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Trace rare earth ion containing all silicon-1 molecular sieve based catalyst with microspheric MFI topological structure and spray shaping preparation method thereof

A technology of rare earth ions and molecular sieves, which is applied in the preparation of molecular sieve catalysts, physical/chemical process catalysts, and lactams, etc., to achieve obvious cost advantages, high total selectivity and total yield, and reduced energy consumption for product separation

Active Publication Date: 2019-05-21
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0019] So far, there have been no relevant documents or patents on the spray molding of all-silicon-1 molecular sieves containing extremely small amounts of rare earth ions into microspheres and then applied to the gas-phase Beckmann rearrangement reaction of cyclohexanone oxime

Method used

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  • Trace rare earth ion containing all silicon-1 molecular sieve based catalyst with microspheric MFI topological structure and spray shaping preparation method thereof
  • Trace rare earth ion containing all silicon-1 molecular sieve based catalyst with microspheric MFI topological structure and spray shaping preparation method thereof
  • Trace rare earth ion containing all silicon-1 molecular sieve based catalyst with microspheric MFI topological structure and spray shaping preparation method thereof

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preparation example Construction

[0057] The invention also discloses a method for preparing the catalyst by spraying, comprising the following steps:

[0058] a. Mix silicon source, rare earth ion source, organic template and water to obtain a colloidal mixture; wherein, SiO in the colloidal mixture 2 The molar ratio of organic templating agent and water is 1: (0.05-0.50): (5-100); in terms of silicon dioxide, the mass ratio of silicon source and rare earth ion is (10000-200000): 1; The above colloidal mixture is hydrothermally crystallized at 50-60°C for 0.5-3 days, then hydrothermally crystallized at 80-120°C for 0.5-3 days, and the obtained crystallized product is membrane filtered and washed until the pH value is 7.5-10 to obtain a molecular sieve slurry with a solid content of 25-35 wt%.

[0059] b. Mixing the molecular sieve slurry with a binder and beating to obtain a molecular sieve-binder mixed slurry with a solid content of 10-35 wt%.

[0060] c. Spray molding the molecular sieve-binder mixed slur...

Embodiment 1

[0082] With tetrapropyl ammonium hydroxide, 14.6gCe(NO 3 ) 4 ·7H 2 O and 440kg of water were mixed and stirred for 5 hours at room temperature to form a colloidal mixture with a pH value of 12.45, and the molar ratio of the mixture was SiO 2 :TPAOH:H 2 O=1:0.2:20, SiO 2 with Ce 3+ The mass ratio is 30300:1, the above mixture is moved into 2m 3 In a stainless steel reaction kettle, hydrothermal crystallization was performed at 50°C for 1 day, and then at 100°C for 2 days. water for washing, the amount of washing water is 7.0m 3 , the pH value of the washing water of the crystallized product reaches 9.1. Concentration of the slurry obtained after washing: 395 kg molecular sieve slurry with a solid content of 26.8% by weight.

[0083] Take a small amount of the molecular sieve slurry and dry it at 120° C. for 20 hours to obtain the original powder of all-silicon-1 molecular sieve containing very small amount of rare earth ions. All-silicon-1 molecular sieve was calcined ...

Embodiment 2

[0091] With tetrapropylammonium hydroxide, 28gCe(NO 3 ) 3 ·6H 2 O and 440kg of water were mixed and stirred for 5 hours at room temperature to form a colloidal mixture with a pH value of 12.47, and the molar ratio of the mixture was SiO 2 :TPAOH:H 2 O=1:0.2:20, SiO 2 with Ce 3+ The mass ratio is 13500:1, the above mixture is moved into 2m 3 In a stainless steel reaction kettle, hydrothermal crystallization was performed at 50°C for 1.5 days, and then at 100°C for 1.5 days. The pH value of the crystallized product was 13.73. of water for washing, the amount of washing water is 6.7m 3 , the pH value of the washing water of the crystallized product reaches 9.0. Concentration of the slurry obtained after washing: 436 kg molecular sieve slurry with a solid content of 24.5% by weight.

[0092] Take a small amount of the molecular sieve slurry and dry it at 120° C. for 20 hours to obtain the original powder of all-silicon-1 molecular sieve containing very small amount of rare...

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Abstract

The invention relates to the field of all silicon-1 molecular sieves and discloses a trace rare earth ion containing all silicon-1 molecular sieve based catalyst with a microspheric MFI topological structure and a spray shaping preparation method thereof. The trace rare earth ion containing all silicon-1 molecular sieve based catalyst with the microspheric MFI topological structure comprises 70-95wt% of all silicon-1 molecular sieve and containing an extremely trace amount of rare earth ions and 5-30 wt% of an adhesive according to the dry basis weight percentage; the particle size of the trace rare earth ion containing all silicon-1 molecular sieve based catalyst with the microspheric MFI topological structure is 20-400 (m, and the abrasion index K of the catalyst is less than 5; the BETspecific surface area of the all silicon-1 molecular sieve is 400-500 square meters / g; and the weight ratio of silicon oxide and the rare earth ions is (10000-200000):1. The trace rare earth ion containing all silicon-1 molecular sieve based catalyst with the microspheric MFI topological structure, disclosed by the invention, has the advantages that the abrasion index of the catalyst is low, andthe technological economy of a new process can be effectively improved when the catalyst is used for vapor phase Beckmann rearrangement reaction of cyclohexanone-oxime in a fluidized bed process.

Description

technical field [0001] The invention relates to the field of all-silicon-1 molecular sieves, in particular to a microspherical MFI topological structure all-silicon-1 molecular sieve catalyst containing a trace amount of rare earth ions and a spray molding preparation method thereof. Background technique [0002] Silicalite-1 molecular sieve (referred to as all-silicon-1 molecular sieve) was successfully synthesized for the first time in 1978 by E.M.Flanigen of UCC, etc., and belongs to the last member of the "Pentasil" family. All-silicon-1 molecular sieve is an aluminum-free all-silicon-1 molecular sieve with MFI topological structure. It is the simplest molecular sieve in the ZSM-5 structural molecular sieve family. The structural unit is SiO 4 tetrahedron. All-silicon-1 molecular sieve has a rich microporous structure and regular and uniform three-dimensional fine channels, and has a definite crystal structure of ZSM-5 molecular sieve, high internal specific surface ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/035C07D201/04C07D223/10
Inventor 王松林沈飞王韩
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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