Performance trapping mass and use thereof in heavy metal trapping

Patent metadata

Field	Value
Publication number	US-9561487-B2
Application number	US-201214349081-A
Country	US
Kind code	B2
Filing date	Sep 12, 2012
Priority date	Oct 4, 2011
Publication date	Feb 7, 2017
Grant date	Feb 7, 2017

Abstract

The present invention concerns the elimination of heavy metals, in particular mercury and possibly arsenic and lead, present in a gaseous or liquid effluent by means of a capture mass comprising a support essentially based on alumina obtained by the gel method and at least one element selected from the group constituted by copper, molybdenum, tungsten, iron, nickel and cobalt. The invention is advantageously applicable to the treatment of gas of industrial origin, synthesis gas, natural gas, gas phase condensates and liquid hydrocarbon feeds.

First claim

The invention claimed is:

1. A capture mass for heavy metals, capable of capturing mercury contained in a gaseous or liquid feed, said mass comprising a porous support comprising gel alumina obtained from aluminum oxy (hydroxide), at least one metal M present at least in part in a sulfide form said metal M being copper, molybdenum, tungsten, iron, nickel or cobalt and in which the porous support comprises a quantity of sodium in the range 1 to 700 ppm by weight of sodium and has a pore diameter distribution such that:
0.4 mL/g<V 0.01 <0.8 mL/g;
and V 0.005 /V 0.03 >1;

V x being the pore volume of the porous support (mL/g) corresponding to the cumulative volume of its porosity, wherein the pore diameter, taken over the whole of the pores of the support, is more than x (in μm).

2. The capture mass according to claim 1 , in which the pore diameter distribution is such that:
0.48 mL/g<V 0.01 <0.75 mL/g; and V 0.005 /V 0.03 >1.8.

3. The capture mass according to claim 1 , in which the sodium content is at least 200 ppm by weight or less.

4. The capture mass according to claim 1 , containing at least 90% of metal M sulphide in the form M x S y .

5. The capture mass according to claim 1 , having a total pore volume in the range 0.20 to 1 cm 3 /g and a specific surface area in the range 20 to 400 m 2 /g.

6. The capture mass according to claim 1 , in which the metal M is copper.

7. The capture mass according to claim 1 , in the form of extrudates with a trilobe shape.

8. The capture mass according to claim 7 , in which the diameters of the extrudates with a trilobe shape are in the range 0.4 to 100 mm.

9. The capture mass according to claim 1 , in which the porous support is 100% alumina gel.

10. The capture mass according to claim 1 , in which the sodium content is less than 200 ppm by weight or less.

11. The capture mass according to claim 1 , wherein the metal M in sulfide form has the formula M x S y , wherein x≦2 and y≦2.

12. The capture mass according to claim 11 , wherein x≦1 and y≦1.

13. The capture mass according to claim 11 , wherein x=1 and y=1.

14. A process for preparing a capture mass for heavy metals, capable of capturing mercury contained in a gaseous or liquid feed, said mass comprising a porous support comprising gel alumina obtained from aluminum oxy (hydroxide), at least one metal M present at least in part in a sulfide form said metal M being copper, molybdenum, tungsten, iron, nickel or cobalt, comprising:
a) bringing an aqueous solution of acidic salts into contact with an alkaline solution of aluminium salts or bringing an aqueous solution of acidic aluminium salts into contact with a basic solution containing no aluminium, or bringing an aqueous solution of basic aluminium salts into contact with an acidic solution containing no aluminium;
b) shaping an alumina gel support obtained from a) by mixing the gel in an acidic or basic medium to transform the product into a paste, followed by passing said paste through a die in order to obtain extrudates;
c) drying the alumina support obtained at the end of b) in the range 70° C. to 150° C., followed by calcining it in the range 250° C. to 1300° C.;
d) preparing an aqueous solution containing at least one precursor of dissolved metals that are copper, molybdenum, tungsten, iron, nickel or cobalt;
e) impregnating the solution obtained from d) onto the alumina support obtained from c);
f) maturing the impregnated support from e) in a closed vessel saturated with water at a temperature which is in the range 20° C. to 60° C., for a duration which is in the range 0.5 h to 8 h;
g) drying the solid from f) in the range 70° C. to 250° C.;
i) finally, sulfurizing the solid in the oxide state to form an active sulfide phase M x S y .

15. The preparation process according to claim 14 , in which before i), the solid from g) is calcined in air at high temperature in the range 300° C. to 800° C.

16. The preparation process according to claim 14 , in which sulfurization i) is carried out using a gaseous mixture of nitrogen and hydrogen sulfide with a molar concentration in the range 1000 ppm to 10% at a temperature in the range 100° C. to 400° C.

17. A process for the elimination of heavy metals, contained in a gaseous or liquid feed, comprising contacting a capture mass awarding to claim 1 with said feed.

Assignees

• Porcheron Fabien
• Barthelet Karin
• Baudot Arnaud
• Daudin Antoine
• Lelias Marc-Antoine
• Gelie Yannick
• Nicolaos Alexandre
• Ifp Energies Now

Inventors

• Porcheron Fabien
• Barthelet Karin
• Baudot Arnaud
• Daudin Antoine
• Lelias Marc-Antoine
• Gelie Yannick
• Nicolaos Alexandre

Classifications

• B01J20/28004

  Sorbent size or size distribution, e.g. particle size · CPC title

• B01J20/28057

  Surface area, e.g. B.E.T specific surface area · CPC title

• B01J20/0237

  Compounds of Cu · CPC title

• B01J20/3007

  Moulding, shaping or extruding · CPC title

• C10G25/003

  Specific sorbent material, not covered by C10G25/02 or C10G25/03 · CPC title