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Preparation method of ZSM-type molecular sieve without binding agent

A binder-free, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of hindering reactants, reducing the effective components of the catalyst per unit mass, and reducing the catalyst reactivity and other problems, to achieve the effect of improving crystallinity, reducing dosage, and high template index

Active Publication Date: 2007-03-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is that the binder existing in the molecular sieve catalyst in the past will reduce the active ingredient in the catalyst per unit mass, hinder the diffusion of reactants and products in the catalyst, reduce the reactivity of the catalyst and produce more side effects. Product problem, provide a new preparation method of binderless ZSM type molecular sieve

Method used

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  • Preparation method of ZSM-type molecular sieve without binding agent
  • Preparation method of ZSM-type molecular sieve without binding agent
  • Preparation method of ZSM-type molecular sieve without binding agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～3

[0013] Weigh 100 grams of silicon-aluminum molar ratio SiO 2 / Al 2 o 3 20 ZSM-5 molecular sieve, 62.5 grams of 40% (weight) silica sol was added and mixed, extruded and dried at 120°C to obtain sample A-1.

[0014] Add 5 grams of tetrapropylammonium bromide, 10 grams of 1, a mixture of 6-hexamethylenediamine and 30 grams of distilled water in advance in the reactor, place 10 grams of sample A-1 in the reactor after being sealed above the porous stainless steel mesh Gas-solid phase treatment was carried out at 180°C for 24 hours, 72 hours, and 120 hours.

[0015] After the product was taken out, it was washed with distilled water, dried in the air and then calcined at 600°C in an air atmosphere. The XRD spectrum of the product processed for 24 hours shows that the crystallinity has increased at this time, indicating that new ZSM-5 molecular sieve crystals are generated; the crystallinity of the product after processing for 72 hours has been higher; the processing time is ext...

Embodiment 4～5

[0017] Weigh 100 grams of silicon-aluminum molar ratio SiO 2 / Al 2 o 3 100 ZSM-5 molecular sieve, 13 grams of 40% (weight) silica sol was added and mixed, extruded and dried at 120° C. to obtain sample B-1.

[0018] Add 2 grams of tetrapropylammonium bromide, 15 grams of 1,6-hexamethylenediamine and 30 grams of distilled water in advance in the reaction kettle, and place 10 grams of sample B-1 in the reaction kettle after being sealed above the porous stainless steel mesh Gas-solid phase treatment was carried out at 120°C for 72 hours and 120 hours.

[0019] After the product was taken out, it was washed with distilled water, dried in the air and then calcined at 550°C in an air atmosphere. The XRD pattern of the product treated for 72 hours showed that the crystallinity of the product was already high; when the treatment time was extended to 120 hours, the crystallinity of the product did not continue to increase.

Embodiment 6～8

[0021] Weigh 100 grams of silicon-aluminum molar ratio SiO 2 / Al 2 o 3 600 ZSM-48 molecular sieve, mixed with 68 grams of water glass with a silica content of 25.9% (weight), extruded and dried at 120°C to obtain sample C-1.

[0022] Add 10 grams of tetrapropylammonium bromide, 5 grams of 1,6-hexamethylenediamine and 30 grams of distilled water in advance in the reaction kettle, and place 10 grams of sample C-1 in the reaction kettle after being sealed above the porous stainless steel mesh. Gas-solid phase treatment was carried out at 200°C for 24 hours, 72 hours, and 120 hours.

[0023] After the product was taken out, it was washed with distilled water, dried in the air and then calcined at 600°C in an air atmosphere. The XRD pattern of the product treated for 24 hours shows that the crystallinity is already high at this time; the crystallinity of the product does not continue to increase when the treatment time is extended to 72 hours and 120 hours.

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Abstract

The present invention relates to preparation process of adhesive-free ZSM type molecular sieve, and aims at solving the problem of adding adhesive causing decrease in effective surface area and limited diffusion. Technologically, the present invention is that adhesive silica in 5-50 wt% and ZSM type molecular sieve powder are made to form mixture, and the mixture is hydrothermally converted inside water solution or steam containing organic amine halide and alkyl diamine into integrated ZSM type molecular sieve. The process of the present invention may be used in the industrial preparation of ZSM type molecular sieve catalyst.

Description

technical field [0001] The invention relates to a method for preparing a binder-free ZSM molecular sieve. Background technique [0002] Molecular sieves have uniform and ordered micropores, large specific surface area, and high hydrothermal stability, and are widely used in the field of catalysis. Small-grain molecular sieves have shorter intracrystalline diffusion channel lengths and larger outer surfaces, which are beneficial to increase the contact opportunities between reactants and active sites in micropores, thereby improving the performance of molecular sieves. Unique advantages, such as unique macromolecular selectivity, high catalytic activity and long catalyst life, etc. However, the size of molecular sieve is too small, which is not very convenient in practical application, and has the disadvantages of difficult recovery, easy deactivation and aggregation. It is necessary to add binder during the molding process, which reduces the eff...

Claims

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Application Information

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IPC IPC(8): C01B39/02C01B39/38
Inventor 滕加伟赵国良金文清
Owner CHINA PETROLEUM & CHEM CORP
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