Method for preparing ZSM-5 zeolite/clay composite catalytic material without amine

A technology of ZSM-5 and catalytic materials, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of polluting the environment and increasing the cost of zeolite preparation, and achieve low preparation cost and tight combination , the effect of avoiding environmental pollution

Active Publication Date: 2010-08-11
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, organic amine templates are used in the synthesis of zeolites, which has the problems of seriously polluting the environment and increasing the cost of zeolite preparation; in terms of molding, extrusion methods are mostly used for molding, and, in solid moldings containing clay, , all contain an additional silicon source and / or aluminum source provided by non-clay. In addition, the prepared composite materials containing ZSM-5 are mostly used to treat nitrogen oxides in exhaust gas

Method used

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  • Method for preparing ZSM-5 zeolite/clay composite catalytic material without amine
  • Method for preparing ZSM-5 zeolite/clay composite catalytic material without amine
  • Method for preparing ZSM-5 zeolite/clay composite catalytic material without amine

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Embodiment 1

[0041] 2700g (dry basis) of hydrated kaolin and 180g of ZSM-5 zeolite were added with water to make a slurry with a solid content of 35%, and 143g of sodium silicate was added as a dispersant for spray molding to obtain 2500g of spray microspheres. The sprayed microspheres were calcined in a muffle furnace at 960°C for 3h to obtain the calcined microspheres A0. After mixing 12g of microspheres A0, 51mL of water glass, 0.6g of ZSM-5 zeolite, 16mL of 3M sulfuric acid and 120mL of water, the mixture was transferred into a stainless steel tank with a polytetrafluoroethylene liner, sealed, and placed at 150°C for crystallization. After 80 hours, filtered, washed and dried, the ZSM-5 zeolite composite material A1 of the present invention was obtained. The ZSM-5 content was determined to be 38% by weight by X-ray diffraction method.

Embodiment 2

[0043] The calcined microspheres A0 12g obtained in Example 1, 51mL water glass, 2g commercial solid silicon oxide (solid content 97%), 16mL 3M sulfuric acid and 120mL water were mixed, after mixing evenly, the mixture was transferred into a tank equipped with polytetrafluoroethylene. In a lined stainless steel tank, seal, stand at 150° C. for 96 hours for crystallization, filter, wash, and dry to obtain composite material A2 of the present invention containing 53% ZSM-5 zeolite.

Embodiment 3

[0045] 100g (dry basis) montmorillonite, 7g ZSM-5 zeolite, 2g sodium hydroxide, 2g sodium pyrophosphate, and 50g water were mixed, ground and mixed in a ball mill for 0.5h, and then extruded by an extruder. Drying at 120°C for 3h, followed by sintering in a muffle furnace at 1000°C for 2h to obtain a roasted strip B0. After mixing 8g of roasted bar B0, 26mL of water glass, 0.26g of ZSM-5 zeolite, 2.4g of NaCl, 7mL of 3M nitric acid and 80mL of water, the mixture was transferred into a stainless steel tank equipped with a polytetrafluoroethylene liner, sealed, Stand at 140°C for 24 hours for crystallization, then raise the temperature to 180°C for 48 hours, filter, wash, and dry to obtain the ZSM-5 zeolite composite material B1 of the present invention. Contains 45% ZSM-5 by X-ray diffraction method.

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Abstract

The invention relates to a method for preparing a ZSM-5 zeolite / clay composite catalytic material without amine. ZSM-5 zeolite is directly synthesized on clay serving as a carrier by taking the ZSM-5 zeolite as a crystal seed and adopting an in-situ crystallization method without using organic amine, alcohols or other additives. The preparation method comprises the following steps of: mixing the clay, the ZSM-5 zeolite serving as the crystal seed and a dispersing agent, and performing band extrusion, tabletting and spray drying on the mixture for molding; roasting the molded product at a high temperature; mixing the roasted product, water glass, an inorganic acid or an alkali metal hydroxide and water, and directly performing hydrothermal crystallization on the mixture under an alkaline condition to form the ZSM-5 zeolite-containing composite material; and after the crystallization is finished, filtering ,washing and drying. The ZSM-5 zeolite / clay composite material prepared by the method does not contain the organic amine and a template agent does not need removing through high-temperature roasting, so that the environmental pollution problem in the crystallization process and caused by roasting the organic amine is solved; meanwhile, the composite material has the advantages of low preparation cost and high abrasion resistance; a molecular sieve and the carrier are tightly bonded; and the requirement of a catalytic reaction on the strength performance of the catalyst is met.

Description

technical field [0001] The present invention relates to an amine-free preparation method of a ZSM-5 zeolite / clay composite catalytic material, in particular, relates to the method of directly synthesizing ZSM-5 zeolite on clay moldings without using organic amines, alcohols or other additional reagents Preparation method of composite catalytic material. Background technique [0002] ZSM-5 zeolite is a shape-selective zeolite (USP 3702886) with a unique three-dimensional channel structure and acid strength distribution successfully developed by Mobile Company in the United States in the late 1960s. It has high silicon-aluminum ratio and lipophilic and hydrophobic characteristics. With the characteristics of high thermal stability and high catalytic activity, it is widely used in petroleum refining and petrochemical processes, such as catalytic cracking, hydrocracking, hydrofining, hydrodewaxing, hydroreforming, xylene isomerization And synthesis gas to hydrocarbons and so on...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J21/16B01J37/08B01J37/04C10G11/05C10G47/02
Inventor 孙书红高雄厚季东庞新梅刘涛汪毅王栋
Owner PETROCHINA CO LTD
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