Zeolite seed crystal, method of producing zeolite seed crystal, method of producing zeolite membrane complex, and separation method

Patent metadata

Field	Value
Publication number	US-10927010-B2
Application number	US-202016819608-A
Country	US
Kind code	B2
Filing date	Mar 16, 2020
Priority date	Mar 26, 2019
Publication date	Feb 23, 2021
Grant date	Feb 23, 2021

Abstract

A seed crystal is a crystal of zeolite that is to be deposited on a support when producing a zeolite membrane complex that includes the support and a zeolite membrane formed on the support. A volume-cumulative particle size distribution of the seed crystal, measured by a laser diffraction scattering method, has a coefficient of variation of 0.5 or less and a kurtosis of 5 or less. Use of these seed crystals improves the bonding of zeolite crystals when producing the zeolite membrane. As a result, a dense zeolite membrane can be formed.

First claim

The invention claimed is:

1. A zeolite seed crystal that is to be deposited on a support when producing a zeolite membrane complex that includes said support and a zeolite membrane formed on said support,
a volume-cumulative particle size distribution of said zeolite seed crystal, measured by a laser diffraction scattering method, having a coefficient of variation of 0.5 or less and a kurtosis of 5 or less.

2. The zeolite seed crystal according to claim 1 , wherein
said coefficient of variation is 0.4 or less, and
said kurtosis is 3 or less.

3. The zeolite seed crystal according to claim 1 , wherein
in an X-ray diffraction pattern obtained by X-ray irradiation to said seed crystal, an intensity of a crystalline component at a diffraction angle 2θ at which a maximum peak appears within a range of the diffraction angle 2θ of 12° to 25° is 35 times or more an intensity of an amorphous component.

4. The zeolite seed crystal according to claim 1 , wherein
said zeolite seed crystal has a specific surface area of 10 m 2 /g or more and 150 m 2 /g or less.

5. The zeolite seed crystal according to claim 1 , wherein
said support is porous.

6. The zeolite seed crystal according to claim 5 , wherein
a 50% diameter of said volume-cumulative particle size distribution is 1.1 times or more and 5 times or less a 50% diameter of a volume-cumulative pore size distribution of said support.

7. The zeolite seed crystal according to claim 1 , wherein
said support is an alumina sintered compact or a mullite sintered compact.

8. A method of producing a zeolite seed crystal that is to be deposited on a support when producing a zeolite membrane complex that includes said support and a zeolite membrane formed on said support, the method comprising:
operation a) synthesizing an original crystal group of zeolite by hydrothermal synthesis and acquiring an intermediate crystal group from said original crystal group; and
operation b) acquiring a crystal group as seed crystals from said intermediate crystal group, the crystal group being determined to have a volume-cumulative particle size distribution having a coefficient of variation of 0.5 or less and a kurtosis of 5 or less, the volume-cumulative particle size distribution being measured by a laser diffraction scattering method.

9. The method of producing a zeolite seed crystal according to claim 8 , wherein
in said operation b), said seed crystals are a crystal group extracted from said intermediate crystal group.

10. The method of producing a zeolite seed crystal according to claim 9 , wherein
in said operation b), said seed crystals are extracted by classification of said intermediate crystal group by centrifugal separation.

11. The method of producing a zeolite seed crystal according to claim 8 , wherein
said operation a) includes:
operation a1) synthesizing said original crystal group by hydrothermal synthesis;
operation a2) pulverizing said original crystal group; and
operation a3) acquiring said intermediate crystal group by recrystallization of said original crystal group pulverized in said operation a2).

12. A method of producing a zeolite membrane complex, comprising:
d) preparing a support;
e) producing a seed-crystal-deposited support by depositing seed crystals produced by the method of producing a zeolite seed crystal according to claim 8 on said support; and
f) immersing said seed-crystal-deposited support in a starting material solution and growing zeolite from said seed crystals by hydrothermal synthesis to form a zeolite membrane on said support.

13. A separation method comprising:
g) preparing a zeolite membrane complex produced by the method of producing a zeolite membrane complex according to claim 12 ; and
h) supplying a mixture of substances including a plurality of types of gases or liquids to said zeolite membrane complex and allowing a high-permeability substance in said mixture of substances to permeate through said zeolite membrane complex to separate said high-permeability substance from other substances.

14. The separation method according to claim 13 , wherein
said mixture of substances includes at least one of following substances: hydrogen, helium, nitrogen, oxygen, water, steam, carbon monoxides, carbon dioxides, nitrogen oxides, ammonia, sulfur oxides, hydrogen sulfides, sulfur fluorides, mercury, arsine, hydrocyanic acids, carbonyl sulfides, C1 to C8 hydrocarbons, organic acids, alcohol, mercaptans, ester, ether, ketone, and aldehyde.

Assignees

• Ngk Insulators Ltd

Inventors

• Kobayashi Ko
• Yoshimura Ryotaro
• Noda Kenichi

Classifications

• B01J20/08

  comprising aluminium oxide or hydroxide; comprising bauxite · CPC title

• B01J20/183

  Physical conditioning without chemical treatment, e.g. drying, granulating, coating, irradiation · CPC title

• C01B39/54 Primary

  Phosphates, e.g. APO or SAPO compounds · CPC title

• C01B37/02

  Crystalline silica-polymorphs, e.g. silicalites {dealuminated aluminosilicate zeolites} · CPC title

• C01P2002/90

  Other crystal-structural characteristics not specified above · CPC title