A kind of preparation method of high-strength binder-free hierarchical porous composite ZSM-5 catalyst

A ZSM-5, binder-free technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of complex experimental process, silicon-aluminum ratio, mechanical strength and insufficient experimental operation, etc. Achieve the effects of low waste liquid generation, simple and easy synthesis method, and high crushing resistance

Active Publication Date: 2016-08-03
中科催化新技术(大连)股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Direct preparation of binderless ZSM-5 molecular sieves usually uses kaolin or clay microspheres to carry out in-situ crystallization (CN1798608A; CN101462740A; CN101462741A) in the seed solution or alkaline solution of Y; or use organic matter etc. as hard templates (J .AM.CHEM.SOC.2005, 127, 12595-12600; Micro.Meso.Mater.2000, 35-36, 621-629); also in the role of Li ions (ZEOLITES, 1992, 11, 521-527) carried out, but the experimental process is complicated
Indirect preparation methods are generally divided into two types: one is to add active species such as zeolite seeds or templates to silicon and aluminum raw materials for molding, then hydrothermal crystallization in quaternary ammonium salt / organic amine solution or in water (or CN1105906A; CN1915820A; CN1927714A; CN101348262A; CN101428231A; CN101259424A; CN102371166A) in the atmosphere of crystallization (CN1105906A; CN1915820A; CN1927714A; Crystallization (Journal of Fuel Chemistry 2008, 36, 149-155; Chem.Mater.2004, 16, 5452-5459), the products obtained by this method have deficiencies in silicon-aluminum ratio, mechanical strength and experimental operation, etc.

Method used

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  • A kind of preparation method of high-strength binder-free hierarchical porous composite ZSM-5 catalyst
  • A kind of preparation method of high-strength binder-free hierarchical porous composite ZSM-5 catalyst
  • A kind of preparation method of high-strength binder-free hierarchical porous composite ZSM-5 catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Synthesize ZSM-5 molecular sieve according to literature method as reference sample (VerifiedSynthesisofZeoliticMaterials2 nd Ed, Elsevier, 2001, 198-199), recorded as sample 1#, its XRD results are shown in Table 1, and the XRF elemental composition and nitrogen physical adsorption results are shown in Table 2.

[0040] XRD result of table 1 sample 1#

[0041]

[0042]

[0043] Table 2 Composition of sample 1# and nitrogen physical adsorption results

[0044]

[0045] a Analysis by XRF method

Embodiment 2

[0047] The types and performance parameters of the mesoporous silica precursors used are shown in Table 3.

[0048] Table 3 Types and performance parameters of mesoporous silica precursors

[0049]

[0050] Concrete preparation process is as follows:

[0051] (a) Immerse the mesoporous silica precursor (Qingdao Ocean Chemical Co., Ltd., silica gel) in sodium hydroxide, aluminum salt or an aqueous solution of sodium hydroxide and aluminum salt, then dry and roast to obtain solid A.

[0052] (b) Place solid A in a place containing tetrapropylammonium ion (abbreviated as TPA + ) in an aqueous solution and dried to obtain solid B.

[0053] (c) Put the solid B in water vapor or the mixed steam of organic amine and water, and crystallize it at 120-210°C for 10-200h. After the solid is dried and roasted, a high-strength binder-free hierarchical porous composite ZSM can be obtained. -5 catalyst. Table 4 shows the corresponding relationship between the sample number and the type...

Embodiment 3

[0057] The samples obtained in Example 2 were characterized by XRD, and the XRD data were similar to those in Table 1, that is, the peak shapes and positions were the same, and the peak intensities were slightly different. Among them, the XRD data of typical sample 2# are shown in Table 5.

[0058] XRD result of table 5 sample 2#

[0059]

[0060]

[0061] Taking sample 1# as reference standard sample, by the strongest diffraction peak intensity (I) among each sample XRD figure in embodiment 2, according to formula:

[0062] ZSM content=(I 样品 / I 1# )×100%

[0063] The content of ZSM-5 in each sample is higher than 95%, as shown in Table 6.

[0064] The crush resistance of each sample in Example 2 was measured on a ZQJ-II intelligent particle strength testing machine of Dalian Intelligent Testing Machine Factory, and the results are shown in Table 6. The crush resistance of samples 2-8# are all higher than 40N / piece. The crush resistance of the product obtained by c...

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Abstract

The invention discloses a preparation method of a high-strength binding-agent-free multi-orifice compound ZSM-5 (Zeolite Socony Mobil-5) catalyst. The preparation method is characterized in that the high-strength binding-agent-free multi-orifice compound ZSM-5 molecular sieve based catalyst is prepared by a gas-phase synthesis method under a vapor or water and organic amine mixed steam atmosphere after aluminum is immersed by an aluminum source and organic amine ions are immersed by adopting mesoporous silica as a precursor, wherein the ratio of silicon to aluminum can be freely regulated within a certain range.

Description

technical field [0001] The invention relates to a preparation method of ZSM-5 catalyst. Background technique [0002] Silico-alumina molecular sieves have regular and uniform pore structure, large specific surface area, high adsorption performance, excellent acidity and shape-selective catalytic performance, and good thermal / hydrothermal stability. They have been widely used in adsorption separation, ion exchange and industrial catalysis and other important fields. Because molecular sieve materials are small in size and relatively loose, they cannot be directly applied, so they must go through a molding process to obtain ideal size, shape and strength properties. However, the binder material that must be used in the molding process will block the pores of some molecular sieves, reduce the effective specific surface area of ​​the molecular sieve, increase the mass transfer resistance of the molecular sieve, and seriously affect the effective performance of the molecular siev...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/40C01B39/40
Inventor 张琳田鹏刘中民杨虹熠
Owner 中科催化新技术(大连)股份有限公司
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