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Method for preparing fluorine-containing mordenite zeolite membrane

A technology of mordenite and molecular sieve, which is applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems that there are no literature reports on mordenite molecular sieve membranes, achieve good permeability, broad application prospects, and simple synthesis devices Effect

Active Publication Date: 2010-06-02
JIANGXI NORMAL UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] Summarizing the preparation process and performance characterization of mordenite molecular sieve membranes reported in the above patents and literatures, the synthesis liquids investigated by the researchers are all composed of aluminum source, silicon source, alkali source and deionized water, and the addition of fluorine salt There is no literature report on the preparation of mordenite molecular sieve membrane

Method used

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  • Method for preparing fluorine-containing mordenite zeolite membrane
  • Method for preparing fluorine-containing mordenite zeolite membrane
  • Method for preparing fluorine-containing mordenite zeolite membrane

Examples

Experimental program
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Embodiment 1

[0045] The preparation of embodiment 1 mordenite molecular sieve

[0046] SiO powder, sodium metaaluminate, sodium hydroxide, ammonium fluoride and deionized water are used as raw materials to prepare raw material solution SiO 2 -Al 2 o 3 -NaOH-NH 4 F-H 2 O system, the molar ratio of each component is:

[0047] SiO 2 / Al 2 o 3 =20,H 2 O / SiO 2 =15,

[0048] Na 2 O / SiO 2 =0.15, NH 4 F / SiO 2 =0.4

[0049] The prepared raw material solution was aged at room temperature for 12 hours, put into a stainless steel reaction kettle lined with polytetrafluoroethylene, and put the stainless steel reaction kettle into an oven at 180°C for 24 hours to synthesize. The synthesized crystals were washed with deionized water until neutral and then dried at 105° C. for 12 h. The synthesized powder was characterized by XRD, such as figure 1 As shown, it is consistent with the standard spectrum of MOR molecular sieve, and it is pure mordenite.

Embodiment 2

[0050] Embodiment 2 Preparation of fluorine-containing mordenite molecular sieve membrane

[0051] The support used in this experiment is tubular mullite produced by Nikkato Co., Ltd. in Japan (the composition of mullite is 67wt.%Al 2 o 3 and 33wt.% SiO 2 ) as a carrier for synthesizing mordenite membranes, the inner diameter and outer diameter of the carrier are 9mm and 12mm respectively, the length is 100mm, the porosity is about 43%, and the average pore diameter is about 1 μm. After pretreatment such as water ultrasonic cleaning and drying, a thin layer of mordenite molecular sieve powder is coated on the surface of the support body, and the loading density of the seed crystal is 0.5-2mg / cm 2 , and the seeded supports were dried at 30 °C for 1 hour before use.

[0052] Take aluminum hydroxide as the aluminum source, silica sol as the silicon source, sodium fluoride as the fluorine source and sodium hydroxide as the alkali source, mix with a certain amount of deionized w...

Embodiment 3

[0060] Embodiment 3 Preparation of fluorine-containing mordenite molecular sieve membrane

[0061] The raw material and operation of the synthetic liquid used are the same as in Example 2, only the time is shortened to 12h. The synthesized molecular sieve membranes were used for pervaporation experiments and characterizations, and the results of the pervaporation experiments are shown in M-3 and M-4 in Table 2.

[0062] Table 2 Pervaporation performance of fluorine-containing mordenite molecular sieve membranes on mullite carrier in water / ethanol system (75°C)

[0063]

[0064]

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Abstract

The invention provides a method for preparing high-performance fluorine-containing mordenite zeolite membrane. The method is characterized in that crystallization is performed for 5 to 30 hours at a synthesis temperature between 130 and 190 DEG C by a secondary growth method so as to form a layer of dense defect-free fluorine-containing mordenite zeolite membrane on the outer surface of a porous tubular supporting body; the molar ratios of synthesis materials are as follow: the molar ratio of SiO2 to Al2O3 is 10 to 60; the molar ratio of H2O to SiO2 is 15 to 60; the molar ratio of Na2O to SiO2 is 0.15 to 0.5; and the molar ratio of F- to SiO2 is 0.01 to 2. NaF, KF, AlF3, (NH4) SiF6 and NH4F and the like can be used as a fluoride source. The preparation method avoids adding expensive organic template agents, and the fluoride source added greatly improves the permeability and acid resistance of the membrane. For example, when the method is applied to permeation experiment on water / ethanol (10 / 90 percent by weight) system at 75 DEG C, the average water permeation flux J is 1.2 to 2.5 kg / m2 h; the separation factor (alpha) is more than 1,000; and the synthesized membrane still maintains good stability in acid solution with a pH of less than 1. The method has the advantages of simple novel process, good repeatability and suitability for industrial production.

Description

technical field [0001] The invention provides a preparation method of a fluorine-containing mordenite molecular sieve membrane and its application in an ethanol-water mixture, belonging to the field of permeation and separation of inorganic materials. Background technique [0002] In recent decades, due to the requirements of environmental protection and energy saving, the use of pervaporation process (PV for short) in the separation of organic solvent mixtures has become a research hotspot in this field, especially since the 1980s, the successful industrialization of PV in the separation process of organic aqueous solutions, It provides some important theoretical basis for the PV separation of organic solvent mixtures. As a new membrane separation technology, it has the advantages of high single-stage separation, no pollution, energy saving, simple equipment, etc. The separation of solids; the removal of trace water in organic solvents and mixed solvents and the separation...

Claims

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Application Information

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IPC IPC(8): B01D71/02B01D67/00
Inventor 陈祥树周荣飞胡娜胡中丽段龙乔
Owner JIANGXI NORMAL UNIV
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