# US 9,873,111 B2 · Process for the preparation of a catalyst support

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- Number: US 9,873,111 B2
- Document ID: US9873111B2
- Status: Granted
- Kind: B2
- Application number: 15/431,962
- Filed: 2017-02-14
- Published: 2017-06-29
- Granted: 2018-01-23
- Earliest claimed: 2010-04-19
- Applicants: Shell Oil Company
- Inventors: László Domokos; Peter Geerinck; Aan Hendrik Klazinga
- Web page: https://patentgrep.com/patent/US9873111B2

## CPC

- B01J 29/44: Noble metals
- B01J 29/40: of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
- B01J 29/405: {containing rare earth elements, titanium, zirconium, hafnium, zinc, cadmium, mercury, gallium, indium, thallium, tin or lead}
- B01J 35/19: {Catalysts containing parts with different compositions}
- B01J 35/37: Crush or impact strength
- B01J 35/40: characterised by dimensions, e.g. grain size (in a colloidal state B01J35/23; crystallite size B01J35/77)
- B01J 35/60: characterised by their surface properties or porosity
- B01J 35/615: {100-500 m2/g}
- B01J 35/635: {0.5-1.0 ml/g}
- B01J 35/70: characterised by their crystalline properties, e.g. semi-crystalline (catalysts comprising carbon B01J21/18; molecular sieves B01J29/00)
- B01J 35/77: Compounds characterised by their crystallite size
- B01J 37/0009: {Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst}
- B01J 37/0207: {Pretreatment of the support}
- B01J 37/04: Mixing {(B01J37/0009, B01J37/0018 take precedence)}
- B01J 37/08: Heat treatment {(B01J37/0009, B01J37/0018 take precedence)}
- B01J 37/30: Ion-exchange
- C07C 4/18: Catalytic processes
- C07C 15/04: Benzene
- C10G 35/065: {containing crystalline zeolitic molecular sieves, other than aluminosilicates}
- C10G 35/09: Bimetallic catalysts in which at least one of the metals is a platinum group metal
- B01J 2229/16: to increase the Si/Al ratio; Dealumination
- B01J 2229/186: not in framework positions
- B01J 2229/20: to introduce other elements in the catalyst composition comprising the molecular sieve, but not specially in or on the molecular sieve itself
- B01J 2229/32: Reaction with silicon compounds, e.g. TEOS, siliconfluoride
- B01J 2229/42: Addition of matrix or binder particles
- C07C 2529/40: of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
- C07C 2529/44: Noble metals
- C10G 2300/1096: Aromatics or polyaromatics
- C10G 2400/30: Aromatics
- Y02P 20/52: using catalysts, e.g. selective catalysts
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- 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
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

Process for preparing a catalyst support which process comprises a) mixing pentasil zeolite having a bulk silica to alumina molar ratio in the range of from 20 to 150 with water, a silica source and an alkali metal salt, b) extruding the mixture obtained in step (a), c) drying and calcining the extrudates obtained in step (b), d) subjecting the calcined extrudates obtained in step (c) to ion exchange to reduce the alkali metal content, and e) drying the extrudates obtained in step (d); process for preparing a catalyst by furthermore impregnating such support with platinum in an amount in the range of from 0.001 to 0.1 wt % and tin in an amount in the range of from 0.01 to 0.5 wt %, each on the basis of total catalyst; ethylbenzene dealkylation catalyst obtainable thereby and a process for dealkylation of ethylbenzene which process comprises contacting feedstock containing ethylbenzene with such catalyst.

## Claims

### Claim 1

A process for preparing a catalyst, which process comprises:
a) mixing pentasil zeolite having a bulk silica to alumina molar ratio in the range of from 20 to 150 with water, a silica source and an alkali metal salt;
b) extruding the mixture obtained in step (a);
c) drying and calcining the extrudates obtained in step (b);
d) treating the extrudates obtained in step (c) with an aqueous solution of fluorosilicate salt to provide fluorosilicate-treated extrudates;
e) subjecting the fluorosilicate-treated extrudates obtained in step (d) to ion exchange with an aqueous ammonium containing solution to reduce the alkali metal content;
f) drying the extrudates obtained in step (e); and
g) impregnating the catalyst support with platinum in an amount in the range of from 0.001 to 0.1 wt % and tin in an amount in the range of from 0.01 to 0.5 wt %, each on the basis of total catalyst.

### Claim 2 (depends on 1)

A process as recited in claim 1, wherein the silica source is selected from the group consisting of powder form silica, silica sol, and mixtures of powder form silica and silica sol.

### Claim 3 (depends on 2)

A process as recited in claim 2, wherein silica source is a mixture of powder form silica and silica sol in a weight ratio of powder form silica-to-silica sol in the range of from 1:1 to 10:1, and wherein the powder form silica comprises small particulates having a mean particle size in the range of from 2 to 10 μm as measured by ASTM C690-1992.

### Claim 4 (depends on 3)

A process as recited in claim 3, wherein the catalyst support comprises silica in the range of from 30 to 80 wt % and zeolite in the range of from 20 to 70 wt %.

### Claim 5 (depends on 4)

A process as recited in claim 4, wherein the fluorosilicate salt is represented by the formula:
(A)2/bSiF6
wherein “A” is a metallic or non-non-metallic cation other than H+ having the valence “b”.

### Claim 6 (depends on 5)

A process as recited in claim 5, wherein the fluorosilicate salt is ammonium hexfluorosilicate (AHS).

### Claim 7 (depends on 6)

A process as recited in claim 6, wherein extrudates obtained in step (f) have a flat plate crush strength of at least 120 N·cm−1.

### Claim 8 (depends on 7)

A process as recited in claim 7, wherein extrudates obtained in step (f) have a B.E.T. surface area in the range of from 150 to 250 m2/g and a pore volume determined by mercury intrusion in the range of from 0.5 to 0.9 ml/g.

### Claim 9 (depends on 8)

A process as recited in claim 8, wherein the pentasil zeolite is ZSM-5 and is in the form of a powder comprising particles having diameters in the range of from 20 nm to 10 μm.