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Method for preparing NaA type zeolite membrane for ethanol dehydration

A technology of ethanol dehydration and zeolite membrane, applied in A-type crystalline aluminosilicate zeolite, chemical instruments and methods, crystalline aluminosilicate zeolite, etc., can solve problems such as limited use, difficult cleaning, and difficulty in applying high-purity ethanol. Achieve the effects of enhanced mechanical strength, extended service life, and excellent separation performance

Inactive Publication Date: 2015-04-29
DALIAN CITY SHAHEKOU DISTRICT SMALL MEDIUM & MICRO ENTERPRISES SERVICE CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In practical application, the rectification method is difficult to apply to large-scale industrial production of high-purity ethanol due to its high energy consumption, that is, the economic feasibility is low
The organic polymer membrane separation method, due to the limitations of the membrane itself, is not easy to clean, low mechanical strength, short service life, etc., which limits its use in the separation of ethanol / water systems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] α-Al with a porosity of 50% 2 o 3 A ceramic tube was used as a carrier, and both ends were sealed with Teflon plugs. Place the sealed carrier tube in an oven at 170°C for 2 hours, then quickly put the hot carrier into a large seed solution with a mass concentration of 8wt.% for 20 seconds, then take it out slowly, remove the polytetrafluoroethylene plug and release the carrier tube water, and dried at 50°C for 24 hours to form the first layer of NaA molecular sieves. The second layer of NaA molecular sieve is introduced by the coating method to form a dense ultra-thin seed layer.

[0019] Using silica sol, sodium hydroxide, sodium metaaluminate and deionized water as raw materials, the molar ratio of SiO 2 :Al 2 o 3 =0.5, Al 2 o 3 :Na 2 O=2,H 2 O: Al 2 o 3 =100 to prepare crystallization mother liquor. First add silica sol to sodium hydroxide solution, stir at room temperature for 16 hours to form solution A; then slowly add sodium metaaluminate to solution ...

Embodiment 2

[0026] α-Al with a porosity of 50% 2 o 3 A ceramic tube was used as a carrier, and both ends were sealed with Teflon plugs. Place the sealed carrier tube in an oven at 170°C for 2 hours, then quickly put the hot carrier into a large seed solution with a mass concentration of 8wt.% for 20 seconds, then take it out slowly, remove the polytetrafluoroethylene plug and release the carrier tube water, and dried at 50°C for 24 hours to form the first layer of NaA molecular sieves. The second layer of NaA molecular sieve is introduced by the coating method to form a dense ultra-thin seed layer.

[0027] Using silica sol, sodium hydroxide, sodium metaaluminate and deionized water as raw materials, the molar ratio of SiO 2 :Al 2 o 3 =3, Al 2 o 3 :Na 2 O=6, H 2 O: Al 2 o 3 =300 to prepare crystallization mother liquor. First add silica sol to sodium hydroxide solution, stir at room temperature for 16 hours to form solution A; then slowly add sodium metaaluminate to solution A...

Embodiment 3

[0034] α-Al with a porosity of 50% 2 o 3 A ceramic tube was used as a carrier, and both ends were sealed with Teflon plugs. Place the sealed carrier tube in an oven at 170°C for 2 hours, then quickly put the hot carrier into a large seed solution with a mass concentration of 8wt.% for 20 seconds, then take it out slowly, remove the polytetrafluoroethylene plug and release the carrier tube water, and dried at 50°C for 24 hours to form the first layer of NaA molecular sieves. The second layer of NaA molecular sieve is introduced by the coating method to form a dense ultra-thin seed layer.

[0035] Using silica sol, sodium hydroxide, sodium metaaluminate and deionized water as raw materials, the molar ratio of SiO 2 :Al 2 o 3 =1.5, Al 2 o 3 :Na 2 O=4, H 2 O: Al 2 o 3 =250 to prepare crystallization mother liquor. First add silica sol to sodium hydroxide solution, stir at room temperature for 16 hours to form solution A; then slowly add sodium metaaluminate to solution...

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Abstract

The invention discloses a method for preparing a NaA type zeolite membrane for ethanol dehydration. NaA type molecular sieves are taken as seed crystals, an ultra-thin uniform seed crystal layer is directly introduced into the surface of a porous support tube, and high-performance NaA type zeolite membranes with different silica-alumina ratios are synthesized by hydrothermal crystallization. The preparation method is implemented by the following steps of introducing a layer of NaA type molecular sieve into the surface of the porous support tube by adopting a hot dipping method, and then introducing a second layer of NaA type molecular sieve to form a dense ultra-thin seed crystal layer by adopting a dip coating method; preparing crystallization mother liquid from silica sol, sodium hydroxide, sodium metaaluminate and de-ionized water; adding the prepared crystallization mother liquid into a stainless steel reaction kettle containing polytetrafluoroethylene, placing the porous support tube pre-planted with seed crystals, and performing hydrothermal synthesis for 4 to 10h at the reaction temperature of 60 to 80 DEG C; taking out the support tube after reaction, washing the support tube with de-ionized water, and drying the support tube at 80 DEG C.

Description

technical field [0001] The invention belongs to the technical field of osmotic separation of inorganic materials, and relates to a preparation method of a zeolite molecular sieve membrane, in particular to a preparation method of a NaA molecular sieve used for ethanol dehydration. Background technique [0002] Under the background of energy shortage and increasingly internationalized environmental problems, people in the industry have begun to seek new energy that can replace traditional energy, and ethanol has become the focus of people's attention. Traditional rectification and pressure swing adsorption consume a lot of energy, while supported zeolite membranes are favored due to their remarkable separation effect in alcohol / water mixtures. [0003] There are three main methods for industrially producing high-purity ethanol: (1) rectification; (2) organic polymer membrane separation; (3) zeolite molecular sieve membrane separation. At present, the main method for producin...

Claims

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Application Information

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IPC IPC(8): B01D71/02B01D69/10B01D67/00C01B39/14C07C31/08C07C29/76
Inventor 秦宏佳
Owner DALIAN CITY SHAHEKOU DISTRICT SMALL MEDIUM & MICRO ENTERPRISES SERVICE CENT
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