Vysokoglinozemistyj carrier, a catalyst for heterogeneous reactions and method thereof

 

(57) Abstract:

The invention relates to holders for various fields of technology and catalysts used in the deep oxidation of hydrocarbons (afterburning of exhaust gases), hydrogenation (acetylene, nitrobenzene), oxidation of sulfur dioxide (sulphuric acid), partial oxidation of hydrocarbons (epoxidation of ethylene, propylene), conversion of ammonia in the production of nitrogen and hydrogen cyanide) and other Vysokoglinozemistyj media includes silicon oxide in the amount of more than 70 wt.%, the NMR spectrum MAS 29Si the state of the silicon carrier is characterized by the presence of lines with chemical shifts -100 3 M. D. (line Q3and -110 3 M. D. (line Q4) when the ratio of the integral intensities of the lines of Q3/Q4from 0.7 to 1.2, in the infrared spectrum has absorption band of hydroxyl groups with wave number 3620-3650 cm-1and the width of 65-75 cm-1and the carrier has a specific surface area measured by the BET method by thermal desorption of argon, SAr=0.5 to 30 m2/g and the magnitude of the surface, measured by the method of alkaline titration, SNa=10-250 m2/g at a ratio of SNa/SAr=5-30. Using this, but the hydrocarbons, partial oxidation of hydrocarbons, alkylation of hydrocarbons, oxidation of sulfur dioxide, hydrogenation of hydrocarbons, the conversion of ammonia and other, containing at least one active component selected from the group comprising platinum, palladium, rhodium, iridium, silver, zirconium, chromium, cobalt, Nickel, manganese, copper, tin, gold, titanium, iron, molybdenum and/or their oxides in an amount of not more than 2 wt.% (in terms of metal). The active ingredient is administered during the contact of the carrier with solutions of compounds of the respective active elements at a temperature of 40-200C. and a pressure of 1-200 MPa. Vysokoglinozemistyj media has unique physicochemical properties, which allows to achieve high efficiency and selectivity of catalytic processes, the catalysts are characterized by high chemical and thermal stability, strength characteristics. 3 S. and 11 C.p. f-crystals, 7 tab., 2 Il.

The invention relates to holders for various fields of technology and catalysts used in the deep oxidation of hydrocarbons (afterburning of exhaust gases), hydrogenation (acetylene, nitrobenzene), oxidation of sulfur dioxide (sulphuric acid), partial oxidation Poty), etc.

Usually the catalysts for these processes are active metals, their oxides or salts deposited on the media (amorphous or crystalline oxides of silicon and/or aluminium, magnesium and so on), made in the form of cylindrical pellets, rings, multi-line blocks. The most important role of the media is the provision of highly active state damage catalytic components due to their dispersion, the optimal allocation for the carrier of the active component, changing the chemical and electronic States.

The use of carriers and catalysts in the form of fine fibers has obvious advantages over the traditional geometric forms of mechanical, aerodynamic, thermal and physical properties. In some cases it is proposed to use fibers of silicate glasses or products (fiberglass, glass wool, stellarton and so on), the advantages of which are the availability and relatively low cost (Patent RF N 2010597, IPC5B 01 J 23/89, B 01 D 53/36, 1994). Fiberglass, as a rule, have low dispersion and porosity. To create the necessary media textural parameters application use fiberglass vysokodispersnom dispersing more valuable substrate for the catalytic elements for example, noble metals (U.S. Patent N 5552360, MCP B 01 J 21/04, 21/08,1996).

Another technique for increasing the surface of steklovata is a selective extraction from the glass side components (leaching) and the subsequent application of active ingredients (Japan Patent N 51 - 19837, IPC B 01 J 35/06, 1976).

Textural parameters of leached glass depend on their composition and preparation conditions. If in the process of leaching is a significant increase in the surface and the formation of meso - and macropores, it is accompanied by a significant decrease in strength (U.S. Patent N 4933307, IPC C 03 C 11/00, C 03 C 12/00, 1990). More durable leached materials are characterized by the absence of meso - and macropores and the low value of the surface. Applied to components that are mainly located on the outer surface of the fibers. Their disadvantage is the low dispersion and lack of a strong bond with the surface. The latter causes low catalytic activity and high surface mobility of the catalytically active metals, leading to their agglomeration in the process, the detachment from the surface of the carrier phase of the catalytically active metals and possible mechanical entrainment gas flow even DL the Oia adhesion of the catalytically active metals to the surface of the carrier in the patent of Russian Federation N 2069584, IPC B 01 J 23/38, 23/70, 1996 - the closest analog in the composition of the medium, made in the form of filaments, fibers, woven and nonwoven materials from oxides of silicon and/or aluminum impose additional alloying elements also of catalytically active metals and/or their oxides. The alloying additive is introduced into the mixture during the operation of obtaining a melt-based silicon oxide. So manufactured fiber media next pass through the weaving operation and application of the catalytic component on the surface of the woven material.

The disadvantage of this method is the localization of a significant part of the metal in the Central part of the fiber and, therefore, inefficient use in catalysis, as well as possible technological losses of valuable metal in the early stages of its introduction.

Object of the present invention to provide a marked components in the active form through the use of vysokokremnezemnstogo media with specific pseudolite structure, and by way of injecting the active component, providing a preferential distribution in the surface layers of fiberglass in highly dispersed active form, resistant to montemiscoso media including silicon oxide in the amount of more than 70 wt.%, for which the NMR spectrum MAS29Si the state of the silicon carrier is characterized by the presence of lines with chemical shifts -100 3 M. D. (line Q3and -110 3 M. D. (line Q4) when the ratio of the integral intensities of the lines of Q3/Q4from 0.7 to 1.2, in the infrared spectrum has absorption band of hydroxyl groups with wave number 3620-3650 cm-1and the width of 65-75 cm-1and the carrier has a specific surface area measured by the BET method by thermal desorption of argon, SAr= 0.5 to 30 m2/g and the magnitude of the surface, measured by the method of alkaline titration, SNa= 10-250 m2/g, with a ratio of SNa/SAr= 5-30.

Vysokoglinozemistyj media contains at least one of the metals and/or oxides of groups I and II of the Periodic system in an amount not more than 1 wt.% and has the form of fibers, beads, tubes, woven and nonwoven materials.

The problem is solved through the proposed use of the above media to obtain catalysts heterogeneous reactions (e.g., deep oxidation of hydrocarbons, partial oxidation of hydrocarbons, alkylation of hydrocarbons, oxidation dioxygenase, selected from the group comprising platinum, palladium, rhodium, iridium, silver, zirconium, chromium, cobalt, Nickel, manganese, copper, tin, gold, titanium, iron, molybdenum and/or their oxides in an amount of not more than 2 wt.% (in terms of metal) on vysokokremnezemnstogo media, comprising more than 70 wt.% oxides of silicon, the NMR spectrum MAS 29Si the state of the silicon carrier is characterized by the presence of lines with chemical shifts -100 3 M. D. (line Q3and -1103 M. D. (line Q4) when the ratio of the integral intensities of the lines (Q3/Q4from 0.7 to 1.2, in the infrared spectrum has absorption band of hydroxyl groups with wave number 3620-3650 cm-1and the width of 65-75 cm-1and the carrier has a specific surface area measured by the BET method by thermal desorption of argon, SAr= 0.5 to 30 m2/g and the magnitude of the surface, measured by the method of alkaline titration, SNa= 10-250 m2/g at a ratio of SNa/SAr= 5-30.

The active component in the catalyst for heterogeneous reactions is in the surface layers pseudolite object structure.

The catalyst for heterogeneous reactions further comprises at least one metal and/or oxide selected from 1,2,3,4 g is, tubes, woven and nonwoven materials.

The problem is solved by the method of producing a catalyst for heterogeneous reactions (e.g., deep oxidation of hydrocarbons, partial oxidation of hydrocarbons, alkylation of hydrocarbons, oxidation of sulfur dioxide, hydrogenation of hydrocarbons, the conversion of ammonia and other), including introduction to vysokoglinozemistyj media containing more than 70% of the oxides of silicon, compounds active ingredients selected from the group of platinum, palladium, rhodium, iridium, silver, zirconium, chromium, cobalt, Nickel, manganese, copper, tin, gold, titanium, iron, molybdenum in an amount of not more than 2 wt.% (in terms of metal), heat treated, for the preparation of catalysts using the medium in which the NMR spectrum MAS29Si the state of silicon is characterized by the presence of lines with chemical shifts -100 3 M. D. (line Q3and -110 3 M. D. (line Q4) when the ratio of the integral intensities of the lines of Q3/Q4from 0.7 to 1.2, in the infrared spectrum has absorption band of hydroxyl groups with wave number 3620-3650 cm-1and the width of 65-75 cm-1and the carrier has a specific surface area measured by the BET method by thermal desorption arg m2/g at a ratio of SNa/SAr= 5-30, the active ingredient is administered during the contact of the carrier with solutions of compounds of the respective active elements at a temperature of 40-200oC and a pressure of 1-200 MPa. Solutions of the active compounds of the elements have a value of pH 2-10, impregnating the solution of the active element may further comprise at least one of the elements 1, 2, 3, 4 groups of the Periodic system in an amount of not more than 1.5 wt.%, or for the preparation of the catalyst using a carrier that before contact with a solution of the active element is impregnated with at least one of the elements 1, 2, 3, 4 groups of the Periodic system in an amount of not more than 1.5 wt.%, or after contact of the carrier with a solution of the active element are impregnated with at least one of the elements 1, 2, 3, 4 groups of the Periodic system in an amount of not more than 1.5 wt.% After contact with the impregnating solution are shaded catalyst 3 - to 10-fold excess of water, with pH 3-8, heat treatment is performed at a temperature of 100-800oC in a gas environment or vacuum up to 10-4mm RT. Art.

The presence of the inventive lines in the spectrum of the NMR MAS29Si chemical shifts -100 3 M. D. and -110 3 M. D. provided that the ratio of the intensity of halogen with exceptiona who INIA Q4corresponds to polymer fragments of si tetrahedra linked siloxane bonds. The silicas of the si tetrahedra forms a continuous three-dimensional grid. Line Q3at low (<2%) content of cations of group 1 and 2 corresponds to only silanol groups.

With a large content of Q3(~40-60%) in two SiOH groups have 3-4 polymerized tetrahedron Q4. This is only possible for specific layered structures, where thin layers of 3-4 tetrahedra separated by narrow interlayer spaces. 1). Spatula C. M., Lapin O. B., Moudrakovski I. L. Nuclear magnetic resonance in heterogeneous catalysis. Novosibirsk: Nauka. 1992. 224 S. 2.) Engelhard, G., Michel, D. High Resolution State NMR of Silicates and Zeolites/John Willy@ Sons. 1987. 486 pp.

Declare us band 3620-3650 cm-1indicates the presence of a large number of Oh groups in geometrically constrained conditions, i.e., within a narrow interlayer spaces (see Fig. 2).

The active components are introduced into the interlayer space, under the influence of the matrix carrier should exhibit a high catalytic activity. However, diffusion difficulties may impede the introduction (intercalation) of cations in mislevy the oxygen fragments, if the layers are thin enough (high ratio of Q3/Q4), and in the interlayer space contains a large number of Oh groups, protons are capable of cation exchange (absorption band 3620-3650 cm-1). The ability of relatively coarse carrier (SAr= 0.5 to 30 m2/d) chemosensitivity cations reflects the third claimed us sign: high specific surface area, determined by chemisorption of the cations sodium (method Sears, 1. G. W. Sears //Anal. Chem. 1956. V. 28. p.1981; 2. P. Ailer. The chemistry of silica. M: Peace. 1982. So 2. C. 480.) the value of specific surface area determined by the BET method by adsorption of argon (SNa/SAr=5-30).

The proposed media derived from silicate glassy materials, made in the form of granules, fibers, and woven and non-woven products from them.

The inventive structure can be formed by leaching of these glass fibre materials with acid solutions by varying the composition and structure of glass, nature and concentration of acid, the leaching conditions and subsequent heat treatment thereby to obtain pseudolite structure with the stated properties. For example, we have found that the important conditions of formirovanie silicon-containing source material;

b) lack of coalescence of cavities when removing cations and/or subsequent chemical and thermal treatments.

Based on the proposed media we have developed a number of highly efficient catalysts containing small amounts of metals (platinum, palladium, silver, etc), is very promising for use in many chemical processes (oxidation of methane, propane, butane, ammonia, sulfur, hydrogenation of vegetable oils, hydrogenation of aromatic compounds), where they exhibit higher activity than conventional catalysts.

In the proposed media the totality of the claimed features indicates the presence of specific loosened pseudoelastic structures in the surface layer where possible the introduction and stabilization of the catalytic components in a finely dispersed non-equilibrium, and therefore, highly active state. But this localization of active components is possible under certain optimal conditions for the preparation of catalysts.

These conditions of entry (intercalation) of the active component are: the use of high temperature, high pressure, using solutions act of 1, 2, 3, 4 groups of the Periodic system, before, simultaneously or after contact of the carrier with a solution of the active component.

After contact with the impregnating solution are shaded catalyst 3 - to 10-fold excess of water, with pH 3-8 to remove loosely associated with the media connections of the active component. This allows to obtain highly active catalysts with very low content of the active component. Heat treatment of the obtained catalysts is carried out at a temperature of 100-800oC in a gaseous environment, modifying it in accordance with the requirements of the catalyst depending on the area where the catalyst will be tested.

The NMR spectra of29Si using the rotation of the sample under magic angle (MAS magic angle spinning) were recorded on a pulse Fourier transform NMR spectrometer "Bruker (Germany) MSL-400 (magnetic field of 9.4 T). The rotation of the samples under magic angle was performed using a high-speed sensor company Asp-Rotor-Consult (Denmark) rotors silicon nitride and zirconium oxide with a speed of 8-10 thousand revolutions per second (Fig. 1).

Infrared spectra were recorded on a spectrometer IFS 113 V (Bruker) in the range 1100-7000 cm-1with a resolution of 4 cm-1(Fig. 2).

< / the excess oxygen on model mixtures, containing n-butane, propane and carbon monoxide.

Test for n-butane and carbon monoxide is performed on a flow-circulation installation at atmospheric pressure, the same space velocity of the gas mixture and the same test conditions.

For measure the catalytic activity of the catalyst in the oxidation of n-butane adopted reaction rate / (cm3C4H10/ the hydrographic 10-2/ oxidation of n-butane at a temperature of 400oC. the higher the speed of reaction of complete oxidation of butane corresponds to a more active catalyst.

For measure the catalytic activity of the catalyst in the oxidation of carbon monoxide adopted the temperature at which achieved 85% degree of oxidation of carbon monoxide. The lower the temperature reach 85% degree of oxidation of carbon monoxide, the higher the catalyst activity.

Tests on propane is carried out in an isothermal flow reactor. For measure of catalytic activity adopted value of the degree of conversion at a given temperature.

The measurement of catalytic activity in the oxidation of SO2in SO3spend on the installation of flow type on the standard m is (, As Boreskov. Catalysis in the production of sulfuric acid. M: Goskomizdat, 1954, S. 87). The test is performed flow-through method when the composition of the gas mixture of 10 vol.% SO2, to 18.9% vol. O2, 71,1% vol. N2the reaction temperature 485oC, flow rate of gas providing a constant contact time of 0.9 seconds. On the inlet and outlet of the catalyst bed to measure the concentration of SO2and changes assess the degree of transformation of SO2(XRefthat is a measure of the activity of the parent catalyst selected standard conditions.

thermal stability of the catalyst is determined by the method of accelerated thermal aging, as Boreskov. Catalysis in the production of sulfuric acid. M: Goskomizdat, 1954, S. 153), which are as follows: the standard method to determine the initial activity of the catalyst at 485oC (XRef), then the temperature was raised to 700oC and maintain the catalyst within 50 hours. After that, the temperature in the flow reactor is reduced to 485oC and at this temperature, measure the residual activity of the sample (XRef).

In addition, to evaluate thermal stability carry out the measurement of activity at 700oC highly concentrated g the quantum (, s) necessary to achieve some constant degree of conversion Xconstaway from equilibrium reactions. As in the above test conditions, the equilibrium degree of transformation is Xp~ 51%, to map the activities we have chosen the constant Xconst= 39%. Was measured contact times sourceRefand after the test at 700oC for 50 hoursConECs.. Small values and their stability in long time tests at 700oC are evidence of high activity and thermal stability of the catalysts.

The catalysts of experience in the oxidation of ammonia to oxides of nitrogen, NOx reduction by methane in the reaction of alkylation of isobutane with butylene.

Data on the composition of the medium shown in table 1, Fig. 1, 2.

Data on the composition of the catalysts are shown in table 2.

The results are given in tables 2-6.

The following examples illustrate the invention.

Getting media

Sample No. 1. For preparation of media use sodium silicate newamericanow fiberglass composition SiO2-65,1%, Na2O - 16,3%, Al2O3oC for 120 minutes, washed with water until the pH in the wash water to 5,5-7,0, treated at 70oC and a pressure of 3 MPa for 4 hours, then calcined at a temperature of 200oC.

Sample No. 2. Glass of the same composition as in sample No. 1, calcined at 350oC for 2 hours, then treated with 7.5% HNO3when 90oC for 60 minutes, washed with water to pH 6,5-7,0, processing performed by the ultrasound with a frequency in the range of 20-40 kHz.

This is followed by a heat treatment in an air stream at 250oC for 10 hours.

Sample No. 3 (prototype)

In furnace for glass melting add platinum chloride in an amount of 0.1% in the finished product.

Received kremneftoristyj tissue media leached in 10-17% H2SO4when 93-98oC with subsequent washing. This is followed by drying and heat treatment at 650oC.

Sample # 4. The carrier is prepared by leaching of silica having the composition of 97% SiO2, 2,4 Na2O 0,6 Al2O3and calcined at 1200oC, treated with 7.5% HNO3when 90oC, then spend processing, as revealed characteristics (sample N 1, 2).

Example 1

The medium (sample No. 1, PL. 1) enter in contact with the solution emmakate platinum [Pt(NH3)4] Cl2if 120oC and a slight excess pressure of 2 MPa, the reactants are taken in the right quantities to obtain the estimated weight metal concentrations in the media, then the fabric is washed with water to separate loosely coupled with the carrier compounds of the metal, dried at 110oC, calcined in air at 300oC 2 hours and restore in a stream of hydrogen at 300oC for 2 hours.

Example 2

For the preparation of the catalyst using the media characteristics of the sample N 2 (PL. 1).

Before contact of the carrier with an aqueous solution of H2PtCl6in the media enter the cesium cation from the solution of CsCl in the amount of 0.2 wt.%.

The introduction of platinum is carried out at a temperature of 200oC and a pressure of 10 MPa in an acidic environment.

Example 3

The catalyst is prepared analogously to example 2, only as a solution of the active component used ammicht palladium, additional cations in the catalyst does not enter.

Example 4

The catalyst is prepared analogously to example 1, only as an active ingredient is administered palladium from a solution of PdCl>/P>Examples 5-11

The catalysts are prepared analogously to example 1, except that different active components, their quantity, conditions, contact with the media data are shown in table 2.

Example 12 (prototype)

For the preparation of the catalyst used fiberglass media, alloyed with platinum in an amount of 0.1 wt.% (sample N 3, PL. 1), then the catalyst is prepared analogously to example 1, except that different amounts of platinum, conditions, contact with the media.

Thus, from the above examples that the proposed vysokoglinozemistyj media has unique physical and chemical properties. This allows to achieve high efficiency and selectivity of catalytic processes, the catalysts are characterized by high chemical and thermal stability, strength characteristics.

In addition, the proposed media can be used in various fields of technology: manufacturing inorganic membranes, chromatographic columns, for receiving fiber optical materials, fabrication and other filters

1. Vysokoglinozemistyj media, including silicon oxide in the amount of more than 70 wt. %, ohimicheskie shifts - 100 3 M. D. (line Q3and -110 3 M. D. (line Q4) when the ratio of the integral intensities of the lines of Q3/Q4from 0.7 to 1.2, in the infrared spectrum has absorption band of hydroxyl groups with wave number 3620 - 3650 cm-1and the half-width 65 - 75 cm-1and the carrier has a specific surface area measured by the BET method by thermal desorption of argon, SAr= 0.5 to 30 m2/g and the magnitude of the surface, measured by the method of alkaline titration, SNa= 10 - 250 m2/g at a ratio of SNa/SAr= 5 - 30.

2. Vysokoglinozemistyj media under item 1, characterized in that it contains at least one of the metals and/or oxides of groups I and II of the Periodic system in an amount not more than 1 wt.%.

3. Vysokoglinozemistyj media under item 1, characterized in that it has the form of fibers, beads, tubes, woven and nonwoven materials.

4. The catalyst for heterogeneous reactions, for example, deep oxidation of hydrocarbons, partial oxidation of hydrocarbons, alkylation of hydrocarbons, oxidation of sulfur dioxide, hydrogenation of hydrocarbons, the conversion of ammonia and other , containing at least an active component selected from the group comprising platinum, palladium, rhodium, iReady not more than 2 wt.% (in terms of metal) on vysokokremnezemnstogo media comprising more than 70 wt.% silicon oxide, characterized in that the NMR spectrum MAS29Si the state of the silicon carrier is characterized by the presence of lines with chemical shifts - 100 3 M. D. (line Q3and -110 3 M. D. (line Q4) when the ratio of the integral intensities of the lines of Q3/Q4from 0.7 to 1.2, in the infrared spectrum has absorption band of hydroxyl groups with wave number 3620 - 3650 cm-1and the half-width 65 - 75 cm-1and the carrier has a specific surface area measured by the BET method by thermal desorption of argon, SAr= 0.5 to 30 m2/g and the magnitude of the surface, measured by the method of alkaline titration, SNa= 10 - 250 m2/g at a ratio of SNa/SAr= 5 - 30.

5. The catalyst for heterogeneous reactions according to p. 4, characterized in that the active component is in the surface layers pseudolite object structure.

6. The catalyst for heterogeneous reactions according to p. 4, characterized in that it further contains at least one metal and/or oxide selected from 1, 2, 3, 4 groups of the Periodic system in an amount of not more than 1.5%.

7. The catalyst for heterogeneous reactions according to p. 4, characterized in that the carrier has the form of fibers, beads, TRU is emer, deep oxidation of hydrocarbons, partial oxidation of hydrocarbons, alkylation of hydrocarbons, oxidation of sulfur dioxide, hydrogenation of hydrocarbons, ammonia conversion, etc.. including the introduction in vysokoglinozemistyj media containing more than 70% of silicon oxide, compounds active ingredients selected from the group of platinum, palladium, rhodium, iridium, silver, zirconium, chromium, cobalt, Nickel, manganese, copper, tin, gold, titanium, iron, molybdenum in an amount of not more than 2 wt.% (in terms of metal), heat treatment, characterized in that for the preparation of catalysts using the medium in which the NMR spectrum MAS 29Si the state of silicon is characterized by the presence of lines with chemical shifts -100 3 M. D. (line Q3and -110 3 M. D. (line Q4) when the ratio of the integral intensities of the lines of Q3/Q4from 0.7 to 1.2, in the infrared spectrum has absorption band of hydroxyl groups with wave number 3620 - 3650 cm-1and the half-width 65 - 75 cm-1and the carrier has a specific surface area measured by the BET method by thermal desorption of argon, SAr= 0.5 to 30 m2/g and the magnitude of the surface, measured by the method of alkaline titration, SNa= 10 - 250 m2/g at a ratio of S active elements at a temperature of 40 200oC and a pressure of 1 to 200 MPa.

9. A method of producing a catalyst for heterogeneous reactions according to p. 8, characterized in that solutions of the active compounds of the elements have a pH of 2 to 10.

10. A method of producing a catalyst for heterogeneous reactions according to p. 8, characterized in that the impregnating solution of the active element further comprises at least one element 1, 2, 3, 4 groups of the Periodic system in an amount of not more than 1.5 wt.%.

11. A method of producing a catalyst for heterogeneous reactions according to p. 8, characterized in that for the preparation of a catalyst using a carrier that before contact with a solution of the active element is impregnated with at least one element of 1, 2, 3, 4 groups of the Periodic system in an amount of not more than 1.5 wt.%.

12. A method of producing a catalyst for heterogeneous reactions according to p. 8, characterized in that after contact of the carrier with a solution of the active element are impregnated with at least one element of 1, 2, 3, 4 groups of the Periodic system in an amount of not more than 1.5 wt.%.

13. A method of producing a catalyst for heterogeneous reactions according to p. 8, characterized in that after contact with the impregnating solution are hillshade is moorebank carried out at temperatures of 100 800oC in a gas environment or vacuum up to 10-4mm RT.article

 

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