Catalyst for recombination of hydrogen and oxygen and method of making said catalyst

FIELD: chemistry.

SUBSTANCE: invention can be used for hydrogen recombination in reactor sections of nuclear power stations and other facilities. Description is given of a catalyst for recombination of hydrogen and oxygen, containing a solid porous carrier with hydrophobisated catalytic coating of a platinoid metal. This catalyst is distinguished by that, the carrier is made from a valve metal, obtained using powder metallurgical technique, with specific surface are of 0.05-1.50 m2/g; the catalyst carrier is made from porous plates of titanium or o tantalum, or niobium, or zirconium of thickness 0.3-2.0 mm. Described also, is a method of making the said catalyst, involving saturation of the carrier with a solution of platinoid compound, reduction of the said compound to a metal, as well as hydrophobisation of the catalytic coating by moistening it with a suspension of fluorine-containing polymer with an organic stabiliser and subsequent calcination. This method is distinguished by that, the carrier is kept in the suspension for 5-30 s. The carrier is held in a single position and all stages for preparation of hydrophobisated catalytic coating are carried out in that position. Translational oscillations at frequency 1-2 Hz are imparted when saturating the carrier.

EFFECT: provision for reliable functioning of the catalyst for recombination of hydrogen and oxygen in conditions of prolonged contact with wet medium, as well as cutting on preparation time.

3 cl, 1 tbl, 1 ex, 2 dwg

 

The invention relates to the manufacture of catalysts and can be used for recombination of hydrogen in the reactor plants nuclear power plants (NPPs) and other business enterprises, where the leak or accident possibly explosive concentration of hydrogen in a confined space. Working (actually catalytic) component of such catalysts is usually a metal from the group of platinum, often dispersed platinum or palladium, which are applied to the media (based on catalyst) of different shapes, made from stainless steel, a highly porous inert oxides, and other chemically resistant materials. Such catalysts can operate in passive mode, i.e. without additional heating, linking the hydrogen reaction

Heat of reaction (1) leads to the heating of the catalyst, so that the resulting water evaporates from the surface, taking some of the heat:

Patinirovanie media is carried out by deposition of the metal-catalyst or applying to a solution of compounds of platinum, often of a solution of hexachloroplatinic acid (PVC), followed by a chemical recovery (often hydrogen) cation to metal molds, as well as thermal decomposition PVC and other salts of platinum.

Forming the I reactions (1) and (2) water, as well as the moisture of the surrounding gas space may block the surface of the catalyst. In the mode of the Fukushima nuclear disaster is not excluded and periodic flooding of the catalyst. Condensation on the catalyst surface slows casamassimo and can lead to complete passivation of recombination. To prevent "wetting" of the catalyst, it is subjected to a hydrophobization, resulting in its surface becomes water-repellent properties. As the water-repellent agent usually use some non-polar chemical compounds and polymers, in particular powdered Teflon-4.

Known catalyst for the recombination of hydrogen and oxygen, containing a porous solid media gidrofobizirovannym catalytic coating of the metal of the platinum group [1] is similar. In this catalyst carrier is made in the form of cylindrical rods of crystal modification of γ-Al2About3with a specific surface area of about 100 m2/, the Catalyst can operate in conditions of periodic contact with water, but because of the high porosity only briefly (about 1 minute). Possessing hydrophilic properties of γ-Al2About3absorbs up to 30 wt.% water, which significantly slows down the self-heating of the catalyst and reduces its starting characteristics, especially when the tempo is the temperature, close to the room.

Known catalyst for the recombination of hydrogen and oxygen, containing a porous solid media gidrofobizirovannym catalytic coating of the metal of the platinum group [2] is a prototype. In this catalyst carrier is made in the form of plates made of stainless steel substrate with a coating of highly porous aluminum oxide and / or other chemically and thermally stable oxides. However, it will be very difficult to achieve a strong adhesion on steel substrate and to prevent its detachment (shedding) in normal operating conditions. The fact that the catalyst must operate in a wide temperature range from room temperature up to about 600°C, and the two contacting phases are the coefficients of thermal expansion that differ by many times. In addition, the production of such a catalyst requires a fairly complex multi-stage technologies with the use of expensive equipment.

One of the expected results of the invention is to ensure reliable operation of the catalyst for the recombination of hydrogen and oxygen under conditions of prolonged contact with a wet environment.

This result is achieved in that in the catalyst for the recombination of hydrogen and oxygen, containing a porous solid media gidrofobizirovannym catalytic coating and the metal of the platinum group, according to the invention the carrier is made of obtained by powder metallurgy valve metal with a specific surface area of 0.05-1.50 m2/, While the carrier can be made of porous plates titanium, or tantalum, or niobium, or zirconium thickness of 0.3-2.0 mm

A known method of manufacturing a catalyst containing a porous solid media gidrofobizirovannym catalytic coating of the metal of the platinum group, comprising a carrier impregnated with a solution of compounds platinoid, the recovery of the compounds to metal and hydrophobic catalytic coating by wetting his suspension fluorine-containing polymer with an organic stabilizer and subsequent annealing [1] the prototype.

Another expected result of the invention is the reduction of cooking time and reduce the cost of the catalyst by reducing the number of stages of the technological process while maintaining the hydrophobic properties of the catalytic coating.

This is ensured by the fact that in the implementation of the method of manufacturing a catalyst containing a porous solid media gidrofobizirovannym catalytic coating of the metal of the platinum group, comprising a carrier impregnated with a solution of compounds platinoid, restore the specified connection to the metal, and g is totalization catalytic coating by wetting his suspension fluorine-containing polymer with an organic stabilizer and subsequent calcination, according to the invention the time-keeping media in suspension is 5-30 s, the carrier is fixed in one position, and in this position perform all stages of preparation gidrofobizirovannogo catalytic coating, during the impregnation of the carrier reported sustained oscillations with a frequency of 1-2 Hz.

Porous metal produced by the method of powder metallurgy, preferably titanium, does not require additional coating of highly porous substrate and has a relatively low specific surface. The number of stages of preparation of a new catalyst is limited by the stage of impregnation of porous titanium in solution PVC (no more than 1 hour), short-term immersion in a suspension of water-repellent (no more than 20 seconds) and annealing in a furnace less than 1 hour. General technological cycle of preparation of a new catalyst requires no more than two hours.

Figure 1 shows schematically the sequence of manufacture of the catalyst according to the invention; figure 2 - setup for testing of the catalyst of this type.

To simplify technology and reducing losses PVC original carrier - plate 1 made of porous titanium clip (figure 1) in a hanging position using titanium wires 2 tripod 3. In this fixed position, the plates pass all three stages (a, b, C) preparation of ka is alistor. Tripod with 3 plates 1 only transferred from one technological cycle in the other, and immersion are only processed plate 1.

In the first stage And the plate 1 made of porous titanium impregnated with a solution PVC in the tub 4, indicated by the lines 5, 6 are not shown in the drawing by thermostat. For intensification of mass transfer in the solution to the arm 3 by means of a vibrator (shaker) 7 report of the horizontal translational oscillations with a frequency of 1-2 Hz. In the second stage In plate 1 5-30 seconds is placed into the tub 8, is filled with a suspension of fluorine-containing polymer with an organic stabilizer. And finally, at the stage With plate 1 calcined in a furnace 9, where both are two main processes: patinirovanie media and the formation of a protective film of a porous water-repellent. During annealing the decomposition of the stabilizer suspension to simple monomers. These products, with strong reducing properties, restore PVC to metallic platinum. As a result, in the pores of the support (porous titanium) is formed of a catalytically active layer of the dispersed platinum mixed with the dispersed phase gidrofobizirovannogo coverage. For the preparation of catalytic plates with a total area of 90 DM2this installation requires no more than two hours.

Catalic the ical phase dispersed platinum firmly adsorbed in the surface of the porous layer of the device - porous titanium, without application of the special substrate-sorbent. Low specific surface of porous titanium (0.05 to 1.50 m2/g) sufficient for sorption of disperse platinum, on the one hand, and practically does not create conditions for the sorption of large quantities of water: maximum water sorption in porous titanium is less than 0.3 wt%. The fact that the metal catalyst (platinum) sorbed directly in the media, good adhesion is achieved platinum.

Check the quality of the prepared catalyst is performed on the test machine (figure 2) in a special chamber 10. The camera is equipped with a thermostat 11, a nozzle 12 for dosed injection of hydrogen from the electrolytic cell (not shown), the analyzer 13 of the hydrogen concentration, the device 14 for dehumidification or humidification of the gas space, the fixing device 15 of the specimen (plate 1 area of 200 cm2) catalyst, a temperature measurement system in the chamber and the samples (not shown) by means of thermocouples 16, and a computer processing system kinetic and temperature data (not shown).

The quality of the catalyst is evaluated by three parameters: activation time (τactin short, specific recombination velocity of hydrogen (i) in milliliters oxidizable hydrogen for 1 minute, referred to the unit width is s the lower part of the sample (ml/min cm), and the time of reactivation (time of return to active status) of the sample in minutes after 10-30 minutes of submersion in water (τreact). For this purpose the samples (plate 1) of the catalyst is alternately placed in the camera 10 (hung under the lid)filled with air with the hydrogen content of about 2% vol. at 25°C. the sample Temperature is controlled using a chromel-alumaloy thermocouple 16.

Example. Plate 1 made of porous titanium with a specific surface area of from 0.05 to 1.50 m2/g of various sizes with a thickness of 0.9 mm, hanging on titanium wires 2 to the tripod 3 (figure 1), was immersed in a solution with PVC at a temperature of 75°C. For intensification of mass transfer to the arm 3 by means of a shaker 7 reported progressive horizontal vibrations with a frequency of 1 to 2 Hz. 10 minutes after the end of the sorption process PVC plate was removed from the bath and for different samples of 5-30 seconds, immersed in a bath of 8 with an aqueous suspension of PTFE powder brand f-4D and then for 30 minutes was placed for calcination in the furnace 9 at a temperature of 310°C. the Cooled after annealing the catalyst samples were tested in the chamber 10 (figure 2). The contact time of the sample with water during the tests was 13 minutes. The test results of samples of different shapes and areas listed in the following table.

Stationary hydrogen concentration, % vol.The activation time (τactin minutesSpecific activity (i) in ml/min cmThe period of reactivation (τreactin minutes
3,2×10,02,07<147,5<1
4,8×10,0to 2.06<144,17<1
10,0 x 10,02,04<143,4<1
10,0×6,42,07<142,5<1
10,0×7,02,07<138,9<1
10,0×7,22,02<136,1<1
15,0×4,02,00<1 39,1<1
20,0×4,01,99<140,0<1

As can be seen from the table, both parameters are: τactand τreactdo not exceed 1 minute, which is considerably less than the time of reactivation for samples of the catalyst according to [1, 2].

Sources of information

1. SU # 1747146, 5 01J 37/02, 1990.

2. A two-pronged approach to hydrogen reduction. / Reinhard Heck and Axel Hill // Nuclear Engineering International. July 1992, p.21-28.

1. The catalyst for the recombination of hydrogen and oxygen, containing a porous solid media gidrofobizirovannym catalytic coating of the metal of the platinum group, characterized in that the carrier is made of obtained by powder metallurgy valve metal with a specific surface area of 0.05-1.50 m2/year

2. The catalyst according to claim 1, characterized in that the carrier made of a porous plates of titanium or tantalum, or niobium, or zirconium thickness of 0.3-2.0 mm

3. A method of manufacturing a catalyst corresponding to one of claim 1 or 2, comprising a carrier impregnated with a solution of compounds platinoid, the recovery of the compounds to metal and hydrophobic catalytic coating by wetting his suspension fluorine-containing polymer is an organic stabilizer and subsequent calcination, characterized in that the time-keeping media in suspension is 5-30 s, the carrier is fixed in one position and in this position perform all stages of preparation gidrofobizirovannogo catalytic coating and during the impregnation of the carrier reported sustained oscillations with a frequency of 1-2 Hz.



 

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