Method for preparing L-zeolite by in-situ crystallization

A technology of in-situ crystallization and zeolite, applied in the direction of crystalline aluminosilicate zeolite, L-type crystalline aluminosilicate zeolite, etc., can solve problems such as difficult to control accurately

Active Publication Date: 2013-07-31
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, it is necessary to dry and adjust the water content of the extrudate, which is difficult to accurately control in actual operation

Method used

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  • Method for preparing L-zeolite by in-situ crystallization
  • Method for preparing L-zeolite by in-situ crystallization
  • Method for preparing L-zeolite by in-situ crystallization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Get 140 grams (dry basis) of industrial coarse-porous silica gel, 10 grams of sage powder and join 200 grams of acidic silica sol (SiO 2 content 30%), stir evenly, add ammonia water to adjust the pH value to 6, knead on the kneader for 15 minutes, extrude on the extruder, cut into strips after health preservation and drying, the diameter of the strips is 2 to 3 mm, and the length is 3 mm. ~6 mm. This bar is named T1. T1 was fired at 450°C for 5 hours, 750°C for 2 hours and 850°C for 1 hour to obtain preforms T1-450, T1-750 and T1-850.

Embodiment 2

[0022] Get 180 grams (dry basis) of white carbon black, 10 grams of L zeolite (dry basis) and join in 200 grams of alkaline silica sol (SiO 2 content 30%), stir evenly, add nitric acid to adjust the pH value to 8, knead on the kneader for 15 minutes, extrude on the extruder, cut into strips after curing and drying, the diameter of the strips is 2 to 3 mm, and the length is 3 mm. ~6 mm. This bar is named T2. T2 was fired at 550°C for 6 hours and 650°C for 4 hours to obtain preforms T2-550 and T2-650.

Embodiment 3

[0024] Get 10 grams of sodium aluminate (analytically pure, Al 2 o 3 content 45%), 10.3 grams of potassium hydroxide (analytically pure, KOH content 96%), added to 23.8 grams of deionized water, dissolved transparently, added 10 grams of preform T1-750, stirred evenly, and transferred to the autoclave , crystallized at 170°C for 10 hours after sealing. The product was filtered, washed, and dried. XRD analysis showed that the product was a pure phase L zeolite. In this embodiment, the weight ratio of the crystallization liquid to the preform is 4.4, and in the crystallization liquid, KOH / Al 2 o 3 (molar ratio) is 4, H 2 O / Al 2 o 3 (Molar ratio) was 30.

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Abstract

The invention relates to a preparation method of L-zeolite. The preparation method comprises the following steps of: uniformly mixing solid silicon dioxide with silica sol, regulating the pH value of a system to 7-8, then forming, drying and calcining at the temperature of 300-900 DEG C for 1-6 hours to get a pre-formed body; adding solid sodium aluminate and potassium hydroxide into deionized water, and stirring till a solution is transparent to get a crystallized solution, wherein the molar ratio of KOH / AL2O3 is 1-20, and the molar ratio of H2O / Al2O3 is 10-120; adding the prepared pre-formed body into the crystallized solution, wherein the weight ratio of the crystallized solution to the pre-formed body is 2-10; and uniformly mixing, then performing hydrothermal crystallization for 6-24hours at the temperature of 100-180 DEG C, filtering, washing, and drying to get the in-situ crystallized L-zeolite. The crystallized L-zeolite has higher relative degree of crystallization and larger pore volume of mesopores, the pore diameter of the mesopores is 5-10nm, and an n-alkane aromatization catalyst prepared by taking the L-zeolite as a carrier has higher yield of arene.

Description

technical field [0001] The invention relates to a preparation method of L zeolite. More specifically, the present invention relates to a preparation method of in-situ crystallization of L zeolite on a preformed carrier, and the crystallized product can be directly used as a catalyst carrier. Background technique [0002] CN 85 103013 discloses a method for synthesizing L-type zeolite by directing agent method, the crystallization method is non-situ crystallization. [0003] CN 200810154213 discloses a method for synthesizing small-grain L-type zeolite, the crystallization method of which is non-situ crystallization. [0004] CN 200710054290 discloses a method for synthesizing L zeolite. Kaolin is roasted to obtain high soil and partial soil. After mixing the two roasted soils in a certain proportion, white carbon black, guiding agent or crystal seed, potassium hydroxide solution, distilled water are added. Crystallize at 100-130°C for 18-24 hours, filter, wash and dry to o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/32
Inventor 潘晖华马怀军阎立军马安田志坚
Owner PETROCHINA CO LTD
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