# US 10,118,160 B2 · Process for preparing a hydrotreating catalyst

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- Number: US 10,118,160 B2
- Document ID: US10118160B2
- Status: Granted
- Kind: B2
- Application number: 15/033,927
- Filed: 2014-11-04
- Published: 2016-09-15
- Granted: 2018-11-06
- Earliest claimed: 2013-11-07
- Assignees: Shell Oil Company
- Applicants: Shell Oil Company
- Inventors: Ferry Winter; Jan Arend Van Welsenes; Marcello Stefano Rigutto; Patricia Johanna Anne Maria Giltay; Johannes Jacobus Maria Van Vlaanderen; Ali Azghay
- Web page: https://patentgrep.com/patent/US10118160B2

## CPC

- B01J 27/19: Molybdenum
- B01J 21/04: Alumina
- B01J 23/883: and nickel
- B01J 35/19: {Catalysts containing parts with different compositions}
- B01J 35/32: Bulk density
- B01J 37/0201: {Impregnation}
- B01J 37/0203: {the impregnation liquid containing organic compounds}
- B01J 37/0205: {in several steps}
- B01J 37/0207: {Pretreatment of the support}
- B01J 37/0215: {Coating}
- B01J 37/0236: {Drying, e.g. preparing a suspension, adding a soluble salt and drying}
- B01J 37/024: {Multiple impregnation or coating}
- B01J 37/08: Heat treatment {(B01J37/0009, B01J37/0018 take precedence)}
- B01J 37/088: {Decomposition of a metal salt}
- B01J 37/20: Sulfiding
- C10G 45/08: in combination with chromium, molybdenum, or tungsten metals, or compounds thereof
- B01J 31/0202: {Alcohols or phenols}
- B01J 31/04: containing carboxylic acids or their salts {(B01J31/0277 - B01J31/0298 take precedence; multi-metal carboxylate complexes like Pd (II) acetate, i.e. Pd3 (OAc) 6 or Cr(II)acetate, i.e. Cr2(OAc)4 B01J31/2226)}
- B01J 35/50: characterised by their shape or configuration
- B01J 35/615: {100-500 m2/g}
- B01J 35/647: {2-50 nm}
- B01J 37/0018: {Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)}
- B01J 37/086: {Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid}
- B01J 37/28: Phosphorising
- B01J 2523/00: Constitutive chemical elements of heterogeneous catalysts
- 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

Process for preparing a hydrotreating catalyst comprising of from 5 wt % to 50 wt % of molybdenum, of from 0.5 wt % to 20 wt % of nickel and of from 0 to 5 wt % of phosphorus, all based on total dry weight of catalyst, which process comprises (a) treating alumina carrier with molybdenum and nickel and of from 1 to 60% wt of gluconic acid, based on weight of carrier, and optionally phosphorus, (b) optionally drying the treated carrier at a temperature of from 40 to 200° C., and (c) calcining the treated and optionally dried carrier at a temperature of from 200 to 650° C. to obtain the calcined treated carrier.

## Claims

### Claim 1

A process for preparing a hydrotreating catalyst, wherein the hydrotreating catalyst comprises from 5 wt % to 50 wt % molybdenum, from 0.5 wt % to 20 wt % nickel, and from 0 to 5 wt % phosphorus, all based on total dry weight of catalyst, which process comprises:
impregnating an alumina carrier with an impregnation solution, consisting essentially of a phosphorus compound, a molybdenum component, a nickel component, and gluconic acid that is present in the impregnation solution in such an amount to provide a ratio of weight of gluconic acid to the total weight of nickel and molybdenum of from 0.1 to 5, and a phosphorus compound, to thereby provide an impregnated carrier;
drying the impregnated carrier at a temperature of from 40 to 200° C. followed by calcining the impregnated carrier at a temperature of from 200 to 650° C. to obtain a calcined impregnated carrier; and
sulphiding the calcined impregnated carrier to obtain the hydrotreating catalyst.

### Claim 2 (depends on 1)

A process according to claim 1, wherein the amount of gluconic acid in the hydrotreating catalyst is of from 2 to 40% wt, based on total dry weight of the alumina carrier.

### Claim 3 (depends on 2)

A process according to claim 2, wherein the amount of phosphorus in the hydrotreating catalyst is of from 1.5 to 3.5% wt, based on total dry weight of hydrotreating catalyst.

### Claim 4 (depends on 1)

A process according to claim 1, wherein the hydrotreating catalyst comprising from 1 wt % to 15 wt % nickel, of from 8 wt % to 40 wt % molybdenum and of from 0.1 to 5 wt % phosphorus, all metal based on total dry weight of hydrotreating catalyst.

### Claim 5 (depends on 4)

A process according to claim 4, in which the alumina of the alumina carrier is gamma alumina.

### Claim 6 (depends on 4)

A process for hydrotreating a sulphur-containing hydrocarbon feedstock, which process comprises: contacting the hydrocarbon feedstock at a hydrogen partial pressure from 1 to 70 bar and a temperature of from 200 to 420° C. with a catalyst obtained according to claim 4.

### Claim 7 (depends on 1)

A process for hydrotreating a sulphur-containing hydrocarbon feedstock, which process comprises: contacting the hydrocarbon feedstock at a hydrogen partial pressure from 1 to 70 bar and a temperature of from 200 to 420° C. with a catalyst obtained according to claim 1.

### Claim 8 (depends on 1)

A process according to claim 1, wherein the gluconic acid concentration of the impregnation solution is such to provide the ratio of gluconic acid to total weight of nickel and molybdenum is of from 0.3 to 2.5.

### Claim 9 (depends on 1)

A process according to claim 1, wherein the gluconic acid concentration of the impregnation solution is such to provide the ratio of gluconic acid to total weight of nickel and molybdenum is of from 0.5 to 2.

### Claim 10 (depends on 9)

A process according to claim 9, wherein the amount of gluconic acid in the impregnated carrier is of from 3 to 30% wt, based on the total dry weight of the alumina carrier.

### Claim 11 (depends on 10)

A process according to claim 10, wherein the hydrotreating catalyst comprising from 2 wt % to 12 wt % nickel, of from 10 wt % to 30 wt % molybdenum and of from 0.2 to 5 wt % phosphorus, all metal based on total dry weight of hydrotreating catalyst.

### Claim 12 (depends on 11)

A process for hydrotreating a sulphur-containing hydrocarbon feedstock, which process comprises: contacting the hydrocarbon feedstock at a hydrogen partial pressure from 1 to 70 bar and a temperature of from 200 to 420° C. with a catalyst obtained according to claim 11.

### Claim 13 (depends on 1)

A process according to claim 1, wherein the gluconic acid concentration of the impregnation solution is such to provide the ratio of gluconic acid to total weight of nickel and molybdenum is of from 0.7 to 1.5.

### Claim 14 (depends on 13)

A process according to claim 13, wherein the amount of gluconic acid in the impregnated carrier is of from 4 to 20% wt, based on the total dry weight of the alumina carrier.

### Claim 15 (depends on 14)

A process according to claim 14, wherein the hydrotreating catalyst comprising from 2 wt % to 12 wt % nickel, of from at least 11 wt % to 30 wt % molybdenum and of from 0.5 to 4.5 wt % phosphorus, all metal based on total dry weight of hydrotreating catalyst.

### Claim 16 (depends on 15)

A process for hydrotreating a sulphur-containing hydrocarbon feedstock, which process comprises: contacting the hydrocarbon feedstock at a hydrogen partial pressure from 1 to 70 bar and a temperature of from 200 to 420° C. with a catalyst obtained according to claim 15.