Protective layer-catalyst bed combination and a method for performing catalytic reaction using the same

FIELD: catalyst preparation methods.

SUBSTANCE: invention proposes combination of protective layer against chlorine compounds and copper-containing catalyst bed. Protective layer is formed from molded members prepared from particles of led carbonate and/or basic led carbonate with weight-average particle size less than 10 μm. Catalytic reaction in presence of above-defined combination is also described.

EFFECT: prevented deactivation of copper-containing catalyst operated with process gas containing chlorine compounds.

11 cl, 3 tbl, 7 ex

 

The invention relates to catalysts and, in particular, copper-containing catalysts.

Copper-containing catalysts are often used for reactions involving hydrogen, for example, for simple reactions of hydrogenation, for example the hydrogenation of aldehydes to alcohols, for methanol synthesis (where carbon oxides react with hydrogen, methanol decomposition (where methanol is often mixed with water vapor, is decomposed to produce hydrogen and carbon oxides) and response bias (where carbon monoxide reacts with steam to produce hydrogen and carbon dioxide) and reverse reactions are offset. Often, in order to obtain optimal activity and stability of catalyst, the catalyst is made of copper in finely dispersed form, for example by precipitation of copper compounds in the presence or in conjunction with one or more media materials, in particular with compounds of zinc, magnesium, chromium and/or aluminum. After such deposition, the composition is heated to convert copper compounds, and if necessary, the materials of the carriers into the corresponding oxides. Before using for the desired reaction of the copper oxide reduced to metallic copper. Catalysts particularly suitable for the above-mentioned reactions are compositions of copper/zinc oxide/XID aluminum and copper/zinc oxide/chromium oxide. In some cases, part of the zinc can be replaced by magnesium, and/or part of the aluminum oxide or chromium oxide can be replaced by cerium oxide or oxide of rare earth element such as lanthanum oxide.

Copper-containing catalysts are easily deactivated by the presence of process gas at the reaction of chlorine compounds, such as hydrogen chloride. Trace amounts of such compounds chlorine can occur due to material contamination, for example, in the hydrocarbon feedstock, water vapour or air, is used for receiving the process gas. Such chlorine compounds react with active copper, forming chloride of copper. Because the chloride copper melts at a relatively low temperature, when a temperature at which the catalysts are usually used, for example, when 150-300°C, the copper will become mobile and will seek to aggregate loss in the dispersion of copper and with the subsequent loss of catalyst activity. In addition, when a component of the catalyst is zinc oxide and/or magnesium, similarly may be formed corresponding chlorides, and they likewise will tend to become mobile with the loss in the stabilizing action of the oxides of zinc or magnesium, again, followed the sweat is she dispersion and activity of copper.

In PCT application of the same applicants (publication WO 01/17674)in parallel consideration, it was proposed the use of a protective layer located before the flowsheet than copper-containing catalyst, where the protective layer is formed in the form of particles of a composition comprising a compound of lead and the media for him. This application describes that the particles of the protective layer can be obtained by impregnating the carrier particles with a solution of a suitable salt of lead, such as lead nitrate, resulting in the deposition of the corresponding lead compounds in the presence of the particles of the medium or in the co-deposition of lead compounds and the carrier, or the precursor medium. The preferred connection of lead is lead nitrate. However, if you use nitrate of lead, there is the risk that in the event of a malfunction of the installation on the protective layer may condense water and leaching of nitrate of lead from the media and wash it, which is situated further along the technological scheme of the copper-containing catalyst. The lead compounds tend to poison the copper-containing catalysts, and therefore there is a danger that the activity of copper-containing catalysts can be reduced. For this reason, it may be predpochtite is determined as being the use of lead compounds, which is insoluble in water. Although lead oxide is insoluble, it was discovered that he was not very effective as protection from chlorine under certain technological conditions. However, it was found that effectively protects from chlorine lead carbonate and basic lead carbonate. Although mentioned earlier PCT application offered that can be used lead carbonate or basic carbonate of lead, it did not describe a specific application of protective layers containing such lead compounds.

It was found that the molded elements suitable for use as protective layers, can be obtained from powdered lead carbonate and/or basic lead carbonate. Accordingly, the present invention provides a combination containing a layer of particles of a copper-containing catalyst and precede it in the flowsheet protective layer formed of molded elements derived from particles of lead carbonate and/or basic lead carbonate with an average (mass-average) particle size less than 100 microns. In particular, particles of lead carbonate and/or basic lead carbonate has an average (mass-average) particle size less than 50 microns, and, preferably, essentially all of the particles have a size less than 120 microns.

The protective layer is present in the form of molded elements: eyprepocnemis have maximum and minimum dimensions in the range from 1.5 to 20 mm, in particular, from 3 to 6 mm, the Aspect ratio of the formed elements, i.e. the ratio of maximum size to minimum, preferably less than 2.

Molded elements may have a regular shape, such as spheres, cylinders and the like, and can be retrieved using "dry" methods, where the powder composition is pressed to obtain the desired shape, for example, in teletrauma machine, or using a wet method in which the powder composition is mixed with a suitable liquid to obtain a paste, which is then ekstragiruyut with obtaining the desired cross-section, and the extrudate is cut or broken into elements of the required length. Alternatively, you can use the method of granulation, in which the powder composition is mixed with a small amount of liquid, often water, is insufficient to obtain a paste, and the resulting moist mixture granularit or tabletirujut using a pellet press, for example, related to the type used for pelleting animal feed, where the granulated mixture is loaded into a rotating perforated cylinder through the perforations of which the mixture is pushed by the rod or roller located inside the cylinder. The resulting extruded mixture is cut off from the surface of the rotating cylinder by means of the scraper knife situated thus, to obtain pellets of the desired length.

In that case, if you use "wet" methods of forming molded items before use is preferably dried.

Formed elements are preferably prepared from a mixture of particles of lead carbonate and/or basic lead carbonate and finely ground particles of the carrier formed from an inert material, such as aluminum oxide, hydrated aluminum oxide, chromium oxide, zirconium dioxide, titanium dioxide or, less preferably, silicon dioxide. A preferred carrier is alumina or hydrated oxide of aluminum.

Whichever method of forming neither used to obtain the formed elements in the powder composition preferably include technological additive, such as a lubricating agent and/or binder. Lubricants, which are in General use when used dry process route, such as tableting include graphite, fatty acids and their salts, such as stearates. Binders which can be used may be inorganic, for example, clay, such as attapulgite, bentonite, thick, or colloidal silicate of magnesium, aluminum, or cement, for example a cement based on calcium aluminate, or organization who technical, for example, soluble carbohydrate, such as starch, alginate or xanthan gum; simple cellulose ether, such as hydroxymethylcellulose; protein; polyvinyl alcohol and its complex ether, acetal or a simple ester or mixed derivative, for example, partially hydrolyzed polyvinyl acetate; polyalkyleneglycol; a polyacrylate or methacrylate; or polyacrylamide or polymethacrylamide. Organic binders are preferred. The amount of binder used in the General case is in the range from 0.5 to 10 wt.%, in particular from 1 to 5 wt.% in the calculation of the combined weight of lead compounds, the media (if available) and a binder.

Preferred compositions containing the binder and the media differ in the level of lead content in the range from 5 to 75 wt.%, in particular from 10 to 60 wt.% lead (in terms of metal) and calculated on the combined weight of lead compounds, the carrier and binder.

If the organic binder is used, regardless of the use of wet or dry method of molding, the molded elements are preferably calcined in air for debinding of the binder. The temperature of calcination, preferably, is in the range from 200 to 400°C, preferably below the temperature of decomposition of lead compounds. The material of the protective layer is elicina specific surface, determined by the method of Brunauer-Emmett-teller, preferably greater than 50 m2/g and, most preferably, greater than 125 m2/, it Was found that the annealing procedure can increase the value of the specific surface of the material of the protective layer. For example, absorbents obtained from the basic lead carbonate and three-hydrate of aluminum oxide and subjected to annealing at 300°With, usually characterized by the value of specific surface area determined by the method of Brunauer-Emmett-teller approximately 150 m2/year

The protective layer and the layer of catalyst used in the fixed layers, and they can be in the same container or in different containers, and a protective layer is placed on technological scheme before the catalyst bed. Process gas is preferably passed through the catalyst bed from the top down: thus, in the case where the protective layer and the catalyst layers are in the same container, the protective layer may be a layer of particles of the protective layer located on top of the particles of the catalyst layer. If desired, to facilitate replacement of the protective layer without disturbing the catalyst layer between the protective layer and the catalyst layer can have a layer of inert material.

Therefore, in accordance with another aspect of izopet the deposits is proposed a method of carrying out catalytic reactions with the use of a layer of a copper-containing catalyst, including passing the process gas through a protective layer formed of molded elements derived from particles of lead carbonate and/or basic lead carbonate with an average (mass-average) particle size less than 100 microns, and the subsequent transmission of the mentioned process gas through a layer of a copper-containing catalyst.

The invention is particularly applicable in the case of response bias. In this way the process gas stream containing carbon monoxide and water vapor, and often other components such as hydrogen, carbon dioxide, methane and/or nitrogen, is passed through a layer of a copper-containing catalyst, particularly a catalyst based on copper/zinc oxide/aluminum oxide or copper/zinc oxide/chromium oxide in which a certain amount of zinc oxide can be replaced by magnesium oxide, and/or some amount of aluminum oxide and/or chromium oxide can be replaced by oxide of rare earth element, at a temperature in the range from 150 to 300°With, in particular when the inlet temperature in the range from 150 to 250°C. Process gas preferably contains from 1 to 4 vol.% of carbon monoxide and at least one mol of water vapor per one mol of carbon monoxide. The process gas preferably contains from 20 to 50 vol.% water vapour. Usually the way to implement when srednecenovojj feed rate of the wet gas in the range from 2000 to 5000 h -1and at pressures ranging from atmospheric to 50 bar absolute pressure.

You must understand that in addition to the absorption of chloride of lead compounds will also absorb and sulfur compounds, and thus, this layer will also serve as a layer of protection against sulfur.

The invention is further illustrated in the following examples, in which various protective layers was tested by loading 0.5 g (about 0.4 ml) of the particles of the standard catalyst precursor to the low-response bias on the basis of copper oxide/zinc oxide/aluminum oxide containing approximately 50 wt.% copper oxide and characterized by particle size in the range of 0.6-1.0 mm, in a microreactor containing 0.25 g (approximately 0.1 ml) of particles of fused alumina with a particle size in the range of 0.6-1.0 mm, arranged in a layer on top of the catalyst precursor response bias, and 0.2 ml (approximately 0.36 g) of the protective material particles with a particle size in the range of 0.6-1.0 mm, located on top of the particles of fused aluminum oxide, to obtain the total catalyst volume, approximately equal to 0.70 ml

The copper oxide in the catalyst precursor was restored to metallic copper in the transmission of a stream of nitrogen containing 2% vol. hydrogen, from top to bottom through the microreactor at a pressure which avnon about 28 bar absolute pressure, at a flow rate of 15 liters/hour (at normal temperature and pressure) at that time, as the microreactor was heated from room temperature to 220°C and kept at this temperature for 95 minutes to complete recovery time equal to 3,5 hours.

The activity of the catalyst for the reaction of bias involving water gas was determined, skipping 50 liters/hour (at normal temperature and pressure) of a gas mixture containing 1 volume part of water vapor, 2 volume parts of gas with a volume consisting of: H255%, CO215%, WITH 5% and N225%through the microreactor at a temperature of 220°and a pressure approximately equal to 28 bar absolute pressure.

Modeling of chloride contamination to the gas mixture after passing through the catalyst bed for about 6 hours was added HCl to obtain the concentration of HCl in the wet gas is 1 ppm (volume). Under fixed test conditions variation of CO conversion depending on the residence time in the processing line were measured using the built-in infrared detector. The decrease in CO conversion with time indicates a loss of catalyst activity.

Example 1

In this example, the absorber chloride were obtained from powdered lead carbonate and three-hydrate of aluminum oxide. Powdered CT is eat lead was characterized by a mass-average particle size of 4.5 μm, moreover, essentially all of the particles size was in the range of 1 to 60 μm. The powdery three-hydrate of aluminum oxide, the specific surface, determined according to the method of Brunauer-Emmett-teller, was equal to 0.5 m2/g, and the mass-average particle size was equal to 22 μm, and essentially all particle size was in the range of from 1 to 100 microns.

94 g of powdery three-hydrate of aluminum oxide were mixed for 5 minutes with 6 g of powdered lead carbonate and 2 g of graphite as a lubricant and using teletrauma machine was molded mixture with low and wide cylindrical pellets with a diameter of 3 mm and a height of 0.6 mm nominal level of lead content in grains was equal to 4.6 wt.%, and their density was equal to 2.3 g/ml.

Example 2

Repeating example 1 with 88 grams of powder three-hydrate of aluminum oxide and 12 g of powdered lead carbonate to obtain granules with a nominal level of lead content of 9.1 wt.% and a density of 2.5 g/ml.

Example 3

Repeated example 1, using 80 g of powdery three-hydrate of aluminum oxide and 24 g of powdered lead carbonate to obtain granules with a nominal level of lead content of 17.6 wt.% and a density of 2.5 g/ml.

Example 4

Repeated example 1 using 60 g of the powder three-hydrate oxydianiline and 48 g of powdered lead carbonate to obtain granules with a nominal level of lead content of 33.8 wt.% and a density of 2.9 g/ml.

Example 5 (comparative)

For the purposes of comparison used commercially available absorber containing lead oxide deposited on alumina, with a nominal level of lead, approximately equal to 20.5 wt.%.

The materials of examples 1-5 were tested in accordance with what was described above: before applying granules were snapped to obtain particles with a size of 0.6-1 mm, Since the material of example 5 was characterized by a significantly lower bulk density in comparison with the materials of examples 1-4, in this case used a similar volume of absorber (approximately 0.2 ml), but its mass is only approximately equal to 0.19,

% conversion was determined over a period of time lasting several days taking measurements at regular intervals. To facilitate comparisons between the results of measurements of CO conversion depending on the residence time in the processing line were applied to the chart and points for each sample were building a smooth curve. (Individual points had minor deviations from the smooth curves). According to the graphic dependences every 24 hours was determined by conversion, and the results are shown forth in the following table 1, where the values of the % CO conversion rounded to the nearest integer.

Table 1
The residence time in the processing line (days)Conversion of CO (%)
Example 1Example 2Example 3Example 4Example 5
18684868585
28282848381
36878838172
44065808050
504275797
664780
74577
8876
9075
1073

Example 6

360 g of poroshkoobraznogo of three-hydrate of aluminum oxide, as was the case in example 1 for 5 minutes, mixed with 287,4 g of powdered lead carbonate, as was the case in example 1 to obtain a powder mixture with a nominal level of lead content equal to 34.4 wt.%. After this powder mixture was dried for 2 hours in an oven at 110°and then divided into four parts. One portion was granulated as described in example 1, with the addition of 2 wt.% graphite as a lubricant. Other portions progulivali for 2 hours at different temperatures before adding 2 wt.% graphite and granulation in accordance with the fact, as described above. In each case, the density of the granules was approximately 2.9 g/ml were Also determined by the mass loss during annealing. Materials testing was performed as described above, and the results are shown forth in the following table 2.

Table 2
Stay in the

technological line (days)
Conversion of CO (%)
Without Prokaeva depositsProKLIMA-tion at 200°ProKLIMA-tion at 300°ProKLIMA-tion at 400°
182858685
279828483
376808382
475798280
574788079
672767878
771757677
870747074
964715868
1055654056
Weight loss (%)-2,416,721,6

Example 7

In this example, the sinks were obtained from the basic lead carbonate and three-hydrate of aluminum oxide. The alumina trihydrate was the same as used in examples 1 to 4. Excess of 99.5 wt.% particles of the basic lead carbonate were of a size less than 63 μm.

47.9 g of powdery basic lead carbonate and 60 g of powdery three-hydrate of aluminum oxide were mixed to obtain a powder mixture with a nominal level of lead content equal to 35.6 mA is.%. After this powder mixture was dried for 2 hours in an oven at 110°and then was divided into three parts. One portion was granulated as described in example 1, with the addition of 2 wt.% graphite as a lubricant. Other portions progulivali for 2 hours at different temperatures before adding 2 wt.% graphite and granulation in accordance with the fact, as described above. In each case, the density of the granules was approximately 2.7 g/ml except for the sample obtained using temperature calcination 200°where the density of the granules was equal to 2.9 g/ml.

Materials testing was performed as described above, and the results are shown forth in the following table 3.

/tr>
Table 3
The residence time in the processing line (days)Conversion of CO (%)
Without dryingDrying at 110°The annealing at 200°The annealing at 300°
179808186
272737484
370707283
470707282
570707280
670707279
759707277
827605372
92251048
10-4010

1. Combination containing a layer of particles of a copper-containing catalyst and precede it in the flowsheet protective layer from chlorine compounds, formed from molded items obtained from particles of lead carbonate and/or basic lead carbonate with mass-average particle size less than 100 microns.

2. The combination according to claim 1, where the molded elements are obtained from compositions containing technological Supplement.

3. The combination according to claim 2, where technological additive includes a binder.

4. Combination according to any one of claims 1 to 3, where the molded elements are obtained from compositions containing particles of a carrier selected from aluminum oxide, hydrated aluminum oxide, chromium oxide, zirconium dioxide and titanium dioxide.

6. Combination according to any one of claims 1 to 5, where mass-average particle size of lead carbonate or basic carbonate of lead, used to produce moulded items, less than 50 microns.

7. The combination according to claim 3, where the molded elements are obtained from compositions containing from 1 to 5 wt.% binder calculated on the combined weight of lead compounds, the media (if available) and a binder.

8. Combination according to any one of claims 1 to 7, where the maximum and minimum sizes of the molded elements are in the range of from 1.5 to 20 mm

9. Combination according to any one of claims 1 to 8, wherein the aspect ratio of the formed elements is less than 2.

10. Combination according to any one of claims 1 to 9, where the molded elements calcined at a temperature greater than 200°but lower temperature of decomposition of lead compounds.

11. The method of carrying out catalytic reactions with the use of a layer of a copper-containing catalyst, comprising passing the process gas through a layer of protection against chlorine compounds formed from molded items obtained from particles of carbonate the wine and/or basic lead carbonate with mass-average particle size less than 100 microns, and the subsequent transmission of the mentioned process gas through a layer of a copper-containing catalyst.



 

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