# US 10,370,256 B2 · Method for preparing a nanometric zeolite Y

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- Number: US 10,370,256 B2
- Document ID: US10370256B2
- Status: Granted
- Kind: B2
- Application number: 15/542,273
- Filed: 2016-01-07
- Published: 2018-01-11
- Granted: 2019-08-06
- Earliest claimed: 2015-01-08
- Assignees: Ifp Energies Nouvelles
- Applicants: IFP Energies nouvelles
- Inventors: Mathias Dodin; Nicolas Bats
- Web page: https://patentgrep.com/patent/US10370256B2

## CPC

- C01B 39/24: Type Y {(C01B39/205 takes precedence)}
- B01J 29/7007: {Zeolite Beta}
- C01B 39/20: Faujasite type, e.g. type X or Y
- B01J 37/04: Mixing {(B01J37/0009, B01J37/0018 take precedence)}
- B01J 37/10: in the presence of water, e.g. steam
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Preparation of a FAU-structural-type nanometric zeolite Y having a crystal size of less than 100 nm and an Si/Al ratio that is greater than 2: mixing, in aqueous medium, of at least one AO2 source of at least one tetravalent element A that is silicon, germanium, and/or titanium, at least one BOb source of at least one trivalent element B that is aluminum, boron, iron, indium, and/or gallium, at least one C2/mO source of an alkaline metal or alkaline-earth metal C that is lithium, sodium, potassium, calcium, and/or magnesium the C2/mO source also having at least one hydroxide ion source obtaining a gel, curing of the gel after at least 3 days of curing, with addition of at least one source of at least one tetravalent element A and the hydrothermal treatment of the gel obtained at a to achieve crystallization of the FAU-structural-type nanometric zeolite Y.

## Claims

### Claim 1

A method for preparation of a FAU-structural nanometric zeolite Y that has a crystal size of less than 100 nm and an Si/Al ratio that is greater than 2, with said method comprising at least the following:
i) mixing, in aqueous medium, of at least one AO2 source of at least one tetravalent element A that is silicon, germanium, or titanium, by itself or in a mixture, at least one BOb source of at least one trivalent element B that is aluminum, boron, iron, indium, or gallium, by itself or in a mixture, at least one C2/mO source of an alkaline metal or alkaline-earth metal C that is lithium, sodium, potassium, calcium, or magnesium, by itself or in a mixture, with said C2/mO source of alkaline metal or alkaline-earth metal C also comprising at least one hydroxide ion source, obtaining a gel, with the reaction mixture having the following molar composition:
v AO2:w BOb:x C2/mO:y H2O
with v being between 1 and 40,
with w being between 0.1 and 5,
with x being between 1 and 40,
with y being between 30 and 1000,
with b being between 1 and 3, b being a whole number or a rational number,
with m being equal to 1 or 2,
ii) curing of the gel obtained at the end of (i) at a temperature of between −15° C. and 60° C., with or without stirring, for a time period of between 1and 60 days,
iii) after at least 3 days of curing, a step consisting of a one-time or repeated addition of at least one AO2 source of at least one tetravalent element A that is silicon, germanium, or titanium, by itself or in a mixture, in said gel, with the molar composition of the gel at the end of the addition being as follows:
vAO2:wBOb:xC2/mO:yH2O
with v being between 5 and 50,
with w being between 0.1 and 5,
with x being between 1 and 40,
with y being between 200 and 1000,
with b being between 1 and 3, b being a whole number or a rational number,
with m being equal to 1 or 2,
(iv) hydrothermal treatment of the gel that is obtained at the end of (iii) at a temperature of between 20° C. and 200° C., under autogenous reaction pressure, for a time period of between 1 hour and 14 days, to obtain crystallization of said FAU-structural nanometric zeolite Y.

### Claim 2 (depends on 1)

The method according to claim 1, in which A is silicon.

### Claim 3 (depends on 1)

The method according to claim 1, in which B is aluminum.

### Claim 4 (depends on 1)

The method according to claim 1, in which C is sodium.

### Claim 5 (depends on 1)

The method according to claim 1, in which the reaction mixture in (i) has the following molar composition:
v AO2:w BOb:x C2/mO:y H2O
with v being between 15 and 20,
with w being between 0.2 and 1.5,
with x being between 1 and 20,
with y being between 100 and 400,
with b being between 1 and 3, b being a whole number or a rational number,
with m being equal to 1 or 2,
where A, B and C have the same definition as above.

### Claim 6 (depends on 1)

The method according to claim 1, in which seeds comprising FAU-structural zeolite crystals are added during mixing in (i).

### Claim 7 (depends on 1)

The method according to claim 1, in which the tetravalent element A added in curing in (iii) is identical to the tetravalent element A that is added in mixing in (i).

### Claim 8 (depends on 1)

The method according to claim 1, in which the one-time or repeated addition of at least one source of at least one tetravalent element A is carried out during the curing (ii).

### Claim 9 (depends on 8)

The method according to claim 8, in which the one-time or repeated addition of at least one source of at least one tetravalent element A is carried out after at least 5 days of curing.

### Claim 10 (depends on 1)

The method according to claim 1, in which the one-time or repeated addition of at least one source of at least one tetravalent element A is carried out after curing in (ii).

### Claim 11 (depends on 1)

The method according to claim 1, in which the molar composition of the gel at the end of the addition in (iii) is as follows:
v AO2:w BOb:x C2/mO:y H2O
with v being between 20 and 30,
with w being between 0.2 and 1.5,
with x being between 1 and 20,
with y being between 200 and 500,
with b being between 1 and 3, b being a whole number or a rational number,
with m being equal to 1 or 2,
where A, B and C have the same definition as above.

### Claim 12 (depends on 1)

The method according to claim 1, in which the FAU-structural nanometric zeolite Y that is formed at the end of (iv) is filtered, washed, and then dried at a temperature of between 20° C. and 150° C.

### Claim 13 (depends on 12)

The method according to claim 12, in which said zeolite that is obtained at the end of drying undergoes at least one calcination and at least one ion exchange.

### Claim 14 (depends on 1)

The method according to claim 1, in which the tetravalent element A added in curing in (iii) is different from the tetravalent element A that is added in mixing in (i).

### Claim 15 (depends on 1)

The method according to claim 1, wherein (iii) consists of, after at least 3 days of curing, one time addition of and AO2 source of one tetravalent element A.

### Claim 16

A method for preparation of a FAU-structural nanometric zeolite Y that has a crystal size of less than 100 nm and an Si/Al ratio that is greater than 2, with said method consisting of:
i) mixing, in aqueous medium, of at least one AO2 source of at least one tetravalent element A that is silicon, germanium, or titanium, by itself or in a mixture, at least one BOb source of at least one trivalent element B that is aluminum, boron, iron, indium, or gallium, by itself or in a mixture, at least one C2/mO source of an alkaline metal or alkaline-earth metal C that is lithium, sodium, potassium, calcium, or magnesium, by itself or in a mixture, with said C2/mO source of alkaline metal or alkaline-earth metal C also comprising at least one hydroxide ion source, obtaining a gel, with the reaction mixture having the following molar composition:
v AO2:w BOb:x C2/mO:y H2O
with v being between 1 and 40,
with w being between 0.1 and 5,
with x being between 1 and 40,
with y being between 30 and 1000,
with b being between 1 and 3, b being a whole number or a rational number,
with m being equal to 1 or 2,
ii) curing of the gel obtained at the end of (i) at a temperature of between −15° C. and 60° C., with or without stirring, for a time period of between 1and 60 days,
iii) after at least 3 days of curing, a one-time or repeated addition of at least one AO2 source of at least one tetravalent element A that is silicon, germanium, or titanium, by itself or in a mixture, in said gel, with the molar composition of the gel at the end of the addition being as follows:
v AO2:w BOb:x C2/mO:y H2O
with v being between 5 and 50,
with w being between 0.1 and 5,
with x being between 1 and 40,
with y being between 200 and 1000,
with b being between 1 and 3, b being a whole number or a rational number,
with m being equal to 1 or 2,
(iv) hydrothermal treatment of the gel that is obtained at the end of (iii) at a temperature of between 20° C. and 200° C., under autogenous reaction pressure, for a time period of between 1 hour and 14 days, to obtain crystallization of said FAU-structural nanometric zeolite Y.