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Method for solid-phase synthesis of wettability controllable ZSM-5 zeolite

A ZSM-5, solid-phase synthesis technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of limited control range, affecting the acidity of zeolite, and impossible to obtain. Achieving improved performance, reduced emissions, and controlled synthesis

Active Publication Date: 2018-07-10
PETROCHINA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the control range of the wettability of zeolite through the silicon-aluminum ratio is relatively limited, and the change of the silicon-alumina ratio will also affect the acidity of the zeolite, which leads to limitations of this method
For example: it is not possible to obtain hydrophobic (requires high silicon-aluminum ratio) zeolites with high acid density (requires low silicon-aluminum ratio) by this method

Method used

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  • Method for solid-phase synthesis of wettability controllable ZSM-5 zeolite
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  • Method for solid-phase synthesis of wettability controllable ZSM-5 zeolite

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Effect test

Embodiment 1

[0042] Embodiment 1: solid-phase synthesis hydrophilic ZSM-5 zeolite molecular sieve

[0043] First, weigh 1.2g of white carbon black as a solid raw material, 0.8g of organic silicon prepared by hydrolysis of dimethyldimethoxysilane, 0.665g of Al 2 (SO 4 ) 3 18H 2 0, 2.6g tetrapropylammonium bromide template (T) and 0.26g NaOH are poured into a mortar, then ground and mixed, ground for 10 minutes, the reaction raw materials are added in a polytetrafluoroethylene stainless steel reactor, 180 After 2 days of crystallization at ℃, the crystallization is complete, and the product is dried and calcined at 550°C for 4 hours in an oxygen atmosphere to obtain the product. The proportioning of reaction raw material is as follows:

[0044] SiO 2 :0.03Al 2 o 3 :0.1Na 2 O: 0.3T.

[0045] According to X-ray diffraction analysis, its structure is ZSM-5 zeolite molecular sieve. figure 1 The XRD pattern of the product synthesized by this method.

Embodiment 2

[0046] Embodiment 2: solid-phase synthesis hydrophilic ZSM-5 zeolite molecular sieve

[0047] First, weigh 1.6g of white carbon black as a solid raw material, 0.4g of organic silicon prepared by hydrolysis of diethyldiethoxysilane, 0.465g of Al 2 (SO 4 ) 3 18H 2 O, 2.0g tetrapropylammonium bromide template agent and 1.316g NaOH, pour it into a mortar, grind and mix, grind for 10 minutes, add the reaction raw materials into a polytetrafluoroethylene stainless steel reaction kettle, and crystallize at 180°C The crystallization is complete in 1 day, the product is dried, and roasted at 550 degrees under an oxygen atmosphere for 4 hours to obtain the product. The proportioning of reaction raw material is as follows:

[0048] SiO 2 :0.02Al 2 o 3 :0.5Na 2 O: 0.23T.

[0049] According to X-ray diffraction analysis, its structure is ZSM-5 zeolite molecular sieve. figure 2 The XRD pattern of the product synthesized by this method.

Embodiment 3

[0050] Embodiment 3: solid-phase synthesis hydrophilic ZSM-5 zeolite molecular sieve

[0051] First, weigh 1.8g of white carbon black as a solid raw material, 0.2g of organic silicon prepared by hydrolysis of diethyldiethoxysilane, 0.022g of sodium metaaluminate, 1.74g of tetrapropylammonium bromide template and 1.11g of NaOH , pour it into a mortar, grind and mix again, grind for 10 minutes, add the reaction raw materials into a polytetrafluoroethylene stainless steel reactor, crystallize at 120°C for 8 days and then completely crystallize, the product is dried and 550°C in an oxygen atmosphere Roasting obtains product for 4 hours. The proportioning of reaction raw material is as follows:

[0052] SiO 2 :0.004Al 2 o 3 :0.3Na 2 O: 0.2T.

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Abstract

A method for solid-phase synthesis of wettability controllable ZSM-5 zeolite includes the steps: grinding and mixing template agents or seed crystals with silicon sources, alkali sources and / or aluminum sources of solid raw materials; placing grinded mixture into a reactor and crystallizing the mixture for 1-10 days under the condition of the temperature of 100-180 DEG C; taking out crystallized solid products and then drying the solid products to obtain a ZSM-5 zeolite molecular sieve. When the template agents are used in the first step, the silicon sources are SiO2, the aluminum sources areAl2O3, the alkali sources are Na2O, and the mole ratio of the raw materials is SiO2:Al2O3:Na2O:the template agents=1:(0.004-0.03):(0.1-0.5):(0.1-0.3). When the seed crystals are used in the first step, the mass ratio of the seed crystals to the silicon sources is 4-10%. Organic silane is added in the synthesis process, organic groups are controllably introduced into a zeolite framework, and hydrophobicity of the zeolite framework is improved. By high-temperature roasting, the organic groups can be transformed into silicon hydroxyl, and the hydrophilcity of the silicon hydroxyl is improved. Bycontrolling wettability, the adsorption and catalytic performances of the zeolite for different substrates can be obviously improved, controllable synthesis of the ZSM-5 zeolite is realized, and the ZSM-5 zeolite has high application values.

Description

technical field [0001] The invention belongs to a molecular sieve preparation method, in particular to a method for synthesizing ZSM-5 zeolite with controllable wettability under solid-phase crystallization conditions. Background technique [0002] Zeolite molecular sieve is a clean bench aluminosilicate mineral with a spatial network structure of silicon-oxygen tetrahedrons and aluminum-oxygen tetrahedrons interlaced. This structural feature makes zeolite molecular sieves have three major characteristics: selective adsorption separation, ion exchange and catalysis. At present, zeolite has been widely used in the fields of petrochemical, coal conversion and fine chemical industry. Zeolite has become the core technology of these fields and has brought huge economic benefits. The advancement of zeolite synthesis technology is also closely related to industrial development. The exploration of new synthetic routes and performance regulation of molecular sieves is one of the ho...

Claims

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Application Information

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IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72
Inventor 王亮沈宜泓王成涛崔岩王晓化庞新梅
Owner PETROCHINA CO LTD