waste liquid and energy consumption.

Method used

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  • Method for synthesizing SAPO-34 molecular sieve by using hectorite
  • Method for synthesizing SAPO-34 molecular sieve by using hectorite
  • Method for synthesizing SAPO-34 molecular sieve by using hectorite

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Add 5.2g of morpholine to 15.5g of water to disperse evenly, add 8.16g of aluminum isopropoxide, stir magnetically at room temperature for 2h, take 3.92g of phosphoric acid and continue stirring for 1h, and finally add 14.5g of hectorite with a mass fraction of 8% to disperse The solution was stirred for 3 hours to obtain a mixed material, and then the mixed material was transferred to a stainless steel reactor with a polytetrafluoroethylene liner, crystallized at 180°C for 9 hours under hydrothermal conditions, cooled to room temperature, and centrifugally washed until neutral. After drying in an oven for 12 hours, the product was calcined in a muffle furnace at 550ºC for 6 hours, and the product obtained was SAPO-34 molecular sieve. Such as Figure 6 As shown, after XRD characterization, the sample is SAPO-34 zeolite molecular sieve. Such as image 3 As shown, it can be seen that the overall shape of the sample is a cube, and the particle size is 10 μm.

Embodiment 2

[0037] Add 5.2g of morpholine to 15.5g of water and disperse evenly, add 8.16g of aluminum isopropoxide and stir magnetically at room temperature for 2 hours, take 3.92g of phosphoric acid and continue stirring for 1 hour, and finally add 14.5g of hectorite dispersion with a mass fraction of 8%. Stir for 3 hours to obtain the mixed material, then transfer the mixed material to a stainless steel reactor with a polytetrafluoroethylene liner, crystallize at 180ºC for 18 hours under hydrothermal conditions, cool to room temperature, and centrifugally wash until neutral. The product was dried for 12 hours in a muffle furnace at 550ºC for 6 hours to obtain a SAPO-34 molecular sieve.

[0038] Such as Figure 4As shown, the molecular sieve prepared in this example is analyzed as a molecular sieve by XRD (X-ray diffraction), has a typical CHA topology, and the purity and quality of the sample are high. Such as Figure 5 The SEM (scanning electron microscope) picture shown shows that ...

Embodiment 3

[0040] Add 5.2g of morpholine to 15.5g of water and disperse evenly, add 8.16g of aluminum isopropoxide and stir magnetically at room temperature for 2 hours, take 3.92g of phosphoric acid and continue stirring for 1 hour, and finally add 14.5g of hectorite dispersion with a mass fraction of 8%. Stir for 3 hours to obtain the mixed material, then transfer the mixed material to a stainless steel reactor with a polytetrafluoroethylene liner, age for 24 hours, crystallize at 180ºC for 36 hours under hydrothermal conditions, cool to room temperature, and centrifugally wash until neutral, the obtained solid Dry in an oven at 100ºC for 12h, and calcinate the product in a muffle furnace at 550ºC for 6h to obtain SAPO-34 molecular sieve. Such as Figure 6 As shown, the molecular sieve prepared in this embodiment is analyzed as SAPO-34 molecular sieve by XRD (X-ray diffraction), which has a typical CHA topological structure, and the purity and quality of the sample are relatively high....

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Abstract

The invention provides a method for synthesizing SAPO-34 molecular sieve by using hectorite. The method comprises the following steps that (1), hectorite nanoparticles are swelled by using deionized water and dispersed to prepare a hectorite dispersing liquid; (2), an organic structure-directing agent, an aluminium source and a phosphorus source are added to water for mixing and stirring in sequence, the hectorite dispersing liquid prepared in the step (1) is used as a silica source to be added, and stirring continues to be conducted to obtain initial gel is obtained; (3), the initial gel prepared in the step (2) is added to a reaction kettle for hydrothermal crystallization, and cooled to room temperature to obtain original molecular sieve powder, the original molecular sieve powder is washed to be neutral, placed in a drying oven for drying, and finally calcined in a muffle furnace to obtain the SAPO-34 molecular sieve. In the method, all the silica source is provided by the hectorite, neither calcination nor alkali treatment of the hectorite is needed, it is achieved that the zeolite molecular sieve is directly synthesized by using clay minerals, and the synthesizing period is short. The method expands the range of synthetic raw materials for the molecular sieve, and the additive value of a hectorite product is increased.

Description

technical field [0001] The invention relates to the field of molecular sieve preparation, in particular to a method for synthesizing SAPO-34 molecular sieves by using laponite as a raw material to provide all silicon sources required for synthesizing SAPO-34. Background technique [0002] Zeolite molecular sieve, as a porous crystal catalytic material, has unique molecular shape-selective properties, excellent catalytic performance and high hydrothermal stability, and is widely used in the field of petrochemical industry. The silicoaluminophosphate molecular sieve SAPO-34 with CHA topology exhibits excellent catalytic performance in the methanol-to-olefins (MTO) reaction and has attracted widespread attention in the field of industrial catalysis. [0003] Hectorite belongs to the 2:1 structure, expandable hydrous layered silicate, and its structure is composed of two layers of silicon-oxygen tetrahedron sandwiching a layer of magnesium-oxygen octahedron, and part of the magn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
CPCC01B37/08C01B39/54Y02P30/40
Inventor 蒋荣立陈学帅周子涵王兴文
Owner CHINA UNIV OF MINING & TECH
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