Metal oxide-base thickened composition

FIELD: chemical technology.

SUBSTANCE: invention relates to particles of a thickened composition based on metal oxide comprising metal oxide and a binding agent, and to a method for forming particles from the thickened composition based on metal oxide. Metal oxide is chosen from iron and zinc oxides and a binding agent from starch, cellulose, carboxycellulose. The composition can comprise an activating agent additionally. The composition is used for removal of sulfur compound from a fluid medium being at temperature less 200°C mainly. Invention provides preparing stable particles showing high sulfur-capacity.

EFFECT: improved and valuable properties of composition.

29 cl, 8 dwg, 8 ex

 

This invention relates to particles associated or compacted compositions based on metal oxide used in the removal of pollutants, including sulfur compounds from fluid, in addition, the invention concerns a method of manufacturing such a compacted composition based on a metal oxide. More preferably, this invention relates to a compacted granular composition based on iron oxide, and the binder is preferably a water-insoluble composition.

It is well known that metal oxides, in particular oxides of iron (FexOy), used in the reaction layer to remove contaminants, usually sulfur compounds, especially hydrogen sulfide (H2S)of fluid, usually gas streams. Sulfur compounds are removed from the fluid, as they are known, are pollutants that potentially make the flow of gas or other fluids are not suitable for sale. Gas that contains too much sulfur, known as sour gas. In this case, in the gas industry, as well as in related industries, it is considered necessary to remove sulfur compounds from a fluid, including gas. Note that these fluids typically do not contain oxygen. (It is known that oxygen can increase the ability of the reaction between the composition of the oxide-based metal contaminants). From these considerations, there is a need for products that efficiently and economically remove sulfur compounds from a fluid. In addition, it is desirable to have a method or composition that does not require the introduction of an activating agent such as oxygen. Unfortunately, the most accessible song on the basis of iron oxide (the most commonly used for sulfur removal material based on metal oxides), which operate at ambient conditions and are generally not activated, keep the amount of sulfur equal to the maximum of 20% wt. by weight of the total composition based on iron oxide. More typically, a material based on iron oxide (such as surface material in this process) will hold an average of 0.12 kg (lb) H2S 1 kg (lb) of iron oxide. (The percentage of deduction depends, in part, from specific varieties of iron oxide). Increased sorption capacity for H2S for compositions on the basis of iron oxide, greater than 20%, usually requires the addition to the supplied gas caustic or oxygen, which is a dangerous and potentially difficult, especially at high pressures. This is problematic, because approximately 80% of the total number of product-based metal oxide is not used. From these considerations require frequent replacement of the metal oxide. Traces of the tion, it is desirable to increase the mass percent of sulfur, held total number of product-based metal oxide.

Removing sulfur level, which will handle up to millions of cubic feet of gas per day, or on an industrial scale, usually requires the use of large reaction layers, filled environment, or product based on iron oxide. Typically, this environment includes iron oxide and media, such as montmorillonite or wood chips. In order to avoid frequent switching, i.e. replacement of the used medium on the basis of metal oxide (environment, which no longer has the necessary reactivity towards sulfur) new environment-based metal oxide, use large or multiple reaction layers. These reaction layers will be or very high, 3,048 m (10 ft) or greater, or multiple reactors consistently line up, so you can use a number of the reaction layers. If the reaction layers are very small or small, the metal oxide will be produced very quickly. This is due to the fact that when processing large volumes of gas or other fluid, the metal oxide being in an environment-based metal oxide, be quick to respond. In order to have a sufficient service life of the layer that did not require frequent replacement of sredina the basis of metal oxide or iron oxide, must apply large quantities of metal oxide. This is a disadvantage for two reasons. First, the amount of sulfur that are held by composition-based metal oxide, or iron oxide, is relatively low in relation to the total weight of the used product. In order to increase efficiency, it is desirable to have a product that holds a greater percentage of unreacted sulfur per unit mass of total product. Secondly, the amount of space required for sulfur removal, it may increase the cost. It is desirable to be able to reduce the total area required for the removal of H2S. in Other words, it is desirable to retain a greater amount of sulfur reduced number of compositions based on metal oxide.

One way to increase the amount of sulfur retained in the reaction vessel is granulation or compaction of metal oxide. The amount of sulfur held by the composition of the oxide of the metal increases, because the reactor is greater than the available metal oxide. Typically, the metal oxide is applied onto a carrier, which is about 80% wt. by weight of the composition based on a metal oxide. Alternative grains usually contain some amount of a binder comprising from about 1% to about 20% wt. of the mass of the granulated mixture. the AK can be seen, the amount of metal oxide is greatly increased. The binder that was used for the formation of the granular iron oxide particles include cement, bentonite and similar compounds, especially inorganic composition. However, the granulated particles made with these binders, had the disadvantage that, apparently, the efficiency was reduced and the reactivity of the metal oxide is reduced. In particular, the number of retained sulfur was slightly increased compared to the amount of sulfur that are held by the same kinds of metal oxides when applying them to the media. From these considerations, previous attempts granulation of metal oxides were found to be unsuccessful due to inadequate reactivity towards sulfur, in particular inadequate holding capacity. Thus, it is necessary to find a binder that allows you to provide the necessary bonding of particles of metal oxide or iron oxide, without reducing the reactivity or the efficiency of removal of sulfur compounds. More specifically, it is necessary to find a binder that allows the metal oxide retain higher amounts of sulfur, in particular N2S, in the absence of caustic soda or adding oxygen in any form.

As it is known granulation of metal oxides for use in PR is the removal of sulfur compounds from a fluid. In particular, U.S. Patent No. 4732888 (Jha et al.) describes the application of the granules of zinc ferrite desulfurization of hot coal gas. This patent describes a composition comprising oxides of zinc and iron related inorganic and organic binder, and a small amount of activator. Inorganic binders include bentonite, kaolin and Portland cement. Organic binders include starch, methylcellulose and molasses. These granules are very specific structural solution, as they are used in the reaction layers having a temperature of at least 650°C. due to the high temperature of the organic binder is decomposed, resulting granules fragmented and porous. Thus, the organic binder is injected for a particular purpose, namely, to first bind the granules, and then decomposition of the binder to create a large porosity. Although this solution is great when used in high temperature processes desulfuromonas coal, under normal conditions it does not provide a sufficient degree of removal. Apparently, it was found that inorganic binders reduce the amount of sulfur removed granulated metal oxides. As a result, if you apply inorganic binder for binding the granules, probably, sulfur Bud is t to leave enough when environmental conditions or related conditions. It should also be noted that the previously believed that the organic binder is unacceptable for the formation of granules applied at ambient conditions, due to the fact that organic binder usually do not provide granules sufficient crushing strength, or achieved reactivity is insufficient, or the use of these binders results in granules having a too high cost.

This invention relates to particles associated or compacted compositions based on metal oxide used to remove fluid contaminants, preferably sulfur compounds, and to corresponding methods. The compacted particle compositions based on metal oxide includes a number of metal oxide constituting at least 80% wt. by weight of the particles of the compacted composition based on a metal oxide. Besides this the densified composition based metal oxide keeps the average amount of sulfur equal to at least 10% wt. by weight of the particles of the compacted composition based on a metal oxide, and more preferably, the amount of sulfur equal to at least 30% wt. by weight of the particles of the compacted composition based on a metal oxide. It is important that the particle compacted compositions based on metal oxide holds larger quantities of the sulfur, than in the case when types of specific metal oxide used to produce the compacted composition-based metal oxide, used in combination with a carrier. In General, the compacted particle composition based on a metal oxide capable of holding a quantity of hydrogen sulfide (H2S), equal to at least 0.27 kg per 1 kg of weight of particles of the compacted composition based on a metal oxide. An additional advantage of compacted particles of the composition on the basis of metal oxides is that they are sufficiently remove sulfur at temperatures below 200°and that is another big advantage when environmental conditions. Preferably, these particles are compacted compositions on the basis of metal oxide have a crushing strength of at least 1 kg, and more preferably, the crushing strength equal to at least a 3.5 kg

The compacted particle compositions based on metal oxide includes a number of metal oxide, preferably in the form of a powder or particles of small size, and organic binder. The metal oxide has a particle size in the range of from about 0.1 to about 100 microns, which means that the metal oxide is similar to the dust, also known as the fine fraction. The metal oxide has the formula IUxAboutywhere Me is selected from the group Castiadas iron and zinc, x is equal to from 1 to 3, and y is from 1 to 4. In particular, preferred is iron oxide with the formula FeaObwhere a is from 1 to 3 and b is from 1 to 4. As such most preferred are compositions that include ferric oxide with the formula Fe3About4. As the organic binder used starch, cellulose and carboxymethylcellulose. Preferred water-insoluble organic binder, with the most preferred binders are water-insoluble compositions based on cellulose. The organic binder can be added to the metal oxide in a quantity of from 0.5 to 20% wt. by weight of metal oxide, and more preferably in a quantity of from 0.5 to 5% wt. from a metal oxide.

The method according to this invention includes the Union of the specified organic binder, preferably cellulose, with particles of the specified metal oxide, and a thorough mixing of these two components. After mixing the two components, it is necessary to compact the mixture to form particles of the compacted composition based on a metal oxide. The methods used to seal components with obtaining particles of the compacted composition-based metal oxide can be any of a variety of methods or devices, including extrusion or PR is Sovana. Can be applied to any device or packing method, which appropriately formed particles of the compacted composition based on a metal oxide having a sufficient crushing strength. In this invention it is preferable to seal the mixture of metal oxide applied by extrusion or pressing. Components can be passed through the extruder to form a reinforced composition based metal oxide. Conversely, components can be placed in a sealing apparatus for forming a compacted composition based on a metal oxide. The sealing device is a device having at least two balanced wheels, which rotate in opposite directions, thus pressing in between the composition of the oxide-based metal. As was discovered, the use of the extruder, and the sealing device allows to obtain particles having sufficient crushing strength and reactivity in relation to pollutants, especially sulfur compounds. You can apply any of the existing sealing or extrusion devices.

The particles of the compacted composition-based metal oxide can be given the desired size during the molding or they is there to be crushed to the desired size after molding. At least 90% of the particles of the compacted composition based on metal oxide should have a final particle size of equal to from about 0.1 mm to about 200 mm, it is Impossible to have 100% of the particles of the compacted composition based on metal oxide within this interval, since the lower limit of the range will include particles of the compacted composition based on a metal oxide, which are powder or fine fraction, and a small amount of this fraction will be included in the final product. Preferably, the size of the particles is from about 0.1 mm to about 20 mm, More preferably, the size of the particles is from about 0.5 mm to about 5 mm

Preferably, after compaction of the mixture-based metal oxide crushed her in such a way as to obtain particles of the compacted composition based on a metal oxide of the desired size. A smaller final particle size increases the amount of hydrogen sulfide, which is able to absorb these particles are compacted compositions based on metal oxide. Crushed particles compacted compositions based on metal oxide is then sieved to classify by size, in order to ensure at least 90% of the particles of the required size. All particles larger load in a hammer mill, and then served on a sieve. Small fraction, between the in fact, again served in the charge to the compacted composition based on a metal oxide.

This invention has advantages for several reasons. In particular, the particles of the compacted composition based on a metal oxide to provide a product that can be used in the reaction layer, resulting in this product reacts with a large amount of sulfur so that a greater amount of sulfur is in the reaction layer. This is desirable because you can use less overall space and are less likely to produce switching of the reactor. The particle size is preferred because it allows a better use of the material as a whole. This invention also has advantages, because it shows that it is possible to obtain granulated particles of the compacted composition based on a metal oxide having sufficient reactivity towards sulfur. This means that these particles are suitable for use on a commercial scale, in contrast to many other known granular compositions based on metal oxide.

Figure 1 depicts the removal of various sulfur compounds from a stream of liquid propane with the use of pelletized iron oxide with measurements at the initial time, after 6 hours, 14 hours and 22 hours;

Figure 2 depicts the results of standard La the oratorial operational test showing the influence of the particle size of the compacted composition based on a metal oxide for the removal of H2S this song;

Figure 3 depicts the same as Figure 1, except that the removal of sulfur compounds used composition on the basis of zinc oxide;

Figure 4 presents the dependence of the constant bran k for the three flow rates from the number of pounds (kg) N2S in the reaction layer of oxide;

Figure 5 depicts the same as Figure 3, except that here, we compare three different types of iron oxide;

6 depicts the same as Figure 3, except that it refers to another type of iron oxide;

Fig.7 shows the comparison of the form of iron oxide with two types of granular iron oxide, and the yield of H2S refers to the number of pounds (kg) H2S in the reaction layer of oxide; and

Fig refers to the same, and 6, except that here, we compare three different types of granulated iron oxide.

This invention relates to associated or aggregated particles of the composition-based metal oxide, a method for producing such particles and to a method of use of such particles for the removal of pollutants, preferably sulfur compounds from fluid. These particles are compacted composition of the oxide-based metal predpochtitel is but represent particles of the compacted composition based on iron oxide, which are well suited for removal of sulfur compounds, such as H2S, of the fluid. These particles are compacted compositions based on metal oxide have the advantage that they hold more sulfur than other compositions based on metal oxides. The composition is compacted metal oxide can hold an average amount of sulfur, comprising at least 10%, and preferably 30 wt.%. by weight of particles of the compacted composition based on a metal oxide. This densified composition based metal oxide is sufficient to remove sulfur at temperatures less than 200°and at any pressure. More preferably, this densified composition based metal oxide is sufficient to remove sulfur in the environment. To obtain the compacted composition based on a metal oxide comprising at least one metal oxide and a binder, apply sealing device or extruder. A binder can be a composition based on starch, carboxymethyl cellulose or a combination thereof. Suitable binders include compositions based on cellulose. Preferred binders are water-insoluble compositions based on cellulose. The densified composition based metal oxide can then be brought to the con is knogo particle size, equal to from about 0.1 mm to about 200 mm, Preferably the final size of the particles is from about 0.1 mm to about 20 mm, More preferably, the size of the particles is from about 0.5 mm to about 5 mm

This method is carried out, starting with mixing a quantity of a metal oxide with a number of connecting with the formation of a homogeneous mixture of the oxide of the metal. Can be applied with any method of mixing these two components, if only the components were thoroughly mixed and formed of a homogeneous mixture of a binder/metal oxide. It is preferable to add a binder to the metal oxide in a quantity of from about 0.5% to about 20% wt. by weight of metal oxide. More preferably, a binder is added to the metal oxide in a quantity of from 0.5 to 5% wt. by weight of metal oxide.

The present invention is used, the metal oxide having the formula IUxAboutywhere Me is selected from the group consisting of iron and zinc, x is equal to from 1 to 3, and y is from 1 to 4. You can also use a hydrated form of metal oxides. Composition based on iron oxide (FeandAboutb) are the most preferred metal oxides for use in this invention. Preferably the particle associated metal oxide contains Fe3O4. This composition of the commonly sold under the name "black iron oxide" and, as such, black iron oxides are preferred for use in this invention.

The metal oxide may have a particle size in the range from about 0.1 microns to about 100 microns and, more preferably, from about 1.5 to 50 μm. As such, unprocessed or raw metal oxide used to produce the associated product-based metal oxide, is small, or in powder form. Thus, homogeneous body or the associated particle is formed from granulated or fine material. In addition, these particles are preferably porous, so they are believed to have a surface area of at least 25 times greater than other non-porous particles, such as solid particles of the same size. It is assumed that they possess the desired characteristics.

A binder, which is mixed with a metal oxide, should have sufficient binding ability to form an oxide of the metal particles, which will have a crushing strength of at least 1 kg, and preferably 3.5 kg, as measured on the determinant of the hardness of Koala (Kohl). Binder should not only give sufficient crushing strength, but it should be such, so as not to affect the reactivity of the particles of metal oxide with respect to sulfur. Hypotheti the Eski this binder should be such, to allow the particles of the compacted composition based on metal oxide to have some porosity or the ability to transfer that allows you to use the inner part of the particles. Regardless of this binder should allow the compacted particle compositions based on metal oxide to retain some amount of sulfur equal to at least 10% wt. by weight of the particles, and preferably at least 30 wt.%. by weight of the particles. This binder may be added to the metal oxide in a quantity of from 0.5 to 20% wt. by weight of metal oxide, and more preferably in a quantity of from 0.5 to 5% wt. by weight of metal oxide. Binder should be such that it is relatively insoluble in water. It is necessary to avoid substantial dissolution of the binder in water, since these particles are typically used in a wet environment. If the water dissolves the binder, the particles can potentially disintegrate as binder no longer perform its function. Thus, preferred is a water-insoluble binder, which will not deteriorate due to the presence of water. You can use any binders that meet this description; however, it is most preferable to use an organic binder, more preferably not soluble in water com is ositio based on cellulose. Preferably, the amount of cellulose present in the composition for particle-based metal oxide, 15% or less.

The preferred binder is not water-soluble cellulose, or mineral-modified cellulose. Most preferred is a binder containing about 100% water-insoluble cellulose. Preferably this binder absorbs less than 60 wt.%. water. It is preferable aspect ratio from 6 to 7. The preferred density is more than 70 g/l particle Size of the binder should be in the range from 32 to 200 microns. An example of a suitable commercially available binder is TECHNOCEL202 production of Cellulose Filler Factory Corp., Chestertown, Maryland.

In addition to the metal oxide used to produce particles of the compacted composition-based metal oxide, can add to the mixture a quantity of activator metal oxide. The purpose of adding the activator is to increase the reactivity of the particles of the compacted composition based on metal oxide and, in particular, the promotion of more active response of these particles with sulfur compounds. To existing activators include copper oxide, silver oxide, aluminum oxide, gold, platinum oxide, cadmium oxide, Nickel oxide, palladium oxide, lead oxide, mercury oxide, tin oxide, cobalt oxide is a, aluminium oxide, manganese oxide, and combinations thereof. Most preferably, however, use the copper oxide, since it is known that he most strongly increases the reactivity of the metal oxide without the formation of hazardous compounds, as established by the Agency for the protection of the environment. It should be noted that when the applied metal oxide is manganese oxide and the activator will be any available activator, in addition to manganese oxide. The activator should be added in amount equal to from about 0.5% to about 5% wt. by weight of the composition based on the metal oxide used for the formation of particles associated metal oxide.

After the mixture on the basis of metal oxide are mixed, this mixture on the basis of metal oxide is compacted with the formation of the compacted composition based on a metal oxide. Sealing can be done in many ways, it has formed dense particles. It is preferable to skip the song through the sealing device or extruder, to obtain a reinforced composition based metal oxide. You can use any device or method to obtain the compacted composition-based metal oxide, if only remained sufficient reactivity towards sulfur, and the resulting particles had sufficient strength on sdavlivaya. The particles of the compacted composition based on a metal oxide having a desired final particle size can be obtained directly by using an extruder or the sealing device. The desired final size of the particles is from about 0.1 mm to about 200 mm, Preferably the final particle size is from about 0.1 to about 20 mm, More preferably the final particle size is from about 0.5 mm to about 5 mm, At least 90% of the particles of the compacted composition based on metal oxide must be in this interval. It is impossible to have 100% of the particles in the desired range, since the lower end of the range will include a number of particles having dimensions on the level of powder or fine fractions, some of which will be in the final product. If the device gives particles of the compacted composition based on a metal oxide having a desired final particle size, there is no need to crush them or sift. Assume that in these conditions, the obtained particles having sufficient reactivity and crushing strength.

It is preferable, however, that the densified composition based metal oxide was in large pieces when it passes through the sealing device or extruder. Then it is crushed into particles of the compacted composition based on OK the IDA metal with the desired particle size. You can use the standard methods that exist in the industry to obtain pellets of extruded material. The densified composition based metal oxide, as such, has a crushing strength of 3.5 kg and the final particle size is from about 0.1 mm to about 200 mm, Preferably the final size of the particles is from about 0.1 mm to about 20 mm, More preferably the final size of the particles is from about 0.5 mm to about 5 mm smaller the particle size of the final product allows the metal oxide, which is present in the particles to react with an increased number of H2S, increasing, thus, the amount of H2S. Note that the crushing strength of the particles will depend on a number of factors, including moisture content, concentration of starch and particle size.

In addition to molding or extruding metal oxide and a binder can be applied to other forms of seals. Among the available aggregated forms are granules, tablets, lozenges, corrugated shape of the corrugated rings, rings, spheres and extrudates.

Any method may be used to seal the metal oxide, so that the carrier is not necessary, and the metal oxide can be used in the reaction layer. It is also desirable to produce particles, and not just add the powder of the metal oxide is in the reaction vessel, for, if there were sufficient reactivity, space should be provided inside the reactor, allowing fluid to leak. The powder would not allow the stream to flow at a sufficient rate.

If the densified composition based metal oxide is formed by extrusion, it is possible the necessary drying of the granules or particles to reduce their moisture content. For drying, you can use any process, if only particles had a total water content of less than 10% wt. and, more preferably, less than 3% wt. The temperature used for drying the particles can be any temperature which does not decompose and does not fade binder and which will not oxidize the metal oxide. Preferably the temperature should be 150°s or less and, more preferably, the temperature should be 90°With or below. Drying of the granules is necessary in order to get the maximum crushing strength.

The dryer, which can be used include rotary dryer and the belt dryer. Preferred is a rotary dryer.

After drying, it is preferable to maramuresului (marumerize) particles of the compacted composition based on a metal oxide formed by extrusion, as this was discovered, increases the hardness and wear resistance, measured in percentage the ratio is receiving the fine fraction of waste compacted composition of the oxide-based metal. In this invention can be used to implement any paramerization (marumerizers). Drying in a rotary dryer can eliminate the need to use paramerization (marumerizer).

Once formed, the particles of the compacted composition of the oxide-based metal by crushing the compacted composition-based metal oxide, particles diffuse on the sieve to classify by size. Particles remaining on the top sieve, loaded into a hammer mill, and then return to the sieve. Small fraction of return to the charge to the compacted composition based on a metal oxide.

After formation of the particles of the compacted composition based on metal oxide should be placed in the reaction vessel so that they were in contact with fluids contaminated with sulfur compounds. These fluids include gas, liquid and combinations thereof. It is most preferable to remove sulfur compounds from contaminated gas streams, such as propane and gaseous hydrocarbons. Among the sulfur compounds, which can be removed with the use of these particles on the basis of metal oxide, are hydrogen sulfide (H2S), seraikis carbon (COS), carbon disulfide (CS2), dimethyl sulfide (DMS) and mercaptans such as methyl mercaptan (MeSH), ethyl mercaptan (EtSH) and propylmercaptan (PrSH). It should be noted that, probably, and other polluting substances is STV, located in fluids, especially in the gaseous hydrocarbons can be removed with the help of compacted particles of metal oxide. These sulfur compounds can be removed at ambient conditions. More specifically, sulfur compounds can be removed if the temperature is equal to or less than 70°s, and the highest temperature is 200°C. you Can use any pressure, preferably is the ambient pressure. Additionally, the fluid flow can pass over the particles of the compacted composition based on a metal oxide at a rate equal to at least of 0.182 m/min (0,6 feet per minute) for gases and 0,0305 m/min (0,1 feet per minute) for liquids.

The particles of the compacted composition-based metal oxide can hold an average amount of sulfur equal to at least 10%, and preferably 30 wt.%. by weight of particles of the compacted composition based on a metal oxide, and having the ability to hold H2S, is equal to at least 0.27 kg (lb) H2S 1 kg (lb) particles compacted compositions based on metal oxide. Moreover, the particles of the oxide of the metal should have a density in the range from 1.0 to 1.5. From this we can conclude that the particles compacted compositions on the basis of metal oxide have a high capacity retention of sulfur.

The following examples are given for Illus the operational purposes and in no way intend to limit the invention.

EXAMPLES.

Example 1.

Test was performed to determine the effectiveness of extruded pelletized iron oxide in the removal of sulfur-containing pollutants, including hydrogen sulfide, seraikis carbon, mercaptans and possibly carbon disulfide. The test started with the packing in the column with the size of 5.05 cm×30.48 cm (2×12 inches) approximately 567 g (1.25 lbs), or approximately 25.4 cm (10 inches) medium granular iron oxide. These granules based on iron oxide contains black iron oxide and binder is a starch. Inlet valve was located at the bottom of the column, so that contaminated fluid entered into the column from the bottom and leaving the top of the column. The gas, which was subject to the clearing, was a liquid propane contaminated various sulfur-containing pollutants, including hydrogen sulfide, seraikis carbon and light mercaptans. Measurements to determine the amount of sulfur-containing pollutants was carried out on the gas inlet into the column and output it from the speaker; and the measurements were carried out at different points in time. Figure 1 depicts the initial number of different sulfur-containing compounds at the inlet into the column. Contaminants evaluated in the mass parts per million - ppm. The specific conditions in the reactor or column to the following:

Reactor typeA single, verticalThe flow directionThe upward flow
The reactor temperature65°The contact time15 ml/min
The ratio L/D5:1SØR-1Extrusion FM1
Pressure2.5 MPa (360 psig. pounds/square inch)

L/D denotes the ratio of the length of the passage to the diameter filiere extruder.

Containing sulfur contaminants were determined using Gosta on the copper strip, which identified the sulfur content and contaminants in the fluid flow by the ability of polished copper strips to attack in accordance with the method of ASTM D-1838.

As can be seen from Figure 1, the granular iron oxide provides excellent removal of various sulfur compounds. In particular, H2's easy to remove this granular iron oxide. In addition, it is easy to remove COS, CS2and mercaptans. Thus, it was concluded that the granular iron oxide provides excellent removal of sulfur compounds. This was considered important because it was known that previously applied granules of iron oxide was removed sulfur is insufficient compared to the iron oxide nanoscale.

Example 2.

To assess the influence of particle size on the performance characteristics of the compacted composition based on iron oxide particles were obtained compacted composition based on iron oxide with different particle size. These particles are compacted composition based on iron oxide were obtained with the use of the sealing system MS-75 (Hosokawa Bepex). Cellulose binder, TECHNOCEL202, first made hydrational in the ribbon mixer model No. M by downloading 45,36 kg (100 pounds) TECHNOCEL202 in the mixer, turn on the mixer and add 36,29 kg (80 pounds) of water for six minutes and forty seconds when 0,276 MPa (40 psi). The mixer was added for another five minutes to uniformly hydrate TECHNOCEL202. Then added 45,36 kg (100 pounds) of copper oxide (I) (Purple Copp 97N) and faucet included an additional five minutes. This mixture was applied on the level of supply in the sealing device MS-75 and was placed in the exact dosing. 907,2 kg (two thousand pounds) of iron oxide having moisture content of 1.95% and bulk density loose 1377,72 kg/m3(86 lbs/cube ft) poured under gravity in the supply device Acrison. This feeder then move the iron oxide in turbolister model No. TS8. The mixture TECHNOCEL202 they dosaged in turbolister using the exact dotato the and. Turbulator contributed mixture TECHNOCEL202 and iron oxide in the sealing device VS-75. Material feed mixer on the rollers of the device for sealing regulated through a vertical feed screw. After crushing the flakes were unloaded in the shredder flakes, and then mechanically applied for sieves for classification by size. Top product screening unloaded the Hammermill RD-8, and then gave back to the sieves. The trifle was served by recycling directly to the feed hopper and the product meets on the size of the granules was collected.

Composition established for granules, represented 87.7 per cent of iron oxide, 4,4% TECHNOCEL202, 4.4% of copper oxide (I) and 3.5% water.

A sample of the compacted iron composition dissipated into three fractions, as shown in Table 1.

TABLE 1

Distribution % wt.
Sample 1Sample 2Sample 3
+3/8" - 4 mesh47,800
+4-6 mesh15,930,528,6
+6-16 mesh36?369,565,3
36,3+16-30 mesh006,0

Basically, the average particle size decreased with the transition from sample 1 to sample 3, as shown in Table 2.

Table 2
Sample numberThe particle size range, mmThe average particle size, mm
1from 1.0 to 9.54,5
2from 1.0 to 4.752,5
3From 0.5 to 4.752,0

The influence of particle size on performance when using standard laboratory performance test is shown in Figure 2 to Sample 1, which contained particles of the largest size with an average particle size of 4.5 mm, it took about 90 days to fix the breakthrough point at the level of 4 ppm of hydrogen sulfide; sample 2, containing particles with an average size of 2.5 mm, it took approximately 115 days to fix the breakthrough of hydrogen sulfide at the level of 4 ppm, while sample 3, containing particles with an average size of only 2.0 mm, did not give breakthrough certarea at the level of 4 ppm to about 135 days test. These results indicate that the decrease in the average size of the particles increases the effective capacity of the removal of H2S-compacted particles of a metal oxide.

Example 3.

Was carried out the same procedure as in Example 1, except that instead of granulated iron oxide felt granulated zinc oxide. Conditions were as follows:

The type of reactor for processingA single, vertical
The temperature in the reactor65°
The flow directionThe upward flow
The contact time11 ml/min
SØR-12.0 extrusion
The ratio L/D5:1
Pressure sample2.5 MPa (360 psig. pounds/square inch)

The results are given in figure 3. Observed that granular zinc oxide, in General, removing most of the sulfur compounds with the exception of COS. The use of pelletized zinc oxide led to acceptable elimination of most sulfur compounds. This was considered important because generally zinc oxide eliminates sulfur-containing contaminants at higher temperatures. When environmental conditions zinc oxide usually holds from 3 to 8% of the total number of sulfur.

Example 4.

Tests were performed to determine the relative strength crush strength of granulirovanniye based on iron oxide. Were made of granules of three types of iron oxide known as FM1 (ferrimagnetic 1), FM2 (ferrimagnetic 2) and Hoover, all three types of iron oxide were similar black iron oxides. The iron oxides FM1 and FM2 was a ferrimagnetic porous particles of iron oxide with an estimated range of particle sizes from 1.5 to 50 μm and with a hypothetical surface area of 10 m2/, Oxide Hoover, as expected, was a material with a significantly smaller particle sizes and with a very low porosity or pore-free. The iron oxide was mixed with different types of binder, and the binder were mixed in solution with different quantities. Also used the die of the extruder of different lengths. These changes were carried out to determine what combination will result in particles based on iron oxide with sufficient crushing strength. For the formation of granules on the basis of the oxides used pellet mill production Kahl; with all the granules obtained by the press, had a diameter of 6 mm To evaluate the strength of each of the granules used the Vickers hardness of the granules Kahl. In order to obtain accurate data, tests were performed on ten granules obtained by each method; then the results were averaged. Tester Kahl for pellet was manufactured by the company Amandus Kahl Gmblt&Co., Hamburg,Germany. Table 3 depicts the results of the tests, the concrete type of the binder upon receipt of each type of pellet, the length of the die used for molding the pellets, and the average crushing strength.

Table 3.

Summary data for testing LCI.
Oxide% waterBinding*The length of the SpinneretStrength, kgDensity
FM118,2No18Weak1,690
FM115No18Weak1,448
FM1150,0075% CMC18Weak1,406
FM115No36Weak1,477
FM1120,0075% CMC36Weak1,542
FM1130,075% CMC36Weak1,508
FM1130,0075% CMC48Weak1,475
FM1130,0075% CMC60Weak1,454
FM1130,64% starch30Fragile1,359
FM1160,78% starch30Strong-
FM1170,84% starch30the 3.8-
FM115 12.5% bentonite304,31,542
Hoover171.0% starch305,1-
FM2171.0 starch301,6-
FM119,21,34% starch60--
FM1the 17.31,33% starch605,1-
FM117,2133% starch605,98-
*The amount of the binder is provided in a dry oxide.
Oxide% waterBinderThe length of the nozzle, kgStrength, kgDensityELCA faction
FM215.31,04% starch603,11,315,1
FM215.31,04% starch601,91,457,6
FM218.82,36% starch606,651,175,3
FM218.82,36% starch60the 4.71,462,4
FM218.92,34% starch48the 7.651,033,2
FM218.92,34% starch488,31,321,3
FM218.92,34% starch48 6,81,231,8
FM218.92,34% starch366,01,062,1
FM218.92,34% starch366,051,231,7

Given the content of the binder is a percentage of the starch content per mass of dry matter in grains. The percentage of water is a quantity of a solution of a binder and water, mixed with the material of the metal oxide. The density of the granules, apparently, is not associated with the crushing strength of the granules.

As can be seen from these data, the use of starch and bentonite provides a excellent crushing strength I received from them pellets. Carboxymethylcellulose give granules having insufficient crushing strength. In addition, it was determined that the preferred length of the Spinneret at least 30 mm

Example 5.

This example relates to the testing of granular iron oxide FM1, FM2, and Hoover to assess the reactivity and effectiveness of each composition at UDA the attachment of hydrogen sulfide from the gas. Three reaction layer were filled with three different types of iron oxide. 907,2 grams (two pounds) of granular material based on iron oxide was placed in a glass tubular reactor with a length of 1.22 m (4 ft). This stage was repeated for each of the tested compositions are given in Table 4. The sour gas stream containing 3000 ppm by weight of H2S was passed over the various granulated compositions of iron oxide. Specifically, this gas is passed over the layer FM2 once, over a layer FM1 three times and over the layer Hoover three times; all of these cases are listed below. The flow rate of contaminated gas (Q) was set to one of three different values: 2.09 liters per minute (l/min), 3,75 l/min or 5,09 l/min Output H2S recorded depending on the time when the velocity of the stream.

Fig.7 shows the number of H2S Hoover was delayed and FM1 types of iron oxide at a flow rate of 2.09 l/min before breakthrough occurred H2S. in Addition, Fig.7 shows how much sulfur is held on the same type of iron oxide, used to create a composition FM1, but when applying iron oxide on the carrier. As you can see, granular iron oxide retains significantly more sulfur. On Fig shows the same as figure 7, except that the investigated another flow rate, 5,09 l/min, the System was under pressure 42 is PA (6 wt. pounds per square inch), and acid gas had a temperature of 20°C (68°F). The content of H2S was measured using an electronic detector TMX 412 for industrial and research measurements, calibrated against a standard mixture of 124 ppm H2S in the reactor. In addition, used tube Kitagawa as a parallel method to confirm the level of H2S.

Rate constants (k) were calculated based on the definition of the content of H2's output by using the following equations for values of N2S output (lbs): ∑[H2S reacted for Δt (lb)]. Figure 4 gives the dependence of the rate constants from quantity (pounds) H2S in the reaction layer of oxide material FM1. Used three different flow rate. The constant k (constant bran) had the highest value at the highest velocity 5,09 l/min the Slope of the curve is equal to the change in reactivity over time. The steeper the curve, the faster will be reduced reactivity. Thus, the slopes of the lines in Figure 4-6 shows the reactivity. 6 depicts the same as Figure 4, except that was taken iron oxide type Hoover. Figure 5 refers to the same data as figure 4, except that were tested three different types of iron oxides.

FM2 had the highest speed of the ISM is in reactivity; followed FM1. Both composition showed excellent reactivity. Material Hoover, as it was observed, was not such a good candidate for use as two other[ material. From the definition of k was defined as the ability to hold H2's estimated per unit mass, using linear regression analysis of the dependence of k on the number of (pounds) total content of N2S in the reaction layer. The estimated capacity is shown below. In addition, the slope obtained from linear regression analysis, is related to the speed of the reaction between the oxide material and H2S, denoted by R. the intersection of dependency with the x-axis gives the total capacity for holding materials. The results are shown in table 4.

-1,2
Table 4

Linear regression analysis relative To the accumulated quantity (in pounds) H2S, reacted with the reaction layer.
MaterialQ (l/min)TiltEstimated tank capacity lbRange

k

R
LCI (FM2)5,09-1,60,411,35-1,150,976
LCI(FM1)2,090,300,70-0,560,992
LCI(FM1)3,75of-1.50,300,94-0,72is 0.998
LCI(FM1)5,09of-1.40,310,92-0,700,975
LCI (FM1) All--1,70,270,94-0,700,959
data
LCI (Hoover)2,09-2,60,171,72-0,690,982
LCI (Hoover)3,75-4,30,151,28-0,72is 0.998
LCI (Hoover)5,09-6,90,120,90-0,580,992
LCI (Hoover)--5,80,131,58-0,670,984
all data

As you can see, FM2 and FM1 showed excellent results on keeping the number of H2S per pound of oxide jelly is a (see estimated holding capacity per pound).

Example 6.

The reaction rate k from Example 5 was analyzed to determine whether the granular iron oxide higher reaction efficiency than the form of iron oxide. Fig.7 represents the combined dependence of the data on the output of the H2S (ppm) relative to the number of pounds of H2S, which is reacted with the reaction layer of granular material, whether it is (FM1), (Hoover) or ungranulated material based on iron oxide, at a flow rate of 2.09 l/min These curves relate to the data output H2S (ppm) and to the number of H2S, reacted with the reaction layer, and directly illustrate the reaction rate for these materials.

As can be seen in Fig.7, 907,2 grams (two pounds) of product FM1 reacted with 172,368 g (0.38 lb) H2S before the concentration of H2's output reached 900 ppm. This is compared with the form of iron oxide, which showed that only 68,04 grams (0.15 lbs) iron oxide reacted before the content of H2's output reached a level of 900 ppm, which shows that the iron oxide gives the best result and reacts with a large number of H2S than in the form of iron oxide.

Example 7

This example was compared granulated zinc oxide SULFATREAT®(oxide yellow is for the media of montmorillonite). Conditions and results were as follows:

ZnOSULFA TREAT
The height of the reaction layer60,96 cm (2 ft)60,96 cm (2 ft)
Pressure35 kPa (5 psig. pound/square inch)35 kPa (5 psig. pound/square inch)
The flow velocity270 cm3/min270 cm3/min
Temperature21,11°C (70°F)21,11°C (70°F)
The concentration at the entrance3000+ppm H2S in N23000 ppm H2S
Diameter3,81 cm (1.5 inches)3,81 cm (1.5 inches)
Weight1065 g827 g
Volume815 ml815 ml
The total amount of used gas12830 l14774 l
The total number of remote H2S38,5 l44,3 l
The number of days to breakthrough3338

ZnO has worked for 33 days before breakthrough of hydrogen sulfide. This is 5 days shorter than SULFATREAT in the same conditions. Although ZnO did not remove such a large amount of sulfur, as SULFATREAT, the results are positive the I. ZnO, typically used at elevated temperatures, and this test was conducted at room temperature, and still H2S has been deleted.

Example 8.

This example relates to the preparation of example granules based on the metal oxide used for the removal of sulfur from fluid. This method started with a sample of black iron oxide from Ironrite Products Company, Inc., from St. Louis, Missouri. This black iron oxide was analyzed and it was determined that the moisture content amounts to 3% wt. In addition, it was determined that this black iron oxide has a bulk density 1,558 kg/L.

In order to form granules of a metal oxide, 9000 g of black iron oxide was placed in a paddle mixer, manufactured by Sigma Corporation, St. Louis, Missouri. This black iron oxide was added a quantity of a solution of the binder. This binder solution was formed by mixing 118 g of starch, Argo made with boiling water. Starch is measured in such a way that it amounts to 1.34% wt. calculated on dry substance, so that the total amount of binder solution added to the black iron oxide was 17,2% wt. Thus was formed the composition of the binder and oxide of iron, which is then mixed in a paddle meilke within 5 minutes. Received a dough, which was slightly wet and sticky.

the seat of the iron oxide was then submitted to the pellet mill, model 14-175 (produced by Kohl's). This pellet mill operated at 100 rpm and was equipped with a 6-mm Villeroy with the length of the seal 60 mm Power pellet press was about 1,51 kW, and the extrusion speed was equal to 224 kg per hour.

After extrusion, the pellets were treated in paramerization (marumerizer) (manufactured by LCI Corporation, Charlotte, North Carolina) with the friction plates with a gap of 8 mm, rotating at 300 rpm for 10 seconds. Then the granules were dried in a furnace at a temperature of about (93,33° (C) (200°F), it was determined that these granules have a bulk density of approximately 1.25 kg/L. in Addition, it was determined that these granules had a hardness of approximately 6,0 kg

Example 9.

Were obtained granules based on iron oxide containing a binder of cellulose. The retrieval process was as follows:

1. In capacity to 22,68 kg (50 pounds) of cellulose was added 29,03 kg (64 lb) of water and mixed.

2. Then to this mixture of pulp and water was added to the iron oxide in the amount of 453,6 kg (1000 pounds) with a water content of 1% or less.

3. The components were mixed until then, until there was obtained a homogeneous mixture.

4. This mixture was condensed at a pressure of 31 MPa (45000 pounds per square inch) with the formation of granules. The obtained granules had the following composition:

Componentwt.%.
Iron89
Cellulose5
Water6

Thus has been shown and described by way related to the use of compacted compositions based on iron oxide for the removal of pollutants from a fluid, and also shows a method of manufacturing such compacted compositions based on iron oxide, which satisfies all the objectives and expected benefits. However, professionals should be clear that there are many possible changes, variations, modifications and other uses and applications relating to these compacted compositions based on metal oxide and methods for their production, and also such changes, variations, modifications and other uses and applications which do not go beyond the nature and scope of this invention and is supposed to be covered by this invention which is limited only by the following claims.

1. The particles of the compacted composition based on a metal oxide, including

(a) a powder comprising a metal oxide, hydrated form of the oxide or combinations thereof, and the metal oxide has the formula IUxAboutywhere Me is selected from the group consisting of iron and zinc, x is the t 1 to 3, y is from 1 to 4, wherein the powder comprises at least 80 wt.% particles compacted composition based metal oxide;

(b) an organic binder selected from the group consisting of starch, cellulose and carboxymethyl cellulose to bind the powder in the form of particles compacted composition based metal oxide;

(c) distribution of particle sizes in which at least about 90% of the particles of the compacted composition based on metal oxide have a particle size from about 0.1 to about 200 mm; and

(d) the ability to remove sulfur compounds from fluid at temperatures less than 200°and to keep the average amount of sulfur equal to at least 10% of their mass.

2. The particles of the compacted composition based on a metal oxide according to claim 1, where the binder is added to the powder in an amount of from about 0.5 to about 20 wt.% from the mass of powder.

3. The particles of the compacted composition based on a metal oxide according to claim 1, in which the distribution of particle sizes such that at least 90% of the particles compacted compositions on the basis of metal oxide have a particle size from about 0.1 to 20 mm

4. The particles of the compacted composition based on a metal oxide according to claim 1, in which the distribution of particle sizes such that at least 90% of the particles of the compacted composition based on metal oxide they shall have a particle size of from about 0.5 to about 5 mm

5. The particles of the compacted composition based on a metal oxide according to claim 1, which is able to retain the average amount of sulfur equal to at least 30% of their mass.

6. The particles of the compacted composition based on a metal oxide according to claim 1, where the powder has a particle size from about 0.1 to about 100 microns.

7. The particles of the compacted composition based on a metal oxide according to claim 1, which is able to retain H2S constituting at least 0.2 kg H2S per 1 kg of the particles of the compacted composition based on a metal oxide.

8. The particles of the compacted composition based on a metal oxide according to claim 1, where the binder absorbs less than 60 wt.% water has a density of more than 70 g/l and the characteristic ratio from 6 to 7.

9. The particles of the compacted composition based on a metal oxide according to claim 1, having a crushing strength of at least 1 kg

10. The particles of the compacted composition based on a metal oxide according to claim 1, having a crushing strength of at least 3,5 kg

11. The particles of the compacted composition based on a metal oxide according to claim 1, where the powder further includes an activator selected from the group consisting of copper oxide, silver oxide, oxide of gold, platinum oxide, cadmium oxide, Nickel oxide, palladium oxide, lead oxide, mercury oxide, tin oxide, cobalt oxide, aluminum oxide, manganese oxide and their combinations.

12. The particles of the compacted composition based on a metal oxide according to claim 11, where the activator is from about 0.5 to 5% by weight of particles of the compacted composition based on a metal oxide.

13. The particles of the compacted composition based on a metal oxide according to item 12, where Me represents the iron, and the activator is an oxide of copper.

14. The particles of the compacted composition based on a metal oxide according to item 13. additionally comprising water in an amount of about 3.5 wt.%, when this powder is an Fe3About4the number 87,7 wt.%, the copper oxide is a copper oxide (I) in an amount of about 4.4 wt.%, while the content of the organic binder is 4.4 wt.%.

15. The particles of the compacted composition of the oxide-based metal 14 having a particle size range from about 1.0 to 9.5 mm and the average particle size of about 4.5 mm, or particle size range from about 1.0 to 4.75 mm and an average particle size of about 2.5 mm, or particle size range from about 0.5 to 4.75 mm and an average particle size of about 2,0 mm

16. Method of removing sulfur compounds from a fluid comprising passing the fluid over the particles of the compacted composition based on a metal oxide according to any one of claims 1 to 15 for removal of fluid sulfur compounds.

17. The method according to clause 16, in which the removal of sulfur from the fluid undertake Aut at a temperature of less than 200° C.

18. The method according to clause 16, in which the fluid medium is a gas which is passed over the particles of the compacted composition based on a metal oxide with a speed of at least of 0.182 m/min (0.6 m/min).

19. The method according to clause 16, in which the fluid medium is a liquid, which is passed over the particles of the compacted composition based on a metal oxide with a speed of at least 0,0305 m/min (0.1 m/min).

20. The method of forming particles of the compacted composition-based metal oxide, capable of holding the average amount of sulfur equal to at least 10% of their mass, to remove sulfur compounds from a fluid medium at temperatures less than 200°and the method includes

(a) mixing a quantity of the powder with some amount of organic binder selected from the group consisting of starch, cellulose and carboxymethyl cellulose, with the formation of the mixture, and the powder comprises a metal oxide, hydrated form of the oxide or combinations thereof, and the metal oxide has the formula MexOywhere Me is selected from the group consisting of iron and zinc, x is from 1 to 3, y is from 1 to 4, the powder has a particle size from about 0.1 to about 100 microns, and the amount of powder is at least 80% by weight of the mixture:

(b) compacting the mixture to p is by receiving the compacted composition-based metal oxide;

(c) crushing the compacted composition based on the amount of metal with obtaining particles of the compacted composition based on metal oxide and

(d) sieving the particles of the compacted composition based on a metal oxide so that at least 90% of the particles have a finite particle size of from about 0.1 to about 200 mm

21. The method according to claim 20, in which the amount of binder is from about 0.5 to about 20% by weight of the powder.

22. The method according to claim 20, in which the powder further includes an activator selected from the group consisting of copper oxide, silver oxide, oxide of gold, platinum oxide, cadmium oxide, Nickel oxide, palladium oxide, lead oxide, mercury oxide, tin oxide, cobalt oxide, aluminum oxide, manganese oxide, and combinations thereof, where the amount of the activator is from about 0.5 to about 5% by weight of the mixture.

23. The method according to item 22, in which Me represents iron, and the activator is an oxide of copper.

24. The method according to claim 20, in which the sealing operation is carried out, passing the mixture through the sealing device.

25. The method according to claim 20, in which the sealing operation is carried out, passing the mixture through the extruder.

26. The method according to claim 20, further comprising drying the particles of the compacted composition based on a metal oxide at a temperature from ambient temperature up to pace atory less 150° C.

27. The method according to p, further comprising paramerization dried particles compacted compositions based on metal oxide.

28. The method according to claim 20, in which particles of the compacted composition based on a metal oxide material so that at least 90% of the particles have a finite particle size of from about 0.1 to about 20 mm.

29. The method according to claim 20, in which particles of the compacted composition based on a metal oxide material so that at least 90% of the particles have a finite particle size of from about 0.5 to about 5 mm



 

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