Method for preparing a catalyst containing an active nickel phase distributed in a shell and a nickel-copper alloy

Patent metadata

Field	Value
Publication number	US-12551872-B2
Application number	US-202117923353-A
Country	US
Kind code	B2
Filing date	May 18, 2021
Priority date	May 29, 2020
Publication date	Feb 17, 2026
Grant date	Feb 17, 2026

Abstract

A process for preparing a catalyst comprising nickel and copper, comprising the following steps:
impregnating the porous support with a volume of a butanol solution of between 0.2 and 0.8 times the total pore volume of the support; maturing the impregnated porous support for 0.5 to 40 hours; impregnating the matured impregnated support with a solution comprising a precursor of the nickel active phase; impregnating the support with a solution containing a copper precursor and a nickel precursor.

First claim

The invention claimed is:

1 . A process for preparing a catalyst comprising nickel and copper, in a proportion of 1% and 50% by weight of nickel element relative to the total weight of the catalyst, and in a proportion of 0.5% to 15% by weight of copper element relative to the total weight of the catalyst, and a porous alumina support, the support having a core and a crust at a periphery thereof, the nickel being distributed both over a crust at the periphery of the support, and at the core of the support, the thickness of said crust being between 2% and 15% of the diameter of the catalyst, the size of the nickel particles in the catalyst, measured in oxide form, being between 7 nm and 25 nm, said process comprises the following steps:
a) either the porous support or the catalyst precursor obtained at the end of step d) is impregnated with a volume V1 of a butanol solution of between 0.2 and 0.8 times the total pore volume TPV of said support in order to obtain an impregnated support; b) the impregnated porous support obtained at the end of step a) is left to mature for 0.5 hour to 40 hours; c) the sequence of the following sub-steps is carried out:
c1) either the matured impregnated porous support obtained at the end of step b), or the catalyst precursor obtained at the end of step d), is impregnated with a solution comprising at least one precursor of the nickel active phase;
c2) optionally, the catalyst precursor obtained at the end of step c1) is dried at a temperature below 250° C.;
d) the sequence of the following sub-steps is carried out:
d1) either the porous support, or the matured impregnated porous support obtained at the end of step b), or the catalyst precursor obtained at the end of step c), is impregnated with at least one solution containing at least one copper precursor and one nickel precursor at a copper concentration in order to obtain, on the final catalyst, a content of between 0.5% and 15% by weight of copper element relative to the total weight of the final catalyst;
d2) optionally, the catalyst precursor obtained at the end of step d1) is dried at a temperature below 250° C.;
said step d) being carried out either before step a), or between steps b) and c), or after step c), it being understood that:
i) when step d) is carried out before step a), then sub-steps c2) and d2) are compulsory;
ii) when step d) is carried out between steps b) and c), then sub-step c2) is compulsory;
iii) when step d) is carried out after step c), then sub-step d2) is compulsory.

2 . The process as claimed in claim 1 , wherein step b) is carried out at a temperature below or equal to 60° C.

3 . The process as claimed in claim 1 , wherein, in step a), an n-butanol solution is used.

4 . The process as claimed in claim 1 , wherein, when step d) is carried out before step a), the volume V2 of the solution comprising at least one precursor of the nickel active phase supplied in step c1) is such that V2=TPV−V1.

5 . The process as claimed in claim 1 , wherein, when step d) is carried out between steps b) and c), or after step c), the volume V2 of the solution comprising at least one precursor of the nickel active phase supplied in step c1) and the volume V3 of the solution comprising a nickel precursor and a copper precursor supplied in step d1) are such that V2+V3=TPV−V1.

6 . The process as claimed in claim 1 , wherein the copper precursor is copper acetate, copper acetylacetonate, copper nitrate, copper sulfate, copper chloride, copper bromide, copper iodide or copper fluoride.

7 . The process as claimed in claim 1 , wherein the precursor of the nickel active phase is nickel nitrate, nickel chloride, nickel acetate or nickel hydroxycarbonate.

8 . The process as claimed in claim 1 , said process further comprises a step c2′) of calcining the dried catalyst precursor obtained at the end of step c2) at a temperature of between 250° C. and 600° C.

9 . The process as claimed in claim 1 , wherein, in step a), said volume V1 of said butanol solution is between 0.25 and 0.75 times the total pore volume TPV of said support.

10 . The process as claimed in claim 1 , wherein sub-steps c2) and/or d2) are carried out for a time of between 0.5 hour and 12 hours.

11 . The process as claimed in claim 1 , further comprising a step e) wherein the catalyst precursor obtained at the end of the sequence of steps a) to d) is reduced by bringing said catalyst precursor into contact with a reducing gas at a temperature above or equal to 150° C. and below 250° C.

12 . The process as claimed in claim 1 , wherein step d) is carried out before step a).

13 . The process as claimed in claim 1 , wherein step d) is carried out between steps b) and c).

14 . The process as claimed in claim 1 , wherein step d) is carried out after step c).

Assignees

• Ifp Energies Now

Inventors

• Boualleg Malika

Classifications

• B01J35/397

  Egg shell like · CPC title

• C07C2523/755

  Nickel · CPC title

• C07C2523/72

  Copper · CPC title

• C07C5/10

  of aromatic six-membered rings · CPC title

• B01J37/0207

  Pretreatment of the support · CPC title