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Zeolite film and process for producing zeolite film

A manufacturing method and zeolite membrane technology, applied in separation methods, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve problems such as high separation performance, inability to provide large-scale membranes, and membrane defects, and achieve high separation performance, Yield improvement and defect reduction effects

Active Publication Date: 2015-05-06
NGK INSULATORS LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the other hand, for practical use, it is necessary to form a film on a large substrate in the shape of a monolith with a large film area. A difference occurs, and the film will have defects when the structure directing agent is removed from the thicker film
Therefore, it is not possible to provide a membrane with a small amount of defects in the entire large membrane and high separation performance

Method used

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  • Zeolite film and process for producing zeolite film
  • Zeolite film and process for producing zeolite film
  • Zeolite film and process for producing zeolite film

Examples

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preparation example Construction

[0067] [2] Preparation of raw material solution (sol)

[0068] Next, a raw material solution having a predetermined composition containing 1-adamantanamine dissolved in ethylenediamine was prepared.

[0069] Since 1-adamantanamine is the SDA (structure-directing agent) in the synthesis of DDR-type zeolite, that is, the substance (structure-directing agent) used as a mold to form the crystal structure of DDR-type zeolite, it is the same as the raw material of DDR-type zeolite. SiO 2 (Silicon dioxide) molar ratio is important. 1-Adamantadine / SiO 2 The molar ratio must be in the range of 0.002~0.5, preferably in the range of 0.002~0.4, more preferably in the range of 0.002~0.3. 1-Adamantadine / SiO 2 If the molar ratio is less than this range, the 1-adamantanamine in SDA will be insufficient, and it will be difficult to form a DDR type zeolite. On the other hand, if it exceeds this range, 1-adamantanamine will be added in more than the necessary amount, which is not preferable...

Embodiment 1~4）

[0086] According to the following (1)-(4), the samples of Examples 1-4 were produced.

[0087] (1) Introduction of seed crystals (particle attachment process)

[0088] Dilute the seed crystal dispersion containing DDR-type zeolite particles with a particle size of 0.5 μm or less with ion-exchanged water or ethanol, adjust the seed crystal concentration to 0.001~0.36% by mass, stir with a stirrer at a speed of 300 rpm, and introduce the seed crystal Use a suspension. At the lower end of the wide-mouth funnel 32, a porous monolithic substrate 1 (having a diameter of 55 The outer diameter of the through-hole (well 2) Porous base material with a total length of 160 mm (refer to figure 1 , glass seals at both ends), the hole 2 in the unit area of ​​the end face 4 is 7.8 cells / cm 2 ), so that 160mL of the suspension for seed crystal introduction flows from the upper part of the substrate and passes through the hole 2 (refer to image 3 ). Ventilate and dry the inside of the ...

Embodiment 5、6）

[0096] Using a porous monolithic substrate 1 (having a diameter of 2050 The outer diameter of the through-hole (well 2) Porous base material with a total length of 1000 mm (refer to figure 1 , glass seals at both ends)), according to the same method as in Examples 1-4 to produce Examples 5 and 6. That is, similarly to (1) to (3) above, the zeolite membrane 11 was synthesized by heat-treating (hydrothermal synthesis) at 135° C. for 52 or 62 hours using the ethanol-diluted suspension for introducing seed crystals. The He permeation of the membrane after hydrothermal synthesis is below the detection limit (2 kPa), it was confirmed that the cells 2 of the monolithic substrate 1 were covered with the DDR film. In the structure directing agent removal process of (4), while passing oxygen at 37 L / min, heat at 450°C for 50 hours to burn and remove 1-adamantanamine in the micropores as the structure directing agent. Furthermore, by passing oxygen at 37L / min, the O in the furnace ...

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Abstract

There are provided a process for producing a zeolite membrane which, even when large, has few defects and which has higher separation performance than conventional zeolite membranes, and a zeolite membrane obtained by the process. In the process, the structure-directing agent is removed in the atmosphere having an O 2 concentration of 22.0 vol% or more. Specifically, the process includes: a particle adhesion step of allowing zeolite particles functioning as seeds to flow down the surface of the substrate by means of the weight of the slurry itself, thereby adhering to the substrate and a membrane-forming step of forming a zeolite membrane on the substrate by immersing the substrate having the zeolite particles adhering thereto in sol containing the structure-directing agent for hydrothermal synthesis, thereby forming a zeolite membrane on the substrate.

Description

technical field [0001] The present invention relates to a zeolite membrane and a method for producing the zeolite membrane. Background technique [0002] Zeolites are used as catalysts, catalyst supports, adsorbents, etc. In addition, zeolite membrane devices formed on the surface of porous substrates made of metal or pottery can be used as gas separation membranes or pervaporation membranes by utilizing the molecular sieve function of zeolites. [0003] Among zeolites, there are many types (types) with different crystal structures, such as LTA, MFI, MOR, FER, FAU, and DDR. For example, it is known that the main component of DDR (Deca-Dodecasil 3R) type zeolite is silica, and it is formed of microporous polyhedrons composed of oxygen 8-membered rings with a micropore diameter of 4.4×3.6 angstroms. Due to the small pore size in DDR zeolite, it is used as carbon dioxide (CO 2 ), methane (CH 4 ), ethane (C 2 h 6 ) and other low molecular gas molecular sieve membrane applic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/02B01D69/04B01D69/10B01D69/12C01B39/04
CPCB01D53/228B01D63/066B01D67/0051B01D69/02C01B39/48B01D2325/02833B01D71/0281
Inventor 内川哲哉谷岛健二新野真纪子
Owner NGK INSULATORS LTD
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