Method of production of hydrogen and aluminum oxides or hydroxides and the device for the method realization

FIELD: chemical industry; reactor.

SUBSTANCE: the invention is pertaining to reactor. The method includes preparation of suspension of the finely dispersive powdery aluminum in water, creation in the reactor of pressure of the saturated water steams, sputtering of the suspension into the high-pressure reactor, withdrawal from the reactor of the mixture of the steams and hydrogen, and also withdrawal from the reactor of aluminum hydroxide or aluminum oxide into the receiving device, measuring of the temperature in the reactor, measuring of the gas mixture pressure in the reactor. Determine the partial pressure of the saturated water steam in the reactor, determine the partial pressure of hydrogen, determine the free volume of the reactor and, changing the mass of aluminum being introduced in the composition of the suspension according to the formula make adjustment of the pressure and temperatures in the reactor. The device contains: the source of the suspension of the finely-dispersed powdery aluminum with water and the mixer, the reactor, the condenser, the receiving device, the adjustable valve of the mixture withdrawal of the mixture of the water steams and hydrogen, the adjustable valve of withdrawal of aluminum hydroxides or oxides, the sensor of the reactor temperature, the sensor of pressure on the inlet of the suspension delivery into the reactor, the sensor of pressure on the outlet of the steam-gas mixture, and the sensor of pressure in front of the inlet of the steam- gas mixture into the condenser, the adjustable tool of the suspension delivery into the reactor, the main control unit with the inlet and the outlet. At that the source of suspension contains the adjustable tool of the water delivery and the adjustable tool of delivery of the aluminum powder. The invention allows to improve stability of the reactor operation.

EFFECT: the invention ensures the improved stability of the reactor operation.

5 cl, 3 dwg, 1 tbl

 

The invention relates to methods of producing hydroxides or oxides of aluminum, namely a process for the production of oxides or hydroxides of aluminum from aluminum metal oxidation in the aquatic environment. The oxides and hydroxides of aluminum used in various industries as adsorbents, catalysts, and the like, Hydroxides and oxides of aluminum of high purity are used in electronic and optical industry in the form of fine powder as abrasive powders, in particular, for hard disks or magnetic heads. The invention relates in particular to methods for hydroxides of aluminum bemani and bayerite form.

The method also applies to the production of hydrogen, namely to methods of producing hydrogen by chemical interaction of metals and water. Hydrogen can be used in various chemical processes as a deoxidizer, and in certain conditions as fuel.

Aluminum hydroxide exist in different crystalline forms of hydrargillite, bayerite, Diaspora, boehmite, etc., the oxides in the form of alpha, gamma, theta forms. The main difference between these forms is the location of ions of aluminum and oxygen ions relative to each other. In this description, the term "aluminum hydroxide" refers also and hydrated oxides of aluminum Al2About3.

OS the ESD method for industrial preparation of hydroxides of aluminum is the Bayer process, and subsequent drying and calcination leads to the production of aluminum oxide [Chemical encyclopedia, ed, "Soviet encyclopedia", M, 1988, vol. 1, s-214]. However, conventional methods for producing hydroxides of aluminum does not achieve the high purity (and uniformity in the structure of the product.

Known [U.S. patent 5225229, CL 423/629, Aluminum Company of America, publ. 06.07.1993,] the production method hidroxizina aluminum, which reacts with water in the liquid phase at a pH of about 12.4 with aluminum. At such pH hydrolysed aluminum is produced with acceptable speed as when the dispersion with the surface of the particles 75000 mm2/g and 50000 mm2/, Reaction is possible at values less than 50000 mm2/g, up to 20000 mm2/, In accordance with another form of way to the water is added as a catalyst an organic substance is chlorine. The disadvantage of the proposed method is the necessity of increasing pH, which is produced by adding substances that provide such high pH values. Therefore, this method does not provide the necessary hygiene products. In addition, the process proceeds with insufficient speed.

The prototype of the present invention is a method of producing hydroxides or oxides of aluminum and hydrogen from aluminum and water [RF patent 2223221, CL 01 F 7/42, firma RICK SPb", publ. 1.02.2004,], which of the fine alumina particle size of not more than 20 μm preparing a suspension of aluminum powder in water at a ratio of Al:N2O=1:4-16 parts by weight of the Suspension is continuously fed into the reactor high pressure, where it is sprayed when the diameter of droplets less than 100 microns in water. From the reactor the steam gas fed into the condenser, where hydrogen is separated from water vapor. The aluminum hydroxide or aluminum oxide are received in the receiving device for hydroxides. Changing the ranges of temperature and pressure in the rector, and the weight ratio of participating in the reaction of aluminum and water, receive necessary in each case the form of hydroxides of aluminum: beitou, bayerite, and alpha-oxide, theta-oxide, gamma-alumina and a mixture of hydroxides of aluminum bemani and bayerite form. The process occurs in the plant, including the mixer, reactor pressure vessels, equipped with a nozzle, providing a spray suspension of aluminum powder in the water when the diameter of droplets less than 100 microns, a receptor for hydroxides, condenser. To obtain high purity hydrogen using distilled water. The method has a number of advantages: it is continuous, in the reactions involved only water and aluminum, which ensures the purity of the obtained products (hydroxides and oxides of aluminum is Oia, and hydrogen), changes of regimes of temperature and pressure determine the appearance of the products. It should be noted that the ranges of pressure and temperature in the reactor with this method is supported by continuous removal of steam and gas and the suspension of aluminum hydroxide. This support represents a serious technical challenge, because the relationship between pressure, temperature and mass of the exhaust gas and a suspension of aluminum hydroxide is determined by a rather complicated formula that takes into account the partial pressure of saturated water vapor and hydrogen, the mass of injected aluminum, the temperature in the reactor, the free volume of the reactor. Dynamic change of these factors makes it inadequate as a regulatory factor only removal from the reactor the reaction products, does not provide the necessary precision maintenance regimes in the reactor in the absence of feedback between the processes occurring in the reactor, and a source supplied suspension. In addition, during the preliminary preparation of a suspension of fine aluminium powder and water used in this way, there is no possibility to change the composition of the suspension when the variance regimes of temperature and pressure in the reactor. When storing the prepared suspension is partial oxidation of aluminium powder which leads to actual changes in the composition of the supplied suspension. At the same time in the mixer is hydrogen gas, which affects the safety of the process. These problems are eliminated by the proposed method.

The aim of the proposed method is to provide the required parameters of the process to ensure you receive the output products of a given type and purity. We solve such technical problems as increasing the reliability of operation of the reactor and its stability.

The essence of the method consists in obtaining hydroxides or oxides of aluminum and hydrogen from the slurry of fine powder of aluminum in water. It includes the preparation of a suspension of fine powder of aluminum in water, creating a reactor pressure of saturated water vapor, spraying the suspension into the reactor high pressure, the output from the rector of the mixture of water vapor and hydrogen, and the output from the reactor aluminum hydroxide or aluminum oxide in the receiving device, the measurement temperature T in the reactor, measuring the pressure of the gas mixture P in the reactor. (Followed by the distinguishing signs of the way). Determine the partial pressure of saturated water vaporin the reactor, determine the partial pressure of hydrogendetermine the free volume of the reactor VCEand regulate the pressure P and the temperature T in the reactor by changing the mass introduced into the composition of the suspension aluminum m Alin accordance with the formula

where R is the universal gas constant (8,317 j/mol·hail).

In addition, it is proposed a method of producing hydroxides or oxides of aluminum and hydrogen from the slurry of fine powder of aluminum in water, in which the adjustment of the pressure and temperature in the reactor is produced by changing the ratio of Al:N2O in suspension, and to bayerite form of the hydroxide, the ratio of Al:N2O=1:7-14 parts by weight, to obtain bemani form of the hydroxide, the ratio of Al:N2O=1:5-12 parts by weight, to obtain a mixture ballerinas and bemani forms hydroxide, the ratio of Al:N2O=1:5-14 parts by weight, to obtain a gamma-alumina ratio of Al:N2O=1:4-8 parts by weight, to obtain a theta-alumina ratio of Al:N2O=1:4-7 parts by weight, to obtain alpha-alumina ratio of Al:N2O=1:3-5 parts by weight of

The essence of the proposed device for receiving the hydroxides or oxides of aluminum and hydrogen is that it contains a source of fine suspension of aluminum powder with water with a mixer, a reactor, a condenser, a receiver, an adjustable valve is venting the mixture of water vapor and hydrogen, adjustable valve exhaust hydroxides or oxides of aluminum, the temperature sensor in the reactor, the pressure sensor at the inlet p is the giving of the suspension in the reactor, the pressure sensor on the output vapor-gas mixture, and the pressure sensor before entering the vapor-gas mixture in the condenser. (Followed by the distinguishing characteristics of the proposed device). Additionally, it includes adjustable means for supplying slurry to the reactor and master controller with input and output, and the source of suspension contains adjustable means for supplying water and adjustable means for supplying a powder of aluminum, the input controller connected to the temperature sensor in the reactor and the specified pressure sensors, and the output of the controller is connected to the source of the suspension, adjustable means for supplying a suspension of fine powder of aluminum with water in the reactor, valve regulated drain mixture of water vapor and hydrogen, and an adjustable valve exhaust hydroxides or oxides of aluminum.

In addition, it is proposed a device in which the adjustable means for supplying a suspension of fine powder of aluminum in water contains a high-pressure pump and an adjustable valve.

In addition, it is proposed a device in which the adjustable means for supplying a suspension of fine powder of aluminum in water contains an adjustable high-pressure pump.

The controller can be part of automatic control systems and process control and associated with the machine top level inter what Asom.

The proposed method and device for its implementation are explained in the following figures:

figure 1 shows a block diagram of the device

figure 2 shows the functional diagram of the controller,

figure 3 shows a functional diagram of the machine at the top level.

List of approved symbols:

1. adjustable source of fine suspension of aluminum powder with water,

2. adjustable means for supplying aluminium powder,

3. adjustable means for supplying water,

4. adjustable means for supplying a specified suspension in the reactor,

5. the high-pressure pump,

6. valve

7. controller

8. reactor

9. the capacitor

10. the receiving device

11. the pressure sensor at the inlet of the feed suspension in the reactor,

12. the pressure sensor on the output vapor-gas mixture,

13. the pressure sensor before entering the vapor-gas mixture in the condenser,

14. adjustable valve exhaust mixture of water vapor and hydrogen

15. adjustable valve exhaust hydroxides or oxides of aluminum,

16. the temperature sensor inside the reactor,

17. the temperature sensor on the reactor vessel,

18. the input of the controller

19. the output of the controller,

20. mixer,

21. automatic system monitoring and control (ACMS),

22. machine upper level (MVD),

23. input modules discrete signals,

24. input modules analog si is the Nala

25. output modules discrete signals,

26. output modules analog signals

27. the processor module controller

28. network adapter controller

29. network adapter MVD,

30. the processor module MVD,

31. software module process control,

32. database source parameters

33. software module editing the database to the original settings.

In the block diagram of the device shown in figure 1 installation including a source of fine suspension of aluminum powder with water 1, the reactor 8, the receiver (tank for suspension) 10, a condenser 9, adjustable means for supplying a specified suspension in the reactor 4, the controller 7. Source suspension 1 includes adjustable means for supplying powder aluminum 2, representing the auger device with adjustable drive; adjustable means for supplying water 3 - flow regulator company Bronkhorst high-Tech B.V. aluminium Powder and water are sent to the mixer 20 is a vessel made of stainless steel and equipped with a mixing device. Source mixture 1 is connected with an adjustable means for supplying slurry to the reactor 4, which contains a high pressure pump membrane type company URACA 5 and the valve 6 firms LH Automatics. Suspension of aluminium powder with water fed into the reactor 8, which represents the device operating p is d high pressure, equipped with a nozzle, providing a spray suspension of aluminum powder in water to the diameter of droplets less than 100 microns. The reactor has an internal temperature sensor 16, the reactor vessel has a temperature sensor 17, at the entrance of the feed suspension is connected to the pressure sensor 11, the output vapor-gas mixture is connected to the pressure sensor 12. From the upper part of the reactor a mixture of water vapor and hydrogen discharged through the adjustable valve 14 to the condenser 9, where the separation of water vapor from the hydrogen. Before entering the condenser is the pressure sensor 13. From the bottom of the reactor through an adjustable valve 15 in the collector 10 are displayed hydroxides and oxides of aluminum. Adjustable valves 14, 15 firms LH Automatics. For measuring pressure and temperature sensors are used company Metran. The controller 7 has a control input 18 and the output control 19, in addition, it is connected to the computer (machine) top level in figure 1 is not shown.

Figure 2 shows the functional diagram of the controller 7. The processor module controller 27 is connected to the input modules discrete signals 23 and input modules analog signals 24, which, in turn, is connected to the control input of the controller 18. In addition, the processor module controller 27 is connected to the output modules discrete signals 25 and output modules anal the trade signals 26, which, in turn, is connected to the control output of the controller 19. In addition, the processor module controller 27 is connected through network adapters 28 and 29 with the computer the fan 22 (see figure 2 and 3). The controller 7, for example, type CM 1820M CP provides input 128 discrete signals "dry contact" with the power of these contacts from internal (12V) power source, the output 64 of discrete signals through normally open relay contacts 10 a, 220 VAC 50 Hz, input 64 analog signals 4÷20 mA and 4 analogue output 4÷20 mA. The discrete input signals are 4 modules 23 digital I MDW (32 channels per module) and 8 modules cross-discrete I/o MKDV/B1.1 (16 channels per module), the output digital signals is carried out in 2 modules 25 discrete output Mdiv and 4 modules relay cross MCR, input/output of analog signals is provided by 4 modules 26 MEV and 4 modules cross analog input MCAV. The processor module 27 MP has an integrated channel RS232/485 22 for communication with the machine 22 of the upper level at speeds up to 115200 bit/sec.

Figure 3 shows a functional diagram of the machine the upper level 22. The processor module 30 of the fan is connected via a network adapter 29 MVD controller 7. In addition, the module 30 is connected with the software module management is the process of 31, which, in turn, is connected to the base data source parameters 32. Database source settings 32 is connected also with the software module editing database source settings 33.

The implementation of the method

In order to place the active interaction of powdered aluminum metal with water in the reaction

2Al+4H2O=2AlO+3H2(gas)+Q (kcal)

it is necessary to provide a fine atomization of a suspension of aluminium powder with water in a reactor, in which there is water and its vapor at a temperature of 250-400°and the pressure of 10-20 MPa, and the ratio fed to the reactor slurry to the water, and with pairs that are in the reactor, should be 1:50-100 parts by weight of the amount of droplets injected suspension should be less than 100 microns.

When implementing the method in the reactor 8 is pre-supplied water is heated to generate saturated water vapor to a temperature of 250-400°C and a pressure of 10-20 MPa. If we achieve these values of these parameters from source 1 preparation of a suspension with adjustable means of 4 a suspension of fine powder of aluminum with a specified flow rate and the ratio of Al and N2About fed into the reactor 8.

The resulting products are continuously withdrawn from the reactor. The hydrogen in the composition of the gas (about 25 wt.% hydrogen and about 75 wt.% water), hydroc the IDA (oxides) of aluminum in the form of an aqueous suspension (25-35 wt.% hydroxides (oxides) are discharged from the reactor to the stage of separation.

The process control operation is as follows:

In ACMS 21 are inserted into the specified mass flow rate of the obtained hydroxides and hydrogen, the ratio of Al and N2O suspension, specifying the type of the obtained hydroxides, calculated values of pressure and temperature in the reactor. The controller 7 generates the appropriate control signals to the means 2 and 3 supply of aluminium powder and distilled water, asking their nominal costs. Depending on the set values of the mass flow per unit time obtained hydroxides and hydrogen serves control signals to the adjustable valves 14, 15 mounted on the respective lines, defining their area of passage, control signals to the means for supplying the suspension 4 in the reactor (pump and control valve ). Two adjustable elements due to the fact that large expenditures suspension precisely set by adjusting the performance of the pump 5, and a small - adjustable valve 6. In a stationary mode of oxidation of aluminum in the reactor pressure therein is determined by the sum of partial pressures of water vaporand released in the reaction of hydrogen:

the temperature in the reactor Tp(the readings of the sensor is 16) is determined from a table of values of the saturated vapor pressure of water temperature.

The partial pressure of hydrogenis determined from the equation of clayperon-periodic, which is true in these conditions:

,

whereis the mass of hydrogen released per unit of time,

- molar mass,

R is the universal gas constant (8,317·j/mol·hail),

Tp- the temperature in the reactor,

VSt- free volume of the reactor.

Free volume of the reactor VStis part of the geometric volume of the reactor Vpless volume, which is initially poured into water (adjusted for expansion at a given temperature)and volume of a suspension of aluminium powder with water received in the reactor before the start of steady state hydrogen Vsusp.

The reaction of interaction of aluminum with water, 1 g·mol Al gives 1.5 g·mol H2i.e. in the complete oxidation of 9 g Al give 1 g of H2.

Then the equation (2) takes the following form:

,

where mAl- weight of aluminum entering the reactor per unit time.

Thus, in a hundred is ionamim mode

The program of the controller are calculated values: Tass,VSt.

Thus, adjustment of the pressure in the reactor 8, and therefore, the amount of hydrogen can be produced by changing the mass fed to the reactor aluminium.

The controller compares the readings from the pressure sensor R with the selected optimal value of P and, in case of rejection of these values produces by the formula (5) control signals to the means for supplying aluminium, adjusting the mass fed to the reactor aluminium.

The temperature sensor on the reactor vessel 17 serves to prevent emergency situations associated with overheating of the reactor.

If necessary, obtain products of high purity is used purified water such as distilled, however, the way allows you to use regular water.

Table

The results of experimental studies of the modes of obtaining hydroxides and oxides of aluminum
№ p/pBrand aluminium powderThe ratio of Al/N2O suspensionThe parameters in the reactorView of the obtained hydroxides and oxides of aluminum is
P, MPaT °
1ASD-41/6,517360AlOOH boehmite
2ASD-41/717340AlOOH boehmite
3DCA-61/717380AlOOH boehmite
4DCA-61/7,517360AlOOH boehmite
5DCA-61/818340AlOOH boehmite
6ASD-41/915250Al(OH)3bayerite
7ASD-41/1014240Al(OH)3bayerite
8DCA-61/1114250Al(OH)3bayerite
9ASD-41/5,515450θ-Al2About3theta-oxide
10DCA-61/615460θ-Al2About3theta-oxide
11ASD-41/52051 γ-Al2About3gamma-oxide
12DCA-61/520550γ-Al2O3 gamma-oxide
13DCA-61/2251050α-Al2About3alpha-oxide

The resulting method is characterized by waste reduction, manufacturability, performance, and environmental safety. Installation created mainly on the basis of commercially available items, custom-fabricated reactor vessel with the necessary mains input and output of processed products. In addition, we developed the corresponding software CONTROL.

1. The method of producing hydroxides or oxides of aluminum and hydrogen, comprising preparing a suspension of fine powder of aluminum in water, creating a reactor pressure of saturated water vapor, spraying the suspension into the reactor high pressure, the output from the reactor a mixture of water vapor and hydrogen, and the output from the reactor aluminum hydroxide or aluminum oxide in the receiving device, the measurement temperature T in the reactor, measuring the pressure of the gas mixture P in the reactor, characterized in that to determine the partial pressure of saturated water vaporbreakcore, determine the partial pressure of hydrogendetermine the free volume of the reactor VStand, by changing the mass introduced into the composition of the suspension aluminum mAlin accordance with the formula

where R is the universal gas constant,

regulate pressure and temperature in the reactor.

2. The method according to claim 1, characterized in that the adjustment of pressure and temperature in the reactor is produced by changing the ratio of Al:H2O in suspension, and to bayerite form of the hydroxide, the ratio of Al:N2O=1:7-14 parts by weight, to obtain bemani form of the hydroxide, the ratio of Al:N2O=1:5-12 parts by weight, to obtain a mixture ballerinas and bemani forms hydroxide, the ratio of Al:N2O=1:5-14 parts by weight, to obtain a gamma-alumina ratio of Al:N2O=1:4-8 parts by weight, to obtain a theta-alumina ratio of Al:N2O=1:4-7 parts by weight, to obtain alpha-alumina ratio of Al:N2O=1:3-5 parts by weight of

3. A device for receiving hydroxides or oxides of aluminum and hydrogen containing source suspension (1) a fine powder of aluminum with water with a mixer (20), the reactor (8), the condenser (9), the receiving device (10), an adjustable valve (14) removal of the mixture of water vapor and hydrogen, adjustable valve (15) drainage hidroxidului of aluminum oxide, the temperature sensor (16) of the reactor, the pressure sensor (11) at the input of the feed suspension in the reactor, the pressure sensor (12) on the output vapor-gas mixture and the pressure sensor (13) before entering the vapor-gas mixture in the condenser, characterized in that it comprises adjustable means (4) feeding the suspension into the reactor, the control unit (7) with an inlet (18) and outlet (19), and the source of suspension (1) includes adjustable means for supplying water (3) and adjustable means for supplying aluminium powder (2), entrance (18) controller (7) is connected to the sensor (16) the temperature in the reactor and the pressure sensors (11, 12, 13)and the outlet (19) of the controller (7) is connected to the source of suspension (1), adjustable means (4) filing of a suspension of fine powder of aluminum with water in the reactor, an adjustable valve (14) removal of the mixture of water vapor and hydrogen, and an adjustable valve (15) removal of hydroxides or oxides of aluminum.

4. The device according to claim 3, characterized in that the adjustable means (4) filing of a suspension of fine powder of aluminum in water contains a high-pressure pump (5) with adjustable valve (6).

5. The device according to claim 3, characterized in that the adjustable means (4) filing of a suspension of fine powder of aluminum in water contains an adjustable high-pressure pump.



 

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The invention relates to a method and apparatus for obtaining hydroxides or oxides of aluminum, namely a process for the production of oxides or hydroxides of aluminum from aluminum metal oxidation

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The invention relates to the technology of producing alumina, which can be used as desiccant of gases and liquids, absorbent, carrier catalysts

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24 cl, 2 dwg

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36 cl, 2 dwg

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21 cl, 2 dwg, 1 tbl, 9 ex

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21 cl, 2 dwg, 1 tbl, 9 ex

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11 cl, 1 tbl, 8 ex

FIELD: gas production technologies.

SUBSTANCE: invention relates to production of hydrogen-rich and/or carbon monoxide-rich gases, which is accomplished in reactor having upper and lower parts and involves introducing hydrocarbon feedstock preheated to 400-700°C into upper part of reactor. In this part of reactor, hydrocarbon feedstock is mixed with water steam and oxygen-containing atmosphere resulting in a partial oxidation of feedstock. Partially oxidized feedstock, if necessary, comes into contact with reforming catalyst located in lower part of reactor in presence of water steam. At the same time, a part of partially oxidized feedstock contacts with steam reforming catalyst disposed at least on the surface of upper part of reactor. Mixing of feedstock with water steam and oxygen-containing atmosphere is effected in amounts providing oxygen-to-carbon molar ratio between 0.5:1 and 0.7:1 and water steam-to-carbon between 0.5:1 and 1.5:1.

EFFECT: considerably reduced formation of carbon black in combustion zone under critical process conditions.

1 dwg, 1 tbl, 2 ex

FIELD: hydrocarbon conversion catalysts.

SUBSTANCE: catalyst for generation of synthesis gas via catalytic conversion of hydrocarbons is a complex composite composed of ceramic matrix and, dispersed throughout the matrix, coarse particles of a material and their aggregates in amounts from 0.5 to 70% by weight. Catalyst comprises system of parallel and/or crossing channels. Dispersed material is selected from rare-earth and transition metal oxides, and mixtures thereof, metals and alloys thereof, period 4 metal carbides, and mixtures thereof, which differ from the matrix in what concerns both composition and structure. Preparation procedure comprises providing homogenous mass containing caking-able ceramic matrix material and material to be dispersed, appropriately shaping the mass, and heat treatment. Material to be dispersed are powders containing metallic aluminum. Homogenous mass is used for impregnation of fibrous and/or woven materials forming on caking system of parallel and/or perpendicularly crossing channels. Before heat treatment, shaped mass is preliminarily treated under hydrothermal conditions.

EFFECT: increased resistance of catalyst to thermal impacts with sufficiently high specific surface and activity retained.

4 cl, 1 tbl, 8 ex

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