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Method for rapidly preparing supported zeolite inner-membranes

A zeolite inner membrane and support type technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., to achieve the effect of reducing growth, fast speed, and good separation performance

Active Publication Date: 2013-12-18
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The problem to be solved by the present invention is to solve the problems of batch production and industrial application of zeolite inner membranes, and provide a method for adopting rapid batch single-channel or multi-channel zeolite inner membranes, especially the preparation of zeolite inner membranes with a length of 250-1500mm

Method used

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  • Method for rapidly preparing supported zeolite inner-membranes
  • Method for rapidly preparing supported zeolite inner-membranes
  • Method for rapidly preparing supported zeolite inner-membranes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1 Zeolite inner membrane fixation assembly

[0034] refer to figure 1 , a front view of a zeolite inner membrane fixing assembly equipped with a carrier tube according to a preferred embodiment of the present invention, which has the advantages of fast and uniform heating, short crystallization time, effective reduction of zeolite crystals entering the carrier pores and growth and suppression of intergranular defects The resulting zeolite inner membrane is usually thin and dense with high crystallinity.

[0035] Such as Figure 1-4 As shown, the zeolite inner membrane fixing assembly involved in a preferred embodiment of the present invention mainly includes: connecting the sealing part 1, connecting the sealing carrier tube 2 and the protective sleeve 7 through the sealing pin 6, preventing the crystallization reaction liquid from contacting the carrier tube. The surface 2b is in direct contact, and the middle part of the sealing plug 6 is provided with a ...

Embodiment 2

[0037] Embodiment 2 Microwave film reaction device

[0038] A preferred embodiment of the present invention crystallization synthesis step adopts microwave film reaction device 001-C, such as Figure 5 As shown, the device mainly includes: reaction vessel body A1, which is made of polytetrafluoroethylene microwave-transparent material, and the inner cavity 18 of the reaction vessel can manufacture one or more 250-1500mm supported zeolite inner membranes at a time; the reaction vessel The internal cavity 18 of the zeolite contains the crystallization reaction liquid synthesized by the carrier tube 2; the ferrule 20 of the reaction vessel is installed on the surface of the zeolite A1 of the reaction vessel, and is made of mesh and stainless steel. It can increase the compressive strength of the reaction vessel body A1, reduce the thickness and weight of the reaction vessel body A1, so that it meets the standard requirements of the pressure reaction vessel, and does not hinder th...

Embodiment 3

[0042] Example 3 Preparation of Supported Zeolite Inner Membrane

[0043] First, self-made NaA zeolite molecular sieves with an average particle size of 2μm (large seed) and 400nm (small seed) were calcined to prepare a seed liquid of a certain concentration, and the concentrations of the large seed and small seed were 10wt .% and 1wt.%, and the molecular sieve can be fully dispersed by vigorous stirring and ultrasonic vibration. The first step is to pre-set large seeds by vacuum method, and the outer surface of the pre-polished single-channel porous α-alumina carrier tube with an average pore size of 2.2 μm, an outer diameter of 12 mm, an inner diameter of 8 mm, and a length of 1 m is used The fixed component of the zeolite inner membrane is tightly sealed, connect the vacuum buffer tank, then immerse the carrier tube 2 in the large seed liquid, open the vacuum valve for 20 seconds and take it out, then put the carrier tube coated with the large seed into an oven at 80-100°C ...

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Abstract

The invention discloses a method for rapidly preparing supported zeolite inner-membranes, which is characterized in that the method comprises the following steps: a, hermetically protecting the outer surface of a carrier pipe by using a zeolite inner-membrane fixing assembly consisting of a fixed supporting panel, a protective casing and a connecting seal component firstly, then introducing large zeolite seed crystals to the inner surface of the carrier pipe through a dip coating method so as to block an orifice of the inner surface of a carrier, and modifying the carrier pipe by using small zeolite seed crystals through the dip coating method, and finally, forming an ultrathin seed crystal layer on the inner surface of the carrier pipe; and b, hermetically protecting the outer surface of the carrier pipe pre-coated with seed crystals by using the zeolite inner-membrane fixing assembly, horizontally placing the carrier pipe in a crystallization kettle, and slowly injecting crystallized reaction liquid into the crystallization kettle to carry out crystallized synthesis; and after the crystallized synthesis is completed, quenching the crystallization kettle, and after a prepared membrane is taken out, cleaning and drying the membrane so as to obtain a supported zeolite inner-membrane. The method disclosed by the invention can carry out rapid batch preparation on one or more single-channel and multi-channel supported zeolite inner-membranes.

Description

technical field [0001] The invention belongs to the technical field of inorganic membrane separation materials, and in particular relates to a preparation method of a supported zeolite inner membrane, in particular to a method for rapidly batch-preparing a zeolite inner membrane under the condition of microwave radiation heating. Background technique [0002] With the development of inorganic membrane technology, zeolite membranes are widely used, such as in the fields of dehydration of organic solvents, extraction of organic matter in water, separation of organic matter mixed systems, coupling of catalysis-membrane separation, and separation of gas mixed systems. Zeolite membrane preparation technology has become Research hotspots in industry and academia. Zeolite membranes are generally divided into packed zeolite membranes, unsupported zeolite membranes and supported zeolite membranes. However, the mechanical strength of the packed zeolite membrane is too low, and the un...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D69/10B01D67/00
Inventor 陈赞于海斌胡毅臧毅华郑秋红马元威刘宗园
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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