Zeolite production method

Patent metadata

Field	Value
Publication number	US-10308516-B2
Application number	US-201614990431-A
Country	US
Kind code	B2
Filing date	Jan 7, 2016
Priority date	Jul 9, 2013
Publication date	Jun 4, 2019
Grant date	Jun 4, 2019

Abstract

Provided is a method for continuous production of zeolite in which a starting material is continuously supplied to a tubular reactor to produce an aluminophosphate zeolite that contains, in the framework structure, at least aluminum atoms and phosphorus atoms or an aluminosilicate zeolite having 5≤SiO 2 /Al 2 O 3 ≤2000. The tubular reactor is heated using a heat medium; a ratio (volume)/(lateral surface area) of the volume (inner capacity) to the lateral surface area of the tubular reactor is 0.75 cm or smaller; and seed crystals are added to the starting material. Through using a small-diameter tubular reactor and heating with a heat medium, it becomes possible to heat sufficiently the entirety of a starting material (zeolite precursor gel) in a short time, and to allow reaction to proceed at a high rate. The occurrence of irregular pressure fluctuations during continuous production of the zeolite can be prevented by adding seed crystals.

First claim

The invention claimed is:

1. A method for continuous production of zeolite, wherein
a starting material is continuously supplied to a tubular reactor to produce an aluminophosphate zeolite that contains, in a framework structure, at least aluminum atoms and phosphorus atoms or an aluminosilicate zeolite having 5≤SiO 2 /Al 2 O 3 ≤2000,
the starting material comprises a zeolite precursor gel,
the tubular reactor is heated using a heat medium,
a ratio (volume)/(lateral surface area) of the volume (inner capacity) to the lateral surface area of the tubular reactor is 0.75 cm or smaller, and
seed crystals and a template are added to the starting material.

2. The method for continuous production of zeolite according to claim 1 , wherein after heating of the starting material that is supplied into the tubular reactor, the zeolite precursor gel is further added to an intermediate product in the tubular reactor, so as to come into contact with the starting material after heating.

3. The method for continuous production of zeolite according to claim 1 , wherein the zeolite structure of the zeolite, as established by IZA, is AFI.

4. The method for continuous production of zeolite according to claim 1 , wherein the zeolite structure of the zeolite, as established by IZA, is CHA.

5. The method for continuous production of zeolite according to claim 1 , wherein the starting material is aged for 2 hours or longer.

6. The method for continuous production of zeolite according to claim 1 , wherein the framework density of the zeolite ranges from 12.0 T/1,000 Å 3 to 17.5 T/1,000 Å 3 .

7. The method for continuous production of zeolite according to claim 1 , wherein the zeolite comprises a transition metal.

8. The method for continuous production of zeolite according to claim 1 , wherein the tubular reactor comprises an independent tubular reactor having an openable and closable lid; the starting material is supplied to the tubular reactor and the lid is closed; thereafter, the tubular reactor is heated by being placed in the heat medium; and thereafter, the tubular reactor is retrieved from the heat medium, the lid is opened, and a product is retrieved.

9. The method for continuous production of zeolite according to claim 1 , wherein the tubular reactor comprises an independent tubular reactor having an openable and closable lid; the starting material is supplied to the tubular reactor and the lid is closed; thereafter, the tubular reactor is heated by being placed in the heat medium; and thereafter, the tubular reactor is retrieved from the heat medium, the lid is opened, a product is retrieved, and the product is kept at a lower temperature than during reaction.

10. The method for continuous production of zeolite according to claim 1 , wherein
in case of production of aluminophosphate zeolite, the zeolite precursor gel contains an aluminum source and a phosphorus source, and
in case of production of aluminosilicate zeolite, the zeolite precursor gel contains an aluminum source and a silicon source.

11. The method for continuous production of zeolite according to claim 1 , wherein an average particle size of the seed crystals is in a range of 0.1 μm or greater and 100 μm or smaller.

12. A method for continuous production of zeolite, wherein
a starting material is supplied into a tubular reactor, followed by heating the tubular reactor with a heat medium, to produce an aluminophosphate zeolite that contains, in a framework structure, at least aluminum atoms and phosphorus atoms or an aluminosilicate zeolite having 5≤SiO 2 /Al 2 O 3 ≤2000 (molar ratio), wherein a diameter of the tubular reactor is set to be equal to or smaller than 3 cm,
the starting material comprises a zeolite precursor gel,
and seed crystals and a template are added to the starting material.

Assignees

• Mitsubishi Chem Corp
• Univ Tokyo

Inventors

• Okubo Tatsuya
• Wakihara Toru
• Liu Zhendong
• Takewaki Takahiko
• Oshima Kazunori
• Nishioka Daisuke

Classifications

• C01B39/48

  using at least one organic template directing agent · CPC title

• C01B39/04

  using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound · CPC title

• C01B39/54 Primary

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

• B01J29/763

  CHA-type, e.g. Chabazite, LZ-218 · CPC title

• B01J19/243

  spirally, concentrically or zigzag wound · CPC title