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A kind of preparation method of self-supporting metal modified ZSM-5 molecular sieve and its application in the synthesis of isoprene

A ZSM-5, metal modification technology, used in molecular sieve catalysts, including molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of long cycle, complex preparation process, and cumbersome preparation process.

Active Publication Date: 2020-07-28
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, the modified ZSM-5 molecular sieve has problems such as complex preparation process and long cycle time. Usually, in the synthesis method of ZSM-5 molecular sieve, most of the ZSM-5 molecular sieves are crystallized first to obtain zeolite powder, and then modified with metal or non-metal to have functional Moreover, in the practical application of the catalytic process, it needs to be molded into a catalyst with a certain particle size in the later stage. The preparation process is cumbersome, resulting in high cost of catalyst preparation, which limits further popularization and application in actual production.

Method used

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  • A kind of preparation method of self-supporting metal modified ZSM-5 molecular sieve and its application in the synthesis of isoprene
  • A kind of preparation method of self-supporting metal modified ZSM-5 molecular sieve and its application in the synthesis of isoprene

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preparation example Construction

[0040] The invention provides a kind of preparation method of self-supporting metal modified ZSM-5 molecular sieve, comprising the following steps:

[0041] 1) immersing the silica gel particles in a metal salt solution to obtain a metal-containing precursor;

[0042] 2) Mix the metal-containing precursor obtained in the above steps with the basic template agent used to form the ZSM-5 molecular sieve, perform crystallization treatment, and then roast to obtain a self-supporting metal-modified ZSM-5 molecular sieve.

[0043] In the invention, firstly, the silica gel particles are immersed in a metal salt solution to obtain a metal-containing precursor.

[0044] The present invention has no special restrictions on the silica gel particles and their parameters, and the silica gel particles and their parameters for preparing molecular sieves well known to those skilled in the art can be used. Those skilled in the art can carry out according to actual application conditions, produc...

Embodiment 1

[0077] Dissolve 0.63g of aluminum nitrate nonahydrate and 0.26g of ferric nitrate nonahydrate in 7mL of water, add the above solution dropwise to 5g of 40-80 mesh silica gel particle carrier, soak it at room temperature for two hours, Dry in an oven at ℃ for 12 hours, mix the dried iron-aluminum silica gel precursor with 7 mL of tetrapropylammonium hydroxide aqueous solution (mass concentration 25%), put it into the reaction kettle, and crystallize at 180 ℃ for 48 Hours, after drying, calcined at 550°C for 5 hours to obtain a self-supporting metal-modified ZSM-5 molecular sieve.

[0078] The self-supporting metal-modified ZSM-5 molecular sieve prepared in Example 1 of the present invention is detected by SEM and XRD, and the detection results are as follows: figure 1 and figure 2 shown by figure 1 It can be seen that the modified ZSM-5 molecular sieve catalyst maintains the spherical shape and particle size of the original silica gel; figure 2 It can be seen that the mole...

Embodiment 2

[0086] Other implementation conditions and detection conditions are the same as in Example 1, except that the amount of ferric nitrate added is changed to 0.52g.

[0087] The prepared molded catalyst is used in the reaction of preparing isoprene by vapor phase condensation of formaldehyde and isobutene.

[0088] The performance test of the self-supporting metal-modified ZSM-5 molecular sieve prepared in Example 2 of the present invention showed that the conversion rate of formaldehyde was 90.1%, and the yield of isoprene was 46.2%.

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Abstract

The invention provides a method for preparing a self-supporting metal-modified ZSM-5 molecular sieve, comprising the following steps: firstly, immersing silica gel particles in a metal salt solution to obtain a metal-containing precursor; The precursor and the basic template agent used to form the ZSM-5 molecular sieve are mixed and then subjected to crystallization treatment, and then calcined to obtain a self-supporting metal-modified ZSM-5 molecular sieve. In the present invention, the active metal is directly compounded with the silica gel, and then the molecular sieve is synthesized and shaped, so as to realize the one-step preparation of the self-supporting metal-ZSM-5 zeolite molecular sieve catalyst, and avoid the tedious process of the catalyst's post-forming process. The preparation method provided by the invention It is simple, reduces the preparation cost of the catalyst, and has good raw material conversion rate and product yield in the isoprene synthesis reaction, which is beneficial to industrial production and the popularization and application of the metal-ZSM-5 zeolite molecular sieve catalyst.

Description

technical field [0001] The invention relates to the technical field of solid catalyst synthesis, relates to a preparation method and application of a modified ZSM-5 molecular sieve, in particular to a preparation method of a self-supporting metal modified ZSM-5 molecular sieve and its application in the synthesis of isoprene application. Background technique [0002] Isoprene is a colorless and volatile organic chemical raw material with a conjugated double bond structure, which is mainly used in the fields of synthetic rubber and fine chemical products. At present, the main preparation methods of isoprene are divided into physical separation method and chemical synthesis method. The physical separation method is the earliest method to produce isoprene. It extracts its carbon five fraction by cracking naphtha to produce ethylene. With the shortage of petroleum resources and the development of new ethylene technology, the preparation of isoprene by physical separation is gre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/46C07C2/86C07C11/18
CPCB01J29/46B01J37/0018B01J37/0201B01J2229/18C07C2/867C07C2529/46C07C11/18
Inventor 白晨曦曾尚景刘士俊代全权崔龙
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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