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A kind of preparation method and application of ZSM-11 molecular sieve catalyst without binder

A ZSM-11, binder-free technology, which is applied in the field of preparation of binder-free ZSM-11 molecular sieve catalysts, can solve the problems of few reports and achieve the effects of low content, high ethylene conversion rate and high selectivity

Active Publication Date: 2019-07-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are few reports on the synthesis of binder-free ZSM-11 molecular sieve catalysts

Method used

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  • A kind of preparation method and application of ZSM-11 molecular sieve catalyst without binder

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030]Weigh 10 grams of ZSM-11 molecular sieve, add 6 grams of 40% (weight) silica sol and 0.15g of 75% (weight) boehmite, mix, extrude, and dry at 120°C to obtain sample B. A mixture of 5 grams of tetrabutylammonium bromide, 10 grams of 1,6-hexanediamine and 30 grams of distilled water was added to the reaction kettle in advance, and 10 grams of sample B was placed in the reaction kettle above the porous stainless steel mesh and sealed at 180 ° C. The gas-solid phase treatment was carried out for 24 hours.

[0031] After the product is taken out, it is washed with distilled water, dried, roasted at 550°C for 2 hours, exchanged with 0.8mol / L ammonium nitrate solution for 3 times at 80°C, washed twice with water, dried at 120°C, roasted at 540°C for 3h, and steamed at 500°C After 2 hours of treatment, the resulting catalyst was designated as Cat-C. The relative crystallinity of Cat-C is 125%, and the NMR results show that there is very little non-framework aluminum in Cat-C. ...

Embodiment 2

[0033] Weigh 10 grams of ZSM-11 molecular sieve, add 4.8 grams of diatomaceous earth and 0.15 grams of aluminum sulfate. 18H 2 O mixed, extruded, dried at 120°C to obtain sample C; a mixture of 10 grams of 1,6-hexanediamine and 20 grams of distilled water was added to the reaction kettle, and 10 grams of sample C was placed in the reaction kettle Gas-solid phase treatment was carried out at 180° C. for 24 hours after sealing above the stainless steel mesh.

[0034] After the product is taken out, it is washed with distilled water, dried, roasted at 550°C for 2 hours, exchanged with 0.3mol / L ammonium nitrate solution for 3 times at 80°C, washed twice with water, dried at 120°C, roasted at 570°C for 4h, and steamed at 625°C After 3 hours of treatment, the obtained catalyst was designated as Cat-D. XRD results show that the relative crystallinity of Cat-D is 125%, and NMR results show that there is very little non-framework aluminum in Cat-D.

Embodiment 3

[0036] Take by weighing 10 grams of ZSM-11 molecular sieves, add 40 grams of silica content of 20% (weight) of water glass, 0.1g of sodium aluminate, 0.05g of aluminum nitrate after mixing, extrusion molding, through 120 ℃ drying, Sample D is obtained. A mixture of 4 grams of 1,6-hexanediamine and 15 grams of distilled water was added to the reaction kettle in advance, and 10 grams of sample D was placed in the reaction kettle and sealed at 120° C. for 90 hours.

[0037] After the product is taken out, it is washed with distilled water, dried, roasted at 550°C for 2 hours, exchanged twice with 0.4mol / L hydrochloric acid solution at 65°C, washed twice with water, dried at 140°C, roasted at 550°C for 3 hours, and then steamed at 400°C 5h, the obtained catalyst is denoted as Cat-E. XRD results show that the relative crystallinity of Cat-E is 120%, and NMR results show that there is very little non-framework aluminum in Cat-E.

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Abstract

The object of the present invention is to provide a kind of preparation method and the application of ZSM-11 molecular sieve catalyst without binding agent, concrete steps are: the weight content is 10~50% silicon dioxide and aluminum oxide binding agent and ZSM-11 molecule The mixture formed by raw powder, in the aqueous solution or steam containing alkyldiamine and / or halogenated organic amine, undergoes hydrothermal treatment to convert the binder silica into ZSM-11 molecular sieve, and form a whole with the original ZSM-11 molecular sieve Formula binder-free ZSM-11 catalyst; the prepared binder-free ZSM-11 is obtained through ion exchange, drying, roasting, and steam treatment to obtain the required catalyst. The catalyst prepared by the invention is used to catalyze ethylene and benzene in dry gas to prepare ethylbenzene. The invention has the advantages that: compared with the molecular sieve catalyst containing only silicon dioxide and alumina binder, the ethylene conversion rate on the binder-free molecular sieve catalyst can be significantly improved; the selectivity of ethylbenzene and ethylated products is high; Low xylene content.

Description

technical field [0001] The invention belongs to the field of petrochemical industry, and in particular relates to a preparation method and application of a binder-free ZSM-11 molecular sieve catalyst. Background technique [0002] Catalytic cracking dry gas is the by-product tail gas of the refinery, which contains 12-25% (volume fraction) of ethylene. At present, the scale of catalytic cracking units in my country ranks second in the world, and the amount of ethylene in dry gas is considerable. Dry gas is usually burned as fuel gas, which not only causes air pollution, but also wastes precious ethylene resources. The production of ethylbenzene from ethylene in dry gas is a simple and effective technology for direct utilization of dry gas, and it is widely used in my country. [0003] Since the end of the 1930s, a variety of processes for producing ethylbenzene using ethylene and benzene as raw materials have been developed. In the mid-1970s, Mobil Corporation of the Unite...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/40C07C15/073C07C2/66
Inventor 张爽刘盛林辛文杰谢素娟徐龙伢陈福存高扬
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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