Method for manufacturing zeolite and method for manufacturing epsilon-caprolatam

• US 20060004194A1
• Filed: 06/24/2005
• Published: 01/05/2006
• Est. Priority Date: 06/30/2004
• Status: Active Grant

• Current Assignee: Sumitomo Chemical Company Limited
• Original Assignee: Sumitomo Chemical Company Limited
• Inventors: Sugita, Keisuke, Kitamura, Masaru, Hoshino, Masahiro
• Granted Patent: US 7,060,645 B2
• Time in Patent Office: Days
• US Class Current: 540/536
• CPC Class Codes: B01J 2229/38 Base treatment
• CPC Class Codes: B01J 2229/40 Special temperature treatment, i.e. other than just for template removal
• CPC Class Codes: B01J 29/035 Microporous crystalline materials not having base exchange properties, such as silica polymorphs, e.g. silicalites
• CPC Class Codes: B01J 37/06 Washing B01J37/0009, B01J37/0018 take precedence
• CPC Class Codes: C01B 37/02 Crystalline silica-polymorphs, e.g. silicalites dealuminated aluminosilicate zeolites
• CPC Class Codes: C07D 201/04 from or via oximes by Beckmann rearrangement

Abstract

The present invention provides a method for manufacturing a zeolite comprising following steps of: (1): calcining crystals obtained by hydrothermal synthesis reaction of a silicon compound; (2): contact treating a calcined product obtained by the step (1) with an aqueous solution including an amine and/or a quaternary ammonium compound; (3): calcining a treated product obtained by the step (2); and (4): contact treating the calcined product obtained by the step (3) with an aqueous solution including ammonia and/or an ammonium salt. According to the present invention, a method is also provided wherein ε-caprolactam is manufactured by Beckmann rearrangement reaction of cyclohexanone oxime in a gaseous phase in the presence of the zeolite manufactured by the above-described method.

Claims

1. A method for manufacturing a zeolite comprising following steps of:

(1);

calcining crystals obtained by hydrothermal synthesis reaction of a silicon compound;

(2);

contact treating a calcined product obtained by the step (1) with an aqueous solution including an amine and/or a quaternary ammonium compound;

(3);

calcining a treated product obtained by the step (2); and

(4);

contact treating the calcined product obtained by the step (3) with an aqueous solution including ammonia and/or an ammonium salt.

2. The method for manufacturing a zeolite according to claim 1, wherein the zeolite is a pentasil type zeolite.

3. The method for manufacturing a zeolite according to claim 1, wherein the aqueous solution used in the step (2) is an aqueous solution including a quaternary ammonium hydroxide.

4. The method for manufacturing a zeolite according to claim 1, wherein a temperature of the contact treating in the step (2) is not more than 100°

C.

5. A method for manufacturing ε

-caprolactam wherein the ε

-caprolactam is manufactured by Beckmann rearrangement reaction of cyclohexanone oxime in a gaseous phase in the presence of the zeolite manufactured by the method according to claim 1.