Preparation method of Zn/adhesive-free ZSM-11 molecular sieve catalyst

A ZSM-11, molecular sieve technology, applied in molecular sieve catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., to achieve the effect of high conversion rate of butane and yield of aromatics

Active Publication Date: 2017-09-19
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

[0009] The co-feed aromatization of DME and butane to generate aromatics is an effective supplement to the aromatics generated by the aromatization of methanol and butane. At present, there are few reports on the co-feed aromatization of DME and butane. This reaction has not been reported on Zn / binder-free ZSM-11 zeolite catalysts only for ZSM-5-based zeolites

Method used

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  • Preparation method of Zn/adhesive-free ZSM-11 molecular sieve catalyst

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Effect test

Embodiment 1

[0031] Sample-B was prepared according to the method of Comparative Example 2, and then metal zinc was loaded by hydrothermal deposition. The loading amount of zinc was 4.0wt%. Specifically, 10 grams of Sample-B was dipped in 30ml of zinc nitrate (0.21mol / L) and In the mixed solution of urea (zinc nitrate / urea=3 / 1 weight ratio), the hydrothermal temperature in the autoclave is 120℃, and the reaction is 20h. The precipitated mixture is filtered, and then placed in a drying oven at 120℃. 3h, then calcined at 600℃ for 4h to prepare Cat-C. The obtained catalyst Cat-C was tested by XRF, and the Na in the catalyst 2 O is less than 0.05wt%.

Embodiment 2

[0033] Weigh 10 grams of ZSM-11 molecular sieve, add 12 grams of 40% (weight) silica sol to mix, extrude and shape, and dry at 120°C to obtain sample B; add 10 grams of 1,6-hexanedi to the reactor in advance A mixture of amine and 20 grams of distilled water, 10 grams of sample B was placed on a porous stainless steel mesh in the reactor and sealed, and then subjected to gas-solid phase treatment at 180°C for 24 hours. The product was taken out and washed with distilled water, dried, roasted at 550°C for 2h, exchanged with 0.6mol / L ammonium nitrate solution at 80°C for 3 times, washed twice with water, dried at 120°C, roasted at 570°C for 4h, then steamed at 625°C After 3 hours of treatment, the obtained catalyst was recorded as Sample-C. XRD results show that the relative crystallinity of Sample-C is 145%.

[0034] Sample-C is loaded with zinc metal by hydrothermal deposition method, the loading amount of zinc is 6.0wt%, specifically, 10g of Sample-C is immersed in 30ml of a mi...

Embodiment 3

[0036] Weigh 10 grams of ZSM-11 molecular sieve, add 40 grams of water glass with a silica content of 20% by weight, mix, extrude, and dry at 120°C to obtain sample C. A mixture of 4 grams of 1,6-hexamethylene diamine and 15 grams of distilled water was added to the reactor in advance, and 10 grams of sample C was placed on the porous stainless steel mesh in the reactor and sealed, and then subjected to gas-solid phase treatment at 120° C. for 90 hours. The product was taken out and washed with distilled water, dried, roasted at 550℃ for 2h, exchanged twice with 0.7mol / L ammonium nitrate solution at 85℃, washed twice with water, dried at 140℃, roasted at 550℃ for 3h, then steamed at 400℃ After 5 hours of treatment, the obtained catalyst was recorded as Sample-D. XRD results show that the relative crystallinity of Sample-D is 142%.

[0037] Sample-D is loaded with zinc metal by hydrothermal deposition method. The loading amount of zinc is 7.0wt%. Specifically, 10g of Sample-D is ...

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Abstract

The invention provides a preparation method of a Zn/adhesive-free ZSM-11 molecular sieve catalyst. The method comprises the following specific steps: exchanging a synthesized Na-type adhesive-free ZSM-11 molecular sieve with a 0.5 to 1.0mol/L ammonium nitrate solution at the temperature of 70 to 90 DEG C, drying, calcining, and performing steam treatment to prepare an H-type molecular sieve; loading metal zinc on the obtained molecular sieve in an amount of 0.5 to 10.0 percent by weight through a hydrothermal deposition method, drying and calcining to obtain a desired catalyst. Compared with a Zn-loaded ZSM-11 molecular sieve catalyst only containing a silicon oxide adhesive, the Zn-loaded adhesive-free ZSM-11 molecular sieve catalyst has the advantage that the butane transformation rate and the aromatic hydrocarbon yield are increased.

Description

Technical field [0001] The invention belongs to the field of molecular sieve catalysts, and specifically relates to a preparation method of a Zn / binderless ZSM-11 molecular sieve catalyst. Background technique [0002] Aromatics are one of the most important basic raw materials for the production of petrochemical products. They are mainly used in the production of synthetic materials such as nylon, polyurethane, polyester, alkyd resins and as raw materials for phthalic anhydride plasticization. At present, they are mainly derived from catalytic reforming and cracking. Gasoline by-product. As we all know, oil is a non-renewable resource, and it is estimated that it can only continue to be exploited for a few decades according to the current consumption rate [G.A. Olah, Angew. Chem. Int. Ed. Engl. 44 (2005) 2636]. With the depletion of petroleum resources, the sources of aromatics are increasingly being challenged. [0003] One of the ways to solve this problem is the aromatization...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40C07C15/02C07C1/20C07C2/76
CPCB01J29/405B01J2229/60C07C1/20C07C2/76C07C15/02
Inventor 张爽刘盛林辛文杰谢素娟徐龙伢张琬铄
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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