# US 9,433,934 B2 · In-situ produced Y-faujasite from kaolin-derived, pre-shaped particles and the method of preparation and the use thereof

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- Number: US 9,433,934 B2
- Document ID: US9433934B2
- Status: Granted
- Kind: B2
- Application number: 13/899,816
- Filed: 2013-05-22
- Published: 2013-09-26
- Granted: 2016-09-06
- Earliest claimed: 2006-03-02
- Assignees: BASF SE
- Applicants: BASF Corporation
- Inventors: Xingtao Gao; David Stockwell; Gary M. Smith
- Web page: https://patentgrep.com/patent/US9433934B2

## CPC

- B01J 29/084: {Y-type faujasite}
- B01J 29/06: Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J 29/064: containing iron group metals, noble metals or copper
- B01J 29/106: {Y-type faujasite}
- B01J 29/166: {Y-type faujasite}
- B01J 35/40: characterised by dimensions, e.g. grain size (in a colloidal state B01J35/23; crystallite size B01J35/77)
- B01J 35/50: characterised by their shape or configuration
- C10G 45/02: to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G 47/16: Crystalline alumino-silicate carriers
- C10G 47/20: the catalyst containing other metals or compounds thereof
- C10G 65/12: including cracking steps and other hydrotreatment steps
- B01J 35/651: {50-500 nm}
- B01J 37/0009: {Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst}
- B01J 37/0045: {Drying a slurry, e.g. spray drying}
- B01J 37/0072: {Preparation of particles, e.g. dispersion of droplets in an oil bath}
- B01J 37/0215: {Coating}
- B01J 2229/64: in or on refractory materials
- B01J 2235/15: X-ray diffraction
- B01J 2235/30: Scanning electron microscopy; Transmission electron microscopy
- C10G 2400/02: Gasoline
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C10G: CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION (cracking to hydrogen or synthesis gas C01B; cracking or pyrolysis of hydrocarbon gases to individual hydrocarbons or mixtures thereof of definite or specified constitution C07C; cracking to cokes C10B); RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES

## Abstract

A zeolite-containing fixed bed catalyst is formed by pre-shaping a mixture of a reactive aluminum-containing component and a matrix component into pre-shaped particles, and contacting the pre-shaped particles with a reactive liquid containing a silicate for a sufficient time and temperature to form an in-situ zeolite within the pre-shaped particles. The contacting of the pre-shaped particles and the liquid is achieved such that there is relative movement between the pre-shaped particles and the liquid.

## Claims

### Claim 1

A process for preparing a zeolite-containing fixed bed catalyst, the process comprising:
shaping a first mixture of a reactive aluminum-containing component and one or more matrix-forming components into pre-shaped particles having a size suitable for fixed bed catalysis, wherein said shaping comprises extrusion; and
contacting said pre-shaped particles with a liquid containing a reactive silicate component for a time and a temperature sufficient to crystallize zeolite Y on said pre-shaped particles, wherein said contacting comprises providing velocity of at least one of said pre-shaped particles relative to said liquid or said liquid relative to said pre-shaped particles.

### Claim 2 (depends on 1)

The process of claim 1, wherein said reactive aluminum-containing component is metakaolin.

### Claim 3 (depends on 2)

The process of claim 2, wherein said pre-shaped particles comprise hydrous kaolin, and said pre-shaped particles are calcined so as to convert said hydrous kaolin to metakaolin.

### Claim 4 (depends on 1)

The process of claim 1, wherein said one or more matrix-forming components comprise at least one of kaolin calcined through exotherm of the kaolin to spinel, mullite, or alumina.

### Claim 5 (depends on 1)

The process of claim 1, wherein said liquid is contacted with said pre-shaped particles by circulating said liquid through a stationary bed of said pre-shaped particles.

### Claim 6 (depends on 1)

The process of claim 1, wherein said liquid is contacted with said pre-shaped particles by forming a second mixture of said pre-shaped particles in said liquid, and providing movement to said second mixture.

### Claim 7 (depends on 1)

The process of claim 1, wherein said liquid is contacted with said pre-shaped particles by providing said pre-shaped particles in a porous container, and moving said porous container within said liquid.

### Claim 8 (depends on 7)

The process of claim 7, wherein said porous container is a basket and said basket is rotated within said liquid.

### Claim 9 (depends on 1)

The process of claim 1, wherein said pre-shaped particles have a diameter of from about 0.05 to 0.5 inch, and a length of from about 0.05 to 1 inch.

### Claim 10 (depends on 1)

The process of claim 1, wherein said pre-shaped particles have a diameter of about 1/16th inch.

### Claim 11 (depends on 1)

The process of claim 1, wherein said one or more matrix-forming components are such to provide macropores within said pre-shaped particles, and wherein said zeolite Y is crystallized as a layer on walls of said macropores.

### Claim 12 (depends on 1)

The process of claim 1, wherein said catalyst comprises, subsequent to crystallization of said zeolite Y, at least 10 to 65 percent by weight of said zeolite Y.

### Claim 13 (depends on 1)

The process of claim 1, wherein said liquid comprises an aqueous solution of sodium silicate and sodium hydroxide.

### Claim 14 (depends on 13)

The process of claim 13, wherein said liquid further includes zeolite seeds.

### Claim 15 (depends on 1)

The process of claim 1, wherein said temperature sufficient to crystallize said zeolite Y on said pre-shaped particles is 70-120° Celsius, and said time sufficient to crystallize said zeolite Y on said pre-shaped particles is from 2 hours to 1 week.

### Claim 16 (depends on 1)

The process of claim 1, wherein said zeolite-containing fixed bed catalyst is treated to remove sodium ions from said crystallized zeolite Y.

### Claim 17 (depends on 15)

The process of claim 15, wherein said reactive aluminum-containing component is metakaolin.

### Claim 18 (depends on 17)

The process of claim 17, wherein said one or more matrix-forming components comprise at least one of kaolin calcined through exotherm of the kaolin to spinel, mullite, or alumina.