Method for preparing multistage-hole ZSM-5 molecular sieve

A technology of ZSM-5 and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of high production cost of molecular sieve, reduced dosage of template agent, large mesopore volume, etc. Achieve the effect of avoiding partial damage of crystal structure, improving service life and low pollution

Inactive Publication Date: 2016-12-07
HEILONGJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to provide a kind of method for preparing hierarchical porous ZSM-5 molecular sieve, compared with other method for synthesizing hierarchical porous ZSM-5 molecular sieve molecular sieve, has larger mesopore volume, and template agent consumption reduces greatly, solves the problem The high price and high toxicity of organic templates lead to high production costs of molecular sieves and environmental pollution.

Method used

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  • Method for preparing multistage-hole ZSM-5 molecular sieve
  • Method for preparing multistage-hole ZSM-5 molecular sieve
  • Method for preparing multistage-hole ZSM-5 molecular sieve

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specific Embodiment approach 1

[0037] Specific embodiment one: the method for preparing multi-stage porous ZSM-5 molecular sieve in this embodiment is carried out according to the following steps: add tetrapropyl ammonium hydroxide and deionized water to aluminum isopropoxide, stir evenly, become A solution; mix ethyl orthosilicate and deionized water evenly to prepare solution B. Add solution B slowly to solution A under stirring, stir vigorously for 3 hours to make a mixed gel, the molar composition of the mixed gel is Al 2 o 3 : SiO 2 =1:30~100, TPAOH:SiO 2 =0.25~0.40,H 2 O: SiO 2 =8~12. Transfer the mixed gel into a stainless steel airtight reaction kettle with a polytetrafluoroethylene liner, crystallize at a temperature of 100-140°C for 3-12 hours, then cool to room temperature, and make a seed crystal to be prepared use.

[0038] Dissolve sodium metaaluminate in deionized water to make solution A; weigh silica sol, NaOH and deionized water, stir well to make solution B; add solution A to solut...

specific Embodiment approach 2

[0039] Specific embodiment two: the method for preparing multi-stage porous ZSM-5 molecular sieve in the present embodiment is carried out according to the following steps:

[0040] Add 0.071g of aluminum isopropoxide to 5.0g of tetrapropylammonium hydroxide and 0.261g of deionized water, stir evenly, and prepare A solution; weigh 3.691g of tetraethyl orthosilicate and slowly add it to In solution A, stir vigorously for 3 hours to form a mixed gel, and the molar composition of the mixed gel is Al 2 o 3 : SiO 2 =1:50, TPAOH:SiO 2 =0.357,H 2 O: SiO 2 = 10.8. The above mixed gel was sealed in a stainless steel reactor with a polytetrafluoroethylene liner, crystallized at 140° C. for 9 hours, then taken out and cooled to room temperature to obtain seed crystals.

[0041] To 20g of silica sol (SiO 2 content is 30%) and 0.217g sodium metaaluminate, add 31g water, weigh 0.75gNaOH and 16.75g deionized water and add in silica sol, stir well, make A solution; 2 o 3 : SiO 2 =1:...

specific Embodiment approach 3

[0042] Specific embodiment three: this embodiment prepares ZSM-5 molecular sieve according to the method for specific embodiment two, difference is that the amount of adding 3-(phenylamino) propyl trimethoxysilane accounts for SiO 2 5% of the amount, other steps and parameters are the same as in the second embodiment.

[0043] According to the method of the present embodiment, the ZSM-5 molecular sieve whose addition amount of organic silicon reagent can be obtained is 5%, is denoted as ZSM-5 (5), and its XRD spectrogram, SEM photo and N 2 Adsorption and desorption isotherms are shown in Figure 4 , Figure 5 and Figure 6 .

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Abstract

The invention discloses a method for preparing a multistage-hole ZSM-5 molecular sieve, and belongs to the technical field of synthesis of molecular sieves. The invention provides the preparation method of the multistage-hole ZSM-5 molecular sieve which is low in cost and low in pollution, can change a silicon aluminum ratio (30-100) to the molecular sieve in a wide range, and has a large mesoporous volume. The method comprises the following steps of I, preparing crystal seeds for the synthesis of the multistage-hole ZSM-5 molecular sieve; II, preparing mixed gel, and performing stirring at room temperature; III, adding the crystal seeds prepared in the step I into the gel obtained in the step II, performing low-temperature crystallization for a short time, and adding a little organic silicon; and IV, continuing crystallization, performing cooling, performing centrifugal filtration, performing washing, performing drying, and performing roasting so as to obtain the multistage-hole ZSM-5 molecular sieve. According to the method provided by the invention, a few organic amine template agents are used only in the crystal seed synthesizing process, an s small, so that d besides, the addition amount of the added organic silicon as a mesoporous hole forming agent i compared with a method for synthesizing other multistage-hole ZSM-5 molecular sieve, the method disclosed by the invention has the advantages that the dosage of the template agents is small, products have a large mesoporous volume, and the problems that the production cost of the molecular sieve is high and environment is polluted caused by the condition that the organic template agent is high in price and large in toxicity can be solved.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve synthesis; in particular, it relates to a method for preparing a multi-stage porous ZSM-5 molecular sieve. Background technique [0002] Zeolite molecular sieve materials with multi-level channels not only have the strong acidity and hydrothermal stability of zeolite molecular sieves, but also the molecular diffusion coefficient in mesopores (macropores) is higher than that in traditional microporous molecular sieve channels. order of magnitude, making it expected to play an important role in catalytic reactions involving macromolecules. The ZSM-5 zeolite molecular sieve with MFI topology and three-dimensional intersecting channel system has uniform pore size (average pore size 0.54×0.56nm); abundant access channels ("Z" shaped channels and intersecting elliptical straight channels The composition of the pore structure), high thermal stability and hydrothermal stability, moderate acidity ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03
Inventor 武光郑柄辉
Owner HEILONGJIANG UNIV
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