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Primary crystallization hydrothermal preparation method of A-type and X-type molecular sieves containing pure Na ions

A molecular sieve and deionized water technology, applied in the direction of A-type crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the problems of complicated and time-consuming processes, and achieve low production cost, It is convenient for industrial production and the effect of simple synthesis process

Inactive Publication Date: 2012-12-26
KEY LAB OF INORGANIC SYNTHESIS & PEPARATIVE CHEM AT JILIN UNIV IN ZHUHAI
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  • Abstract
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  • Application Information

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Problems solved by technology

Although this method uses cheap reactants, the synthesis process includes aging for 4-6 hours, the first crystallization for 2-4 hours (60-80°C), and the second crystallization for 12-48 hours (90-80°C). 100°C), the process is complicated and time-consuming

Method used

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  • Primary crystallization hydrothermal preparation method of A-type and X-type molecular sieves containing pure Na ions
  • Primary crystallization hydrothermal preparation method of A-type and X-type molecular sieves containing pure Na ions
  • Primary crystallization hydrothermal preparation method of A-type and X-type molecular sieves containing pure Na ions

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Experimental program
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Effect test

Embodiment 1

[0035] Preparation of NaA type molecular sieve (0.7 micron):

[0036] 1.5 g NaAlO 2 Add it into 10 ml of deionized water, stir to dissolve it evenly, add 1.875 g of NaOH and continue to stir for 30 minutes, and let it stand for a while; an aluminum source solution is obtained.

[0037] 1.5 g Na 2 SiO 3 9H 2 O was added to 10 ml of deionized water, stirred and dissolved until uniform to obtain a silicon source solution.

[0038] Then slowly add the aluminum source solution that has been left still to the stirring silicon source solution, continue stirring for 30 minutes, put it into a polytetrafluoroethylene-lined stainless steel reaction kettle, crystallize at 100°C for 5 hours, filter and dry Dry to obtain NaA type molecular sieve (0.7 micron). The obtained samples were uniform in size and well crystallized (attached figure 1 ), the yield is 70-75%, Si / Al=1:1, and the pore size is 0.4nm.

Embodiment 2

[0040] Preparation of NaX type molecular sieve (10 microns):

[0041]Add 0.3 g of NaOH to 6.5 ml of deionized water, stir well, then add 0.13 g of NaAlO 2 Continue to stir for 30 minutes, and let it stand for a while; an aluminum source solution is obtained.

[0042] 1.2 g Na 2 SiO 3 9H 2 O was added to 15 ml of deionized water and stirred until homogeneous to obtain a silicon source solution.

[0043] Then slowly add the aluminum source solution that has been standing still to the stirring silicon source solution, continue stirring for 30 minutes, put it into a stainless steel reaction kettle lined with polytetrafluoroethylene, crystallize at 100 ° C for 3 days, and filter and dry , to get NaX molecular sieve powder (10 microns) (attached figure 2 ), the yield is 70-75%, Si / Al=1:1.3, and the pore size is 1.0nm.

Embodiment 3

[0045] Preparation of NaA type molecular sieve (0.8 micron):

[0046] 0.75 g NaAlO 2 Add it into 10 ml of deionized water, stir to dissolve it evenly, add 0.94 g of NaOH and continue to stir for 30 minutes, and let it stand for a while; an aluminum source solution is obtained.

[0047] 0.75 g Na 2 SiO 3 9H 2 O was added to 10 ml of deionized water, stirred and dissolved until uniform to obtain a silicon source solution.

[0048] Then slowly add the aluminum source solution that has been left still to the stirring silicon source solution, continue stirring for 30 minutes, put it into a polytetrafluoroethylene-lined stainless steel reaction kettle, crystallize at 100°C for 1 hour, filter and dry Dry to obtain NaA-type molecular sieves (0.8 microns). The obtained samples were uniform in size and well crystallized (attached image 3 ), the yield is 70-75%, Si / Al=1:1, and the pore size is 0.4nm.

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Abstract

The invention belongs to the technical field of microporous molecular sieve preparation, in particular to a primary crystallization hydrothermal preparation method of NaA and NaX microporous molecular sieves with adsorption cations which are all Na ions without a template agent, a guide agent and aging time. According to the preparation method, sodium aluminate (NaAlO2), sodium hydroxide (NaOH), sodium metasilicate nonahydrate (NA2SiO3.9H2O) and deionized water are used for synthesis, and two solutions based on a silicon source and an aluminum source are respectively prepared by synthetic steps; and the two solutions are uniformly stirred and then mixed, and after the mixed solution is persistently stirred for a period of time, the mixed solution is crystallized for several days in a high-temperature oven to obtain the NaA and NaX microporous molecular sieves with the adsorption cations which are all Na ions. The preparation method has the advantages of simple synthetic process, easiness of operation, convenience in industrialized production, commonality and easiness of obtaining reaction raw materials and low production cost, and the sizes of sample particles are 0.7-11 micrometers, so that the NaA and NaX microporous molecular sieves are moderate in sizes and convenient to use.

Description

technical field [0001] The invention belongs to the technical field of preparation of microporous molecular sieves, and in particular relates to a primary crystallization hydrothermal preparation method of NaA and NaX microporous molecular sieves without template agent and directing agent and without aging time. Background technique [0002] As a porous material, microporous molecular sieves (pore size less than 2 nm) have extremely attractive properties, such as ion exchange, diffusion and adsorption, shape selectivity and catalytic activity, and they can play an important role in host-guest assembly chemistry. This makes people's demand for microporous molecular sieves, from the initial mining of natural zeolite (a type of microporous molecular sieve), to now mainly relying on artificial commercial synthesis. As of 2006, there are about 170 molecular sieves identified by the International Molecular Sieve Association, of which only 17 have been commercially synthesized, whi...

Claims

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Application Information

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IPC IPC(8): C01B39/16C01B39/22
Inventor 薛铭张文婷康子曦范黎黎裘式纶
Owner KEY LAB OF INORGANIC SYNTHESIS & PEPARATIVE CHEM AT JILIN UNIV IN ZHUHAI
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