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INVENTION
Russian Federation Patent RU2278077
METHOD FOR PRODUCING hydroxides or aluminum oxides
AND HYDROGEN AND DEVICE FOR ITS IMPLEMENTATION
Name of the inventor: Bersh Alexander V. (RU); Ivanov Yuri Leonidovich (RU); Mazalov Yury Alexandrovich (RU); Anton Glukhov (RU); Trubachov Oleg
The name of the patentee: Bersh Alexander V. (RU); Ivanov Yuri Leonidovich (RU); Mazalov Yuri Alexandrovich
Address for correspondence: 107065, Moscow, ul. Khabarovsk, 23, building 3, kv.480, AB Entin
Starting date of the patent: 2005.07.11
The invention relates to the production of hydrogen, aluminum hydroxides or oxides of aluminum metal. The method includes preparing a suspension of finely powdered aluminum in the water, creating a saturated water vapor pressure reactor, spraying the slurry in a pressure reactor, the output from the reactor a mixture of water vapor and hydrogen, but also output from the reactor of aluminum hydroxide or alumina in the receiving device, a temperature measurement in the reactor pressure measurement of the gas mixture in the reactor. Determine the partial pressure of saturated water vapor in the reactor, the hydrogen partial pressure is determined, determine the free volume of the reactor and by changing the weight of aluminum introduced in the suspension in accordance with the formula, produce temperature and pressure control in the reactor. The apparatus comprises a source of a slurry of finely divided aluminum powder and water with a mixer, reactor, condenser, receiver, an adjustable valve discharge a mixture of water vapor and hydrogen adjustment valve outlet hydroxides or aluminas, the reactor temperature sensor, a pressure sensor on the slurry reactor inlet sensor outlet pressure and gas mixture pressure sensor vapor mixture prior to entering the condenser, adjustable suspension means for feeding the reactor with the master controller input and output, wherein the suspension comprises an adjustable source of water supply means and controlled means for feeding alumina powder. The invention increases the stability of the reactor.
DESCRIPTION OF THE INVENTION
The invention relates to methods for producing aluminum oxides or hydroxides, namely - to methods for producing aluminum oxides or hydroxides of aluminum metal by oxidation in an aqueous medium. Aluminum oxides and hydroxides are used in various industrial fields as adsorbents, catalysts, etc. And hydroxides of high purity aluminum oxide used in the electronics and optical industries 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 producing aluminum hydroxide and boehmite bayeritnoy form.
The method applies to the production of hydrogen - namely, to methods of producing hydrogen by chemical interaction of water and metals. Hydrogen can be used in various chemical processes as a reducing agent, and in certain conditions, as a fuel.
aluminum hydroxides exist in different crystal forms - hydrargillite, bayerite, diaspore, boehmite, etc., oxides - as alpha, gamma, theta forms. The main difference between these forms is the arrangement of the aluminum ions and the oxygen ions relative to each other. As used herein, the term "aluminum hydroxide" means and hydrated aluminum oxides and Al 2 O 3.
The main method of industrial production of aluminum hydroxide is the Bayer process and their subsequent drying and calcination results in alumina [Chemical Encyclopedia, ed, "Soviet encyclopedia", M., 1988, vol.1, s.213-214]. However, conventional methods for producing aluminum hydroxide does not provide achievement of high purity (homogeneity and structure) of product.
It is known [US patent 5225229, cl. 423/629, Aluminum Company of America, publ. 7.6.1993 g] gidrokisida method for producing aluminum, in which the reaction of water in the liquid phase at a pH of about 12.4 with aluminum. At this pH gidrokisid alumina produced an acceptable rate of dispersion as in the particle surface with an area of 75,000 mm 2 / g and 50,000 mm 2 / g. Reaction is possible even with values less than 50 000 mm 2 / g, up to 20,000 mm 2 / g. In accordance with another mode of the method the water is added as a catalyst in organic matter - chlorine. A disadvantage of the method is the need to raise the pH, which is made by adding substances providing such a high pH. Therefore, this method does not provide the required product purity. Additionally, the process proceeds with insufficient speed.
The prototype of the proposed invention is a method for producing aluminum hydroxides or oxides and hydrogen from aluminum and water [RF patent 2223221, cl. C 01 F 7/42, ZAO "Firma Rick St. Petersburg", publ. 10.02.2004], wherein the fine alumina particles of size less than 20 microns of aluminum powder suspension was prepared in water at a ratio of Al: H 2 O = 1: 4-16 pbw The slurry is continuously fed into a high pressure reactor, where sprayed less than 100 microns in the water droplet diameter. Steam and gas is fed from the reactor to a condenser, where hydrogen is separated from the water vapor. aluminum hydroxide or aluminum oxide input into the receiving device hydroxides. By varying the temperature and pressure ranges in the reactor, but also the weight ratios involved in the reaction of aluminum and water, is prepared necessary in each case forms of aluminum hydroxide: boehmite, bayeritnuyu and alpha-alumina, theta-alumina, gamma-alumina and a mixture of hydroxides, boehmite and aluminum bayeritnoy form. Implementation of the method occurs in a plant comprising a mixer, a high pressure reactor equipped with a nozzle providing atomization of powdered aluminum in water suspension droplets with a diameter less than 100 microns, the receiving device hydroxides capacitor. To obtain high-purity hydrogen using distilled water. The method has many advantages: it is continuous, participate in reactions only water and aluminum, which ensures the purity of the resulting products (aluminum oxides and hydroxides, hydrogen and a) changes modes - the temperature and pressure determine the type of products obtained. It should be noted that the required temperature and pressure ranges of the reactor during this process are maintained by continuous removal of steam-gas and aluminum hydroxide suspension. This support is a major technical challenge, since the relationship between the pressure, temperature and weight allocated steam-gas and aluminum hydroxide suspension 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 is not doing enough as a regulatory factor only removal of the reaction products, do not provide the required accuracy of the maintenance mode in a reactor in the absence of feedback between the processes taking place in the reactor, and the source of the feed slurry. Furthermore, when pre-cooking the slurry of fine aluminum powder and water used in this method, there is no possibility to change the composition of the suspension mode for deviations in temperature and pressure in the reactor. When storing the prepared suspension is a partial oxidation of aluminum powder, which leads to a change in the actual composition of the feed slurry. In the mixer hydrogen evolution occurs that affects the safety of the process. Given the proposed method eliminates the disadvantages.
The aim of the process is to provide the necessary process parameters to guarantee receipt of the output of products specified type and purity. Solve such technical problems as increasing the reliability of the reactor and its stability.
The essence of the proposed method consists in obtaining hydroxides or aluminum oxides and hydrogen from a suspension of finely powdered aluminum in water. It includes preparing a suspension of finely powdered aluminum in the water, creating a saturated water vapor pressure reactor, spraying the slurry in a pressure reactor, the output from the reactor a mixture of water vapor and hydrogen, but also output from the reactor of aluminum hydroxide or alumina in the receiving device, a temperature measurement T in the reactor, the gas mixture the pressure measurement P into the reactor. (The following are features of the method). Determine the partial pressure of saturated water vapor 
in the reactor the hydrogen partial pressure is determined 
Determine the free volume of the reactor V lo and produce adjustment pressure P and temperature T within the reactor change in composition administered mass m Al aluminum slurry in accordance with the formula
where R - universal gas constant (8.317 J / mol · deg).
Furthermore, a process for producing hydroxides or aluminum oxides and hydrogen from a suspension of finely powdered aluminum in water, wherein the pressure and temperature control in the reactor is produced by changing the ratio of Al: H 2 O in the slurry and to obtain bayeritnoy forms hydroxide ratio Al: H 2 O = 1: 7-14 parts by weight, to obtain a hydroxide form boehmite ratio Al: H 2 O = 1: 5.12 parts by weight to produce a mixture of forms bayeritnoy hydroxide and boehmite ratio Al: H 2 O = 1: 5-14 parts by weight, to obtain gamma-alumina ratio of Al: H 2 O = 1: 4.8 parts by weight for aluminum oxide theta ratio Al: H 2 O = 1: 4 7 parts by weight, the ratio of Al to produce alpha-alumina: H 2 O = 1: 5.3 parts by weight
The essence of the apparatus for producing hydroxides or aluminum and hydrogen oxides consists in the fact that it comprises a source of a slurry of finely divided aluminum powder and water with a mixer, reactor, condenser, receiver, an adjustable valve discharge a mixture of water vapor and hydrogen adjustment valve outlet hydroxides or oxides aluminum, the reactor temperature sensor, pressure sensor slurry feed inlet to the reactor outlet gas mixture pressure sensor and the pressure sensor vapor mixture prior to entering the condenser. (The following are features of the device). Furthermore, it comprises an adjustable means for feeding slurry to the reactor and the main controller with an input and output, and a source of the slurry comprises an adjustable water supply means, and adjustable means for supply of aluminum powder, a controller input coupled to a temperature sensor in the reactor and the said pressure sensors and the controller output connected to the source of the slurry, controlled means for supplying the suspension of fine alumina powder with water in a reactor, outlet valve controlled mixture of water vapor and hydrogen discharge valve and variable aluminum hydroxides or oxides.
Furthermore, it is proposed a device in which an adjustable suspension means for supplying fine powdered aluminum in the water contains a high pressure pump and the steering valve.
Furthermore, it is proposed a device in which an adjustable suspension means for supplying fine powdered aluminum in the water comprises an adjustable high-pressure pump.
The controller may be part of an automatic process control system and is connected to the top-level machine interface.
The proposed method and device for its realization are explained by the following figures:
 |
 |
1 is a block diagram of an apparatus, Figure 2 shows a functional diagram of the controller.
 |
The list of accepted designations: 1. adjustable power suspension of fine aluminum powder with water, |
3 shows the top level functional diagram of the machine. |
In a block diagram in Figure 1 shows an apparatus comprising a source of a slurry of fine particulate alumina with water 1, a reactor 8, the receiver (slurry sump) 10, a capacitor 9, an adjustable means for feeding said slurry into the reactor 4, controller 7. Source 1 comprises adjustable suspension means for feeding alumina powder 2 constituting a screw device with adjustable drive; adjustable means for supplying water 3 - Flow regulator company Bronkhorst Hi-Tech BV aluminum powder and water are sent to a mixer 20 - a vessel made of stainless steel and equipped with a stirrer. Source mixture 1 is connected with adjustable means for supplying the slurry to the reactor 4, which comprises a high pressure membrane type pump company URACA valve 5 and N 6 firm Automation. A suspension of aluminum powder and water is fed into the reactor 8, which is a unit operating under high pressure provided with a nozzle that ensures atomization of aluminum powder suspension in water to a droplet diameter of less than 100 microns. The reactor was equipped with an internal temperature sensor 16 mounted on the casing of the reactor temperature sensor 17, the suspension feed inlet connected to a pressure sensor 11, the output vapor-gas mixture is connected a pressure sensor 12. From the top of the reactor a mixture of water vapors and discharged through the hydrogen adjustment valve 14 to the condenser 9 wherein water vapor is separated from the hydrogen. Before entering the condenser fitted with a pressure sensor 13. From the bottom of reactor 15 through an adjustable valve 10 in the collection are displayed hydroxides and aluminum oxides. Adjustable valves 14 and 15 N Automation company. To measure the pressure and temperature sensors Metran company apply. The controller 7 has a control input 18, control output 19 and, in addition, it is connected with a computer (hereinafter - vehicle) of the upper level, not shown in Figure 1.
2 shows a functional diagram of the controller 7. The controller processor module 27 coupled to discrete modules of input signals 23 and analog input module 24 which, in turn, connected to the control input of the controller 18. In addition, the controller processor module 27 is connected with O modules 25 and digital signals analog output modules 26 which, in turn, connected to control the output controller 19. also, the controller processor module 27 is connected via a network adapter 28 and the computer 29 an IDP 22 (see FIG. 2 and 3). The controller 7, for example, the type of CM 1820M KP2.14 128 provides input digital signals of the "dry contact" with the power of these contacts from the internal (12) power supply, the output of 64 discrete signals through normally open relay contacts 10 A, 220 V AC 50 Hz, 64 input analog signal 4 ÷ 20 mA and 4 analog output signal 4 ÷ 20 mA. Entering the digital signals are 4 digital input modules 23 - MDV4.3 (32 channels per module) and 8-Cross modules Digital I / O MKDV / B1.1 (16 channels per module), the output of discrete signals are 2 modules of 25 MDVyv3.4 digital output modules and 4-Cross MKR3.1 relay, I / O, analog signals provided 4 modules 26 MAV1.8 and 4 analog input modules-Cross MKAV2.7. The processor module 27 MP3.1 has a RS232 integrated channel / 485 22 for communication with the machine 22 top level at speeds up to 115,200 bits / sec.
3 shows the top level functional diagram of the machine 22. The processing unit 30 is connected via an IDP 29, the IDP network adapter to the controller 7. Furthermore, the module 30 is connected to the process control software module 31 which, in turn, is connected to the source database 32. base parameters of initial parameter data 32 is connected with the database software editing module input parameters 33.
SALES METHOD
To been actively reacting aluminum metal powder by reaction with water
2Al + 4H 2 O = 3H 2 + 2AlOON (gas) + Q (kcal)
is necessary to ensure fine atomization of the slurry of aluminum powder with water in a reactor in which there are water and its vapor at a temperature of 250-400 ° C and a pressure of 10-20 MPa, the ratio in the slurry fed to the reactor and its water vapor present in the reactor should be 1: 50-100 parts by weight The size of the injected slurry droplets should be less than 100 microns.
In the method in reactor 8 previously supplied with water, its heating is performed to create a saturated vapor to a temperature of 250-400 ° C and a pressure of 10-20 MPa. When these values of the parameters of said cooking source 1 via an adjustable suspension means 4 feed slurry particulate aluminum powder with a predetermined flow rate and the ratio Al and H 2 O is fed to reactor 8.
The resulting products are continuously removed from the reactor. Hydrogen vapor gas composition (about 25 wt.% Hydrogen and about 75 wt.% Water) and hydroxides (oxides) of aluminum in the form of an aqueous slurry (25-35 wt.% Hydroxide (oxide) are removed from the reactor to the separation stage.
Manage the installation process works as follows:
The ACMS 21 values are entered Asked mass flow obtained hydroxide and hydrogen, the ratio of Al and H 2 O in the suspension, which determines the form of hydroxides obtained, the calculated values of pressure and temperature in the reactor. The controller 7 outputs control signals corresponding to the means 2 and 3 feed aluminum powder and distilled water, setting their nominal cost. Depending on the set values of the mass flow rate per unit time obtained by hydroxides and hydrogen are supplied control signals to the adjustable valves 14, 15 mounted on respective highways, defining their orifice, control signals to means for supplying the suspension 4 to the reactor (the pump and the steering valve). The presence of two adjustable elements because the high costs slurry precisely control the pump set 5, a small - adjustable valve 6. In the steady state of aluminum oxidation process in the reactor pressure therein is determined by the sum of the partial pressures of saturated steam and released as a result of the reaction of hydrogen:
for the reactor temperature T p, (indication of the sensor 16) determined from the table values of the quantities of water vapor pressure on the temperature.
The partial pressure of hydrogen determined from the Clapeyron-Mendeleev equation, which is valid under these conditions:
Where 
- Mass of the extracted hydrogen per unit of time,
- molar mass,
R - universal gas constant (8.317 · J / mol · deg)
T r - the temperature in the reactor,
V St. - the free volume of the reactor.
The free volume of the reactor V binding - it is the geometrical proportion of the reactor volume V p, minus the volume that occupies it initially bathed in water (adjusted for expansion at a given temperature) 
and the volume of the suspension of aluminum powder with water received in the reactor prior to the steady state of hydrogen evolution V susp.
After the reaction between aluminum and water with 1 g · mol Al gives 1.5 g · mol H 2, i.e. the complete oxidation of Al give 9 g 1 g H 2.
Then the equation (2) takes the following form:
.
where m Al - aluminum mass entering the reactor per unit time.
Thus, in a steady state
The controller control program made the calculated values: T ass 
, V St.
Thus, pressure regulation in the reactor 8, and hence the amount of hydrogen can be output to produce a change in mass of aluminum reactor feed.
The controller compares the sensor readings with pressure P12 selected optimal value F and, in case of a deviation of these values, produces formula (5) control signals on alumina supply means adjusting the mass fed to the reactor of aluminum.
Temperature sensor at the reactor casing 17 serves to prevent accidents related to the overheating of the reactor.
If necessary, obtain a high purity product using purified water such as distilled, but a method can be used and ordinary water.
| Table The results of experimental studies of the mode of receipt of hydroxides and oxides of aluminum | |||||
| № p / p | Brand aluminum powder | The ratio Al / H 2 O in the slurry | Parameters in the reactor | View received hydroxides and oxides of aluminum | |
| P, MPa | T, ° C | ||||
| 1 | ASD-4 | 1 / 6.5 | 17 | 360 | AlOOH boehmite |
| 2 | ASD-4 | 1/7 | 17 | 340 | AlOOH boehmite |
| 3 | ASD-6 | 1/7 | 17 | 380 | AlOOH boehmite |
| 4 | ASD-6 | 1 / 7.5 | 17 | 360 | AlOOH boehmite |
| 5 | ASD-6 | 1/8 | 18 | 340 | AlOOH boehmite |
| 6 | ASD-4 | 1/9 | 15 | 250 | Al (OH) 3 Bayerite |
| 7 | ASD-4 | 1/10 | 14 | 240 | Al (OH) 3 Bayerite |
| 8 | ASD-6 | 1/11 | 14 | 250 | Al (OH) 3 Bayerite |
| 9 | ASD-4 | 1 / 5.5 | 15 | 450 |
 -Al 2 O 3 oxide, theta |
| 10 | ASD-6 | 1/6 | 15 | 460 |
-Al 2 O 3 oxide, theta |
| eleven | ASD-4 | 1/5 | 20 | 510 |
 -Al 2 O 3, gamma-alumina |
| 12 | ASD-6 | 1/5 | 20 | 550 |
-Al 2 O 3 oxide, gamma |
| 13 | ASD-6 | 1/2 | 25 | 1050 |
 -Al 2 O 3, alpha-alumina |
The resulting method is characterized wastelessness, processability and high productivity, and environmental and safety. Installation established mainly on the basis of commercially available elements, specially made pressure vessel with the necessary input and output highways processed products. In addition, we developed a corresponding matobespechenie AMCS.
CLAIM
1. A method of producing aluminum hydroxides or oxides and hydrogen, comprising forming a suspension of finely divided aluminum powder in water to create a saturated vapor pressure of the reactor, spraying slurry in a pressure reactor, the reactor output mixture of water vapor and hydrogen and hydroxide and output from the reactor aluminum or aluminum oxide to a receiver, the measurement of the temperature T in the reactor, measuring the gas pressure P in the reactor mixture, characterized in that the determined partial pressure of saturated water vapor in the reactor the hydrogen partial pressure is determined Determine the free volume of the reactor V binding, and altering the composition introduced into the mass m Al aluminum slurry in accordance with the formula
where R - universal gas constant,
and produce pressure regulation of the reactor temperature.
2. A method according to claim 1, characterized in that the pressure and temperature control in the reactor is produced by changing the ratio of Al: H 2 O in the slurry and forms for bayeritnoy hydroxide ratio Al: H 2 O = 1: 7-14 wt. hours to obtain boehmite form hydroxide ratio Al:. h 2 O = 1: 5-12 parts by weight, to obtain a mixture bayeritnoy hydroxide and boehmite forms ratio Al: h 2 O = 1: 5-14 parts by weight, for gamma-alumina ratio of Al: H 2 O = 1: 4.8 parts by weight for Al ratio aluminum oxide theta: H 2 O = 1: 7.4 parts by weight for alpha alumina ratio Al: H 2 O = 1: 5.3 parts by weight
3. The apparatus for producing hydroxides or aluminum oxides and hydrogen containing source suspension (1) finely divided aluminum powder and water with a mixer (20), a reactor (8), capacitor (9), the receiver (10), steering valve (14) removing a mixture of water vapor and hydrogen, an adjustable valve (15) removal of hydroxides or oxides of aluminum, temperature sensor (16) of the reactor, a pressure sensor (11) at the input of the slurry in the reactor, a pressure sensor (12) output vapor-gas mixture and a pressure sensor ( 13) prior to entering the gas-vapor mixture in the condenser, characterized in that it comprises an adjustable means (4) for feeding the slurry into the reactor main controller (7) to the input (18) and the outlet (19), the source of the slurry (1) comprises adjustable means a water supply (3) and adjustable means for feeding alumina powder (2), the input (18) of the controller (7) connected to the sensor (16) the reactor temperature and pressure sensors (11, 12, 13) and output (19) of the controller ( 7) connected to the source of the suspension (1), adjustable means (4) for feeding a suspension of finely divided aluminum powder and water to the reactor, regulated valve (14) diverting a mixture of water vapor and hydrogen and regulated valve (15) removal of hydroxides or aluminum oxides.
4. Apparatus according to claim 3, characterized in that the adjustable means (4) for feeding the fine powdery alumina slurry in water contains a high-pressure pump (5) with an adjustable valve (6).
5. Apparatus according to claim 3, characterized in that the adjustable means (4) for feeding the fine powdery alumina slurry in water comprises an adjustable high-pressure pump.
print version
Publication date 01.03.2007gg
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