Chemistry of inorganic compounds – Modifying or removing component of normally gaseous mixture – Carbon dioxide or hydrogen sulfide component
Reexamination Certificate
2000-05-22
2002-02-26
Griffin, Steven P. (Department: 1754)
Chemistry of inorganic compounds
Modifying or removing component of normally gaseous mixture
Carbon dioxide or hydrogen sulfide component
C423S244010, C423S244060, C423S244090, C423S244100, C502S008000, C502S009000, C502S240000, C502S250000, C502S252000, C502S253000, C502S407000, C502S415000, C502S439000, C502S517000, C210S660000, C210S670000, C210S679000, C210S749000
Reexamination Certificate
active
06350422
ABSTRACT:
BACKGROUND OF THE INVENTION
This invention is related to the field of sorbent compositions.
The removal of sulfur from fluid streams has long been desirable, as well as necessary, for a variety of reasons. If a sulfur-containing-fluid-stream is to be released as a waste stream, removal of the sulfur from the fluid stream is necessary to meet certain environmental regulations. If a sulfur-containing-fluid-stream is to be used in a catalyzed process, removal of the sulfur is often necessary to prevent poisoning of the catalyst.
It is desirable for sorbents to have higher crush strengths because such sorbents will have lower attrition losses, and consequently, a longer life. This lowers the costs associated with sulfur removal processes. Furthermore, it is desirable for sorbents to have higher sulfur loading capacity because such sorbents will remove more sulfur per unit, and consequently, less sorbent is needed. This also lowers the costs associated with sulfur removal processes.
SUMMARY OF THE INVENTION
It is an object of this invention to provide a process to produce a sorbent composition.
It is another object of this invention to provide said sorbent composition.
It is another object of this invention to provide a process for using said sorbent composition.
In accordance this invention a process is provided. Said process comprises:
(1) contacting
(1.1) at least one zinc component, where said zinc component comprises zinc oxide, or a compound convertible to zinc oxide,
(1.2) at least one silica component, where said silica component comprises silica, or a compound convertible to silica,
(1.3) at least one colloidal oxide component, where said colloidal oxide component comprises a mixture that comprises a metal oxide, and optionally
(1.4) at least one pore generator component; and
(1.5) a promotor component, if desired to form a first mixture; and thereafter,
(2) extruding said first mixture to form an extruded, first mixture; and thereafter,
(3) sphering said extruded, first mixture to form a sphered, extruded, first mixture that comprises particles where said particles have a particle size from about 0.5 to about 15 millimeters; and thereafter,
(4) drying said sphered, extruded, first mixture to produce a dried, sphered, extruded, first mixture; or simultaneously therewith, or thereafter,
(5) calcining said dried, sphered, extruded, first mixture to produce a calcined, dried, sphered, extruded, first mixture; and thereafter,
(6) steaming said calcined, dried, sphered, extruded, first mixture, to form a steamed, calcined, dried, sphered, extruded, first mixture; and thereafter,
(7) sulfiding said steam, calcined, dried, sphered, extruded, first mixture, to form said sorbent composition.
In accordance with another embodiment of this invention a sorbent composition is provided. Said sorbent composition is produced by said process.
In accordance with another embodiment of this invention a process to use said sorbent composition is provided. Said process comprises using said sorbent composition to remove a sulfar-containing-compound from a fluid stream.
DETAILED DESCRIPTION OF THE INVENTION
Generally, the zinc component (1.1) is zinc oxide. However, it may be a compound that is convertible to zinc oxide under the conditions of preparation described herein. Examples of such compounds include, but are not limited to, zinc sulfide, zinc sulfate, zinc hydroxide, zinc carbonate, zinc acetate, and zinc nitrate. The amount of the zinc component used in this invention is in the range of about 10 to about 90 weight percent based on the total weight of the components (1.1-1.5). However, an amount in the range of about 25 to about 75 weight percent is preferred and an amount in the range of about 40 to about 60 weight percent is most preferred.
The silica component (1.2) used in this invention can be any suitable form of silicon dioxide (SiO
2
). Silica, for the purposes of this invention includes both naturally occurring silica and synthetic silica. Additionally, the silica component can be in the form of one or more silica compounds that are convertible to silica under the conditions of preparation described herein. Currently, however, natural silica is preferred. Suitable examples of natural silicas are diatomaceous earth (which is also called kieselguhr, diatomite, infasorial earth, or Celite®) and clay. Suitable examples of clay include aluminum silicates, magnesium silicates, and aluminum-magnesium silicates. Suitable examples of aluminum silicates include bentonite, halloysite, kaolinite, montmorillonite, and pyrophylite. Suitable examples of magnesium silicates include hectorite, sepiolite, and talc. Suitable examples of aluminum-magnesium silicates include attapulgite and vermiculite. Suitable examples of synthetic silicas include zeolites, precipitated silicas, spray-dried silicas, and plasma-treated silicas. Mixtures of these silicas can also be used. Any commercially available silica can be used in this invention, however, diatomaceous earth is currently preferred. The amount of the silica component used in this invention is in the range of about 10 to about 60 weight percent based on the total weight of the components (1.1-1.5). However, an amount in the range of about 20 to about 50 weight percent is preferred and an amount in the range of about 30 to about 40 weight percent is most preferred.
The colloidal oxide component (1.3) is generally a mixture comprising finely divided, colloidal-sized particles of a metal oxide. These particles are, in general, homogeneously distributed throughout the mixture. The size of these particles varies, but in general, the size of the particles is in the range of about 10 to about 10,000 angstroms. Typical solid concentrations in such colloidal oxide components can range from about 1 to about 30 weight 5 percent based on the total weight of the colloidal oxide component. The pH of the colloidal oxide component can range from about 2 to about 11 depending on the method of preparation of the colloidal oxide component. The metal oxide, in a preferred embodiment, is selected from the group consisting of alumina, silica, titania, zirconia, tin oxide, antimony oxide, cerium oxide, yttrium oxide, copper oxide, iron oxide, manganese oxide, molybdenum oxide, tungsten oxide, chromium oxide, and mixtures of two or more of said metal oxides. Currently, in a more preferred embodiment the colloidal oxide component comprises colloidal alumina, colloidal silica, or mixtures thereof. The amount of the metal oxide used in the invention in the colloidal oxide component is in the range of about 1 to about 30 weight percent based on the total weight of the colloidal oxide component. However, an amount in the range of about 1 to about 20 weight percent is preferred and an amount in the range of about 5 to about 15 weight percent is most preferred.
Optionally, a pore generator component (1.4) can be used. The pore generator can be any compound that can be mixed with the above components and that is combustible upon heating thereby producing voids. This pore generator helps to maintain and/or increase the porosity of the sorbent composition.
Examples of such pore generators include, but are limited to, cellulose, cellulose gel, microcrystalline cellulose, methyl cellulose, zinc stearate, and graphite. The amount of the pore generator component used in the invention is in the range of about 0.1 to about 15 weight percent based on the total weight of the components (1.1-1.5). However, an amount in the range of about 1 to about 10 weight percent is preferred and an amount in the range of about 3 to about 6 weight percent is most preferred.
The above four components can be contacted together in any manner known in the art. Additionally, they can be contacted in any order. However, it is sometimes preferred to contact the colloidal oxide component with the silica component before they are contacted with the zinc component and the pore generator component. This facilitates the colloidal oxide components coverage of the silica component. In other words, it is preferred if
Engelbert Donald R.
Khare Gyanesh P.
Griffin Steven P.
Phillips Petroleum Company
Richmond, Hitchcock, Fish & Dollar
Vanoy Timothy C
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