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Green preparation method of sodium chabazite with through stepped holes

A technology of gmelinite and stepped pores, which is applied in the field of green preparation of gmelinite, can solve the problems of structural damage of the template agent, inability to recycle, cumbersome template removal methods, etc., and achieve the goal of avoiding damage and realizing recycling Effect

Active Publication Date: 2021-04-02
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN104445264B discloses that polyethylene glycol is used as a template to synthesize gmelinite under the action of fluoride, and the addition of toxic fluorine-containing substances causes the above synthesis process to be a non-green synthesis process, and the gmelinite synthesized above all shows a certain degree of Stacking faults, dabco-GME also showed micropore volume (N 2 Adsorption) is only 0.055cm3.g -1
[0003] The template agent used in the synthesis process of the above gmelinite is non-green ammonium or fluorine-containing substances. The removal method of the template agent is cumbersome and the structure of the template agent is destroyed, so it cannot be recycled.
In addition, there is no report on the synthesis of gmelinite through micro-meso-large stepped pores.

Method used

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  • Green preparation method of sodium chabazite with through stepped holes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 0.363g NaAlO 2 Add 0.67g of CK-2 to 0.374g of 50% NaOH aqueous solution, add 2.42g of water and stir until clear, add 2.5g of Ludox-AS 40, and the molar ratio of the feed meets: 10SiO 2 / Al 2 o 3 / 2Na 2 O / 140H 2 O / 0.01CK-2, aged at 25°C for 48h, transferred the gel to a stainless steel reactor with a polytetrafluoroethylene liner and placed it in a homogeneous reactor at 110°C for crystallization for 15d, after the product was centrifuged and washed, Dry at 100°C to obtain a solid sample. Weigh 0.2 g of the above sample and add it to 10 mL of chloroform, stir at 60°C for 4 hours, extract and remove CK-2, centrifuge the obtained product, wash thoroughly with deionized water, and dry in an oven at 110°C.

[0025] The preparation process of CK-2 used in this example is as follows: 1,4-cyclohexanedimethanol (69.4mmol) and ethylene glycol (17.34mmol) were dissolved in 60mL freshly distilled cyclohexane, and added to 100mL strip distilled In the first three-necked flask...

Embodiment 2

[0028] The order of adding raw materials is the same as in Example 1, using sodium metaaluminate and aluminum sulfate as the aluminum source, and tetraethyl orthosilicate as the silicon source, and adjusting the addition amount so that the molar ratio of the feeding material satisfies: 15SiO 2 / Al 2 o 3 / 2Na 2 O / 140H 2 O / 0.01CK-2, aged at 25°C for 96h, transferred the gel to a stainless steel reactor with a polytetrafluoroethylene liner and placed it in a homogeneous reactor at 100°C for crystallization for 20d, after the product was centrifuged and washed, Dry at 100°C to obtain a solid sample. Weigh 0.2 g of the above sample and add it to 10 mL of n-hexane, stir at 50°C for 12 hours, extract and remove CK-2, centrifuge the obtained product, wash thoroughly with deionized water, and dry in an oven at 110°C.

[0029] The phase of the obtained product as determined by XRD belongs to gmelinite, and the specific surface area is 380m 2 / g, the pore volume is 0.22cm 3 / g, the...

Embodiment 3

[0031]The order of adding raw materials is the same as in Example 1, using aluminum sulfate as the aluminum source, silica sol and white carbon black as the silicon source, and adjusting the addition amount so that the molar ratio of the feed is satisfied: 6SiO 2 / Al 2 o 3 / 2Na 2 O / 140H 2 O / 0.01CK-2, aged at 25°C for 60h, transferred the gel to a stainless steel reactor with a polytetrafluoroethylene liner and placed it in a homogeneous reactor at 120°C for crystallization for 10d, after the product was centrifuged and washed, Dry at 100°C to obtain a solid sample. Weigh 0.2 g of the above sample and add it to 10 mL of n-hexane, stir at 80°C for 4 hours, extract and remove CK-2, centrifuge the obtained product, wash thoroughly with deionized water, and dry in an oven at 110°C.

[0032] The phase of the obtained product as determined by XRD belongs to gmelinite, and the specific surface area is 400m 2 / g, the pore volume is 0.18cm 3 / g, the pore size distribution is aroun...

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Abstract

The invention relates to a green preparation method of sodium chabazite with through stepped holes, and the method comprises the following steps: uniformly mixing a neutral copolymer, deionized water,an aluminum source, an alkali source and a silicon source according to a certain proportion, carrying out hydrothermal crystallization, centrifuging the obtained product, performing drying, performing extracting to remove a template agent, and obtaining the sodium chabazite with through stepped holes. According to the method, the structural characteristics of the sodium chabazite are completely reserved, and the template agent can be recycled, so the method is a green preparation method. The sodium chabazite prepared by the method has the advantages of penetrating through the stepped hole zeolite, being high in specific surface area and pore volume and the like, and is beneficial to selective adsorption and mass transfer application of macromolecules.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve synthesis, and in particular relates to a green preparation method of gmelinite with through-step holes. Background technique [0002] Gmelinite is a large-pore zeolite with a 12×8×8 three-dimensional pore structure, however, both natural and synthetic gmelinite behave like small-pore zeolites in terms of adsorption properties, and this behavior can be attributed to the Stacking faults of zeolites (CHA intergrowth). As can be observed by X-ray diffraction, stacking faults block or limit the main channels of gmelinite, thereby limiting porosity, a property that hinders the development of gmelinite for catalytic research and other applications. In 1977, Mobil synthesized dabco-GME zeolite using the cationic polymer dabco as an organic structure-directing agent (Journal of the American Chemical Society, 1977, 100, 3097-3100). Later, Chiyoda and Davis reported thermal conversion of Y zeolite...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04C08G65/34
CPCC01B39/04C08G65/34C01P2002/72C01P2004/03C01P2004/04C01P2006/17
Inventor 岳源源胡元鲍晓军王婵王廷海朱海波
Owner FUZHOU UNIV
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