Heavy metal capture mass with improved performances

Patent metadata

Field	Value
Publication number	US-10456770-B2
Application number	US-201715627490-A
Country	US
Kind code	B2
Filing date	Jun 20, 2017
Priority date	Jun 21, 2016
Publication date	Oct 29, 2019
Grant date	Oct 29, 2019

Abstract

A capture mass for heavy metals, in particular mercury, contained in a gaseous or liquid feed, said mass comprising:
copper which is present at least in part in the sulphide form, Cu x S y ; a porous support based on alumina;

characterized in that said porous support has a total pore volume (TPV) in the range 0.8 to 1.5 cm 3 /g, a mesopore volume (V 6nm-100nm ) in the range 0.5 to 1.3 cm 3 /g, and a macropore volume (V 100nm ) in the range 0.33 to 0.45 cm 3 /g,

it being understood that the ratio between the mesopore volume and the macropore volume (V 6nm-100nm /V 100nm ) is in the range 1 to 5.

First claim

The invention claimed is:

1. A capture mass capable of capturing heavy metals including mercury, contained in a gaseous or liquid feed, said mass comprising:
copper which is present at least in part in the sulphide form, Cu x S y ;
a porous support based on alumina;
said porous support having a total pore volume (TPV) in the range 0.8 to 1.5 cm 3 /g, a mesopore volume (V 6nm-100nm ) in the range 0.5 to 1.3 cm 3 /g, a macropore volume (V 100nm ) in the range 0.33 to 0.45 cm 3 /g, and a
ratio between the mesopore volume and the macropore volume (V 6nm-100nm /V 100nm ) of 1 to 1.86.

2. The capture mass as claimed in claim 1 , having a copper content, expressed in terms of oxides, in the range 15% to 40% by weight with respect to the total weight of said capture mass.

3. A capture mass capable of capturing heavy metals including mercury, contained in a gaseous or liquid feed, said mass comprising:
copper which is present at least in part in the sulphide form, Cu x S y ;
a porous support based on alumina;
said porous support having a total pore volume (TPV) in the range 0.8 to 1.5 cm 3 /g, a mesopore volume (V 6nm-100nm ) in the range 0.5 to 1.3 cm 3 /g, a macropore volume (V 100nm ) in the range 0.33 to 0.45 cm 3 /g, and a
ratio between the mesopore volume and the macropore volume (V 6nm-100nm /V 100nm ) in the range 1 to 1.86, and having a copper content, expressed in terms of oxides, in the range 18% to 35% by weight with respect to the total weight of said capture mass.

4. The capture mass as claimed in claim 1 , wherein the macropore volume (V 100nm ) is 0.35 to 0.42 cm 3 /g.

5. The capture mass as claimed in claim 1 , wherein the alumina support is obtained by shaping a starting alumina obtained from the rapid dehydration of hydrargillite.

6. The capture mass as claimed in claim 1 , wherein the mesopore volume (V 6nm-100nm ) of said porous support is 0.55 to 1.0 cm 3 /g.

7. The capture mass as claimed in claim 1 , containing at least 90% by weight of copper in the form Cu x S y with respect to the total weight of copper.

8. The capture mass as claimed in claim 1 , wherein the porous support has a grain crush strength (GCS) of at least 0.68 daN/mm.

9. The capture mass as claimed in claim 1 , in the form of a bead.

10. The capture mass as claimed in claim 1 , in the form of cylindrical, trilobed or multilobed, wheel or hollow cylinder extrudates.

11. The capture mass as claimed in claim 1 , wherein 100% of the porous support is flash alumina.

12. A process for the preparation of a capture mass as claimed in claim 1 , comprising:
a) preparing a porous support based on alumina;
b) preparing an aqueous solution containing at least one dissolved copper precursor;
c) impregnating the solution obtained from b) onto the alumina support obtained from a);
d) allowing the impregnated support obtained from c) to mature at a temperature in the range 20° C. to 60° C., for a period in the range 0.5 h to 8 h;
e) drying the solid obtained from d) between 70° C. and 250° C.;
f) optionally, calcining the solid obtained at the end of e), in air at a temperature in the range 300° C. to 800° C. in a dry atmosphere;
g) sulphurizing the solid obtained from e) or f) to form an active sulphurized phase Cu x S y .

13. The process as claimed in claim 12 , in which sulphurization g) is carried out using a gaseous mixture of nitrogen and hydrogen sulphide with a molar concentration which is in the range 1000 ppm to 10% and at a temperature in the range 100° C. to 400° C.

14. A process for the reduction of heavy metals, contained in a gaseous or liquid feed, comprising bringing a capture mass according to claim 1 is brought into contact with said feed, wherein said heavy metals are reduced.

15. The process according to claim 14 , wherein the heavy metals include mercury.

16. A capture mass capable of capturing heavy metals including mercury, contained in a gaseous or liquid feed, said mass comprising:
copper which is present at least in part in the sulphide form, Cu x S y ;
a porous support based on alumina;
said porous support having a total pore volume (TPV) in the range 0.8 to 1.5 cm 3 /g, a mesopore volume (V 6nm-100nm ) in the range 0.5 to 1.3 cm 3 /g, a macropore volume (V 100nm ) in the range 0.35 to 0.42 cm 3 /g, and a
ratio between the mesopore volume and the macropore volume (V 6nm-100nm /V 100nm ) in the range 1 to 1.86.

Assignees

• Ifp Energies Now

Inventors

• Barthelet Karin
• Hugon Antoine

Classifications

• B01D2253/1128

  Metal sulfides · CPC title

• B01D53/64

  Heavy metals or compounds thereof, e.g. mercury · CPC title

• B01J20/28092

  Bimodal, polymodal, different types of pores or different pore size distributions in different parts of the sorbent · CPC title

• B01D2253/311

  Porosity, e.g. pore volume · CPC title

• B01J2220/56

  Use in the form of a bed · CPC title