Preparation method of appearance-controllable L zeolite

A zeolite and morphology technology, applied in the field of molecular sieve materials and their preparation, can solve the problems of inability to control the morphology of modified molecular sieves, single molecular sieves in morphology, low crystallinity, etc., and achieves controllable morphology, reduced production costs, and improved crystallization. high degree of effect

Inactive Publication Date: 2018-06-01
CNOOC TIANJIN CHEM RES & DESIGN INST +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] CN200810154213 uses silica sol as a silicon source, potassium metaaluminate as an aluminum source, and adds a quantitative directing agent during the synthesis process to obtain L zeolite with a particle size of 200-300nm, but there is a problem of relatively low crystal

Method used

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  • Preparation method of appearance-controllable L zeolite
  • Preparation method of appearance-controllable L zeolite
  • Preparation method of appearance-controllable L zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] At room temperature, 32.9g potassium metaaluminate solution (Al 2 o 3 The content is 4.2wt%, K 2 O content is 23.6%) solution is dissolved in 13.2g deionized water, adds 30g silica sol (SiO 2 Content is 30wt%), after mixing evenly, continue to stir for 2h, and then stand and age at 15°C for 24h to prepare the directing agent.

[0035] At 25°C, 225g of potassium metaaluminate solution (Al 2 o 3 Content is 4.5wt%, K 2 The O content is 33.2%) was dissolved in 50 g of deionized water, 400 g of silica sol was added under mechanical stirring, and the stirring was continued to make it completely mixed to obtain the initial L zeolite gel. In the state of stirring, pour the directing agent prepared above into the initial gel, mix evenly, then add 2.4g of ammonium fluorosilicate solid, after stirring for 1 hour, put the obtained silica-alumina gel into the polytetrafluoroethylene liner In a stainless steel crystallization kettle, the temperature was raised to 30°C for cryst...

Embodiment 2

[0037] Each raw material source is with embodiment 1.

[0038] At room temperature, dissolve 7.64g KOH in 24.5g water, heat to 70°C, then add 1.2g Al(OH) 3 , boil the mixed solution until the aluminum hydroxide is completely dissolved, then cool to room temperature, add 6.5g white carbon black (SiO 2 Content is 92wt%), after mixing evenly, continue to stir for 2h, and then stand and age at 25°C for 24h to prepare the directing agent.

[0039] At 25°C, dissolve 10g of NaOH and 16g of KOH in 101g of water, heat to 70°C, and then add 5.67g of Al(OH) 3 , boil the mixed solution until the aluminum hydroxide is completely dissolved, then cool to room temperature, add 87g of white carbon black under mechanical stirring, continue to stir, make it completely mixed, and obtain the initial L zeolite gel. In the state of stirring, pour the directing agent prepared above into the initial gel, mix evenly, then add 0.11g of magnesium fluoride solid, and after stirring for 1 hour, put the o...

Embodiment 3

[0041]Each raw material source is with embodiment 1.

[0042] At room temperature, dissolve 17.1g KOH in 24.5g water, heat to 70°C, then add 1.18g Al 2 o 3 , boil the mixed solution until the alumina is completely dissolved, then cool to room temperature, add 40g of silica sol (SiO 2 Content is 30wt%), after mixing evenly, continue to stir for 2h, and then stand and age at 50°C for 36h to prepare the directing agent.

[0043] At 25°C, dissolve 200g KOH in 1152g water, heat to 80°C, then add 8.16g Al 2 o 3 , boil the mixed solution until the aluminum hydroxide is completely dissolved, then cool to room temperature, add 240g of silica gel under mechanical stirring, continue to stir, make it completely mixed, and obtain the initial L zeolite gel. In the state of stirring, pour the directing agent prepared above into the initial gel, mix well, then add 1.42g of ammonium fluorosilicate solid, after stirring for 1 hour, put the obtained silica-alumina gel into the polytetrafluor...

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Abstract

The invention discloses a preparation method of appearance-controllable L zeolite. The method uses villaumite as an additive; a synthesis method of L zeolite appearance regulation through sectioned crystallization is used. The method comprises the concrete steps of mixing a silicon source with an aluminum source; performing static aging at 5 to 60 DEG C for 2 to 72 hours to obtain a guiding agent;then, mixing the silicon source, the guiding agent, the aluminum source and villaumite to obtain glue, wherein the mole ratio of all ingredients in the reaction mixture gel is 8 to 20K2O:Al2O3:20 to60SiO2:120 to 800H2O: 0.03 to 0.3F<->; then, performing two-stage static crystallization at different temperatures, wherein the first-stage crystallization temperature is 5 to 60 DEG C, and the firststage crystallization time is 12 to 48 hours; the second stage crystallization temperature is 120 to 180 DEG C, and the second stage crystallization time is 12 to 72 hours; finally, performing filtering, washing and drying to obtain an L zeolite molecular sieve. The obtained molecular sieve has high relative crystallinity degree; the appearance is in a particle shape, a round cake shape and a double-cone shape. The preparation method has the advantages that the raw materials can be easily obtained; the preparation cost is low; good industrial application prospects are realized.

Description

technical field [0001] The invention belongs to the field of molecular sieve materials and preparation thereof, in particular to a method for preparing L zeolites with different shapes. Background technique [0002] L zeolite is a kind of artificial synthetic zeolite, it has unique adsorption performance and catalytic performance, and also has good thermal stability. It is a kind of catalytic material with excellent thermal stability, which can be used to prepare Catalysts for hydrocarbon conversion processes such as structuring and alkylation. The skeleton structure of L zeolite is composed of cannonite cages and double six-membered rings. It was first synthesized by Breck and Flanigen in 1965. Subsequently, people have carried out a lot of research on the synthesis of L zeolite. Usually, L zeolite can use silica sol, white carbon black or water glass as a silicon source, potassium metaaluminate or sodium metaaluminate as an aluminum source, and potassium hydroxide and hydr...

Claims

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Application Information

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IPC IPC(8): C01B39/32
CPCC01B39/32C01P2002/72C01P2004/03
Inventor 洪鲁伟刘冠锋于海斌臧甲忠赵云王银斌郭春垒宋万仓王凌涛洪美花季超
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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