# US 2016/0355467 A1 · Titanium-silicalite molecular sieve, method for preparing the same and method for preparing cyclohexanone oxime using the molecular sieve

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- Number: US 2016/0355467 A1
- Document ID: US20160355467A1
- Status: Published application
- Kind: A1
- Application number: 15/241,947
- Filed: 2016-08-19
- Published: 2016-12-08
- Earliest claimed: 2011-08-11
- Assignees: China Petrochemical Development Corporation
- Applicants: China Petrochemical Development Corporation
- Inventors: Ya-Ping Chen; Cheng-Fa Hsieh; Pin-To Yao; Chien-Chang Chiang
- Web page: https://patentgrep.com/patent/US20160355467A1

## CPC

- C07C 249/04: of oximes
- B01J 29/89: Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium {(B01J29/005 takes precedence)}
- C01B 37/005: {Silicates, i.e. so-called metallosilicalites or metallozeosilites}
- C07C 251/44: with the carbon atom of at least one of the oxyimino groups being part of a ring other than a six-membered aromatic ring
- B01J 29/87: Gallosilicates; Aluminogallosilicates; Galloborosilicates {(B01J29/005 takes precedence)}
- B01J 2229/183: in framework positions
- C01B 39/06: Preparation of isomorphous zeolites characterised by measures to replace the aluminium or silicon atoms in the lattice framework by atoms of other elements {, i.e. by direct or secondary synthesis}
- C01B 39/082: {Gallosilicates}
- C01B 39/085: {Group IVB- metallosilicates}
- C07C 2601/14: The ring being saturated
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}

## Abstract

The present invention provides a titanium-silicalite molecular sieve and a method for preparing the same. The method includes the steps of preparing a mixture of a titanium source, a silicon source, a metal source selected from IIA to IVA elements and a template agent; heating the mixture to form a gel mixture; heating the gel mixture in a water bath; and calcining the gel mixture after the gel mixture in the water bath to form the titanium-silicalite molecular sieve. The present invention further provides a method for preparing cyclohexanone oxime by using the titanium-silicalite molecular sieve as the catalyst which results in high conversion rate, high selectivity and high usage efficiency of hydrogen peroxide.

## Claims

### Claim at position 1

1-15. (canceled)

### Claim 16

A titanium-silicalite molecular sieve, comprising:
a silicon oxide;
a titanium oxide; and
a metal oxide, wherein a metal of the metal oxide is at least one selected from IIA to IVA elements, a molar ratio of titanium to silicon is in a range of from 0.005 to 0.1, and a molar ratio of the metal to the silicon is in a range of from 0.00001 to 0.05.

### Claim 17 (depends on 16)

The titanium-silicalite molecular sieve of claim 16, wherein the metal of the metal oxide is positioned inside or outside a skeleton of the titanium-silicalite molecular sieve.

### Claim 18 (depends on 16)

A method for preparing cyclohexanone oxime, comprising the step of:
performing a reaction of cyclohexanone, ammonia and hydrogen peroxide in the presence of a titanium-silicalite molecular sieve of claim 16 as a catalyst and a solvent.

### Claim 19 (depends on 18)

The method of claim 18, wherein a molar ratio of the ammonia to the cyclohexanone is in a range of from 1.1:1 to 2:1.

### Claim 20 (depends on 18)

The method of claim 18, wherein a molar ratio of the hydrogen peroxide to the cyclohexanone is in a range of from 0.7:1 to 2.5:1.

### Claim 21 (depends on 18)

The method of claim 18, wherein the solvent is one or more selected from the group consisting of an alcohol, a ketone and water.

### Claim 22 (depends on 21)

The method of claim 21, wherein the solvent is tert-butanol.

### Claim 23 (depends on 18)

The method of claim 18, wherein an amount of the titanium-silicalite molecular sieve is 0.1 to 10 wt % of a total weight of the cyclohexanone, the ammonia and the hydrogen peroxide.