WO2007008115A1 - Procede et dispositif de fabrication d'hydroxydes ou d'oxydes d'aluminium et d'hydrogene - Google Patents

Procede et dispositif de fabrication d'hydroxydes ou d'oxydes d'aluminium et d'hydrogene Download PDF

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Publication number
WO2007008115A1
WO2007008115A1 PCT/RU2006/000353 RU2006000353W WO2007008115A1 WO 2007008115 A1 WO2007008115 A1 WO 2007008115A1 RU 2006000353 W RU2006000353 W RU 2006000353W WO 2007008115 A1 WO2007008115 A1 WO 2007008115A1
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WO
WIPO (PCT)
Prior art keywords
reactor
water
suspension
aluminum
hydrogen
Prior art date
Application number
PCT/RU2006/000353
Other languages
English (en)
Russian (ru)
Other versions
WO2007008115A8 (fr
Inventor
Aleksandr Valentinovich Bersh
Juriy Leonidovich Ivanov
Juriy Aleksandrovich Mazalov
Anton Viktorovich Glukhov
Original Assignee
Aleksandr Valentinovich Bersh
Juriy Leonidovich Ivanov
Juriy Aleksandrovich Mazalov
Anton Viktorovich Glukhov
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Aleksandr Valentinovich Bersh, Juriy Leonidovich Ivanov, Juriy Aleksandrovich Mazalov, Anton Viktorovich Glukhov filed Critical Aleksandr Valentinovich Bersh
Publication of WO2007008115A1 publication Critical patent/WO2007008115A1/fr
Publication of WO2007008115A8 publication Critical patent/WO2007008115A8/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
    • C01B3/10—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents by reaction of water vapour with metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/42—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
    • C01F7/428—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation by oxidation in an aqueous solution
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Definitions

  • the invention relates to methods for producing aluminum hydroxides or oxides, and in particular to methods for producing aluminum oxides or hydroxides from aluminum metal by oxidation in an aqueous medium.
  • Aluminum oxides and hydroxides are used in various industries as adsorbents, catalysts, etc.
  • High purity hydroxides and oxides of aluminum are used in the electronic and optical industries in the form of a fine powder - as abrasive powders, in particular, for hard drives or magnetic heads.
  • the invention relates, in particular, to methods for producing aluminum hydroxides of boehmite and bayerite form.
  • the method also relates to the production of hydrogen, namely, to methods for producing hydrogen by the chemical interaction of metals and water.
  • Hydrogen can be used in various chemical processes as a reducing agent, as well as in certain conditions as a fuel.
  • Aluminum hydroxides exist in various crystalline forms - hydrargillite, bayerite, diaspora, boehmite, etc., oxides - in the form of alpha, gamma ; theta forms. The main difference between these forms is the location of aluminum ions and oxygen ions relative to each other.
  • aluminum hydroxide also means hydrated aluminum oxides Al 2 Oz.
  • Aluminum hydroxide or aluminum oxide is fed to a hydroxide receiver.
  • the forms of aluminum hydroxides necessary for each specific case are obtained: boehmite, bayerite, as well as alpha-oxide, theta-oxide, gamma-aluminum oxide and a mixture of aluminum hydroxides boehmite and bayerite form.
  • the implementation of the method takes place in an installation including a mixer, a high pressure reactor equipped with a nozzle that provides a spray of a suspension of powdered aluminum in water with a droplet diameter of not more than 100 ⁇ m, a receiving device for hydroxides, a condenser.
  • Distilled water is used to produce high purity hydrogen.
  • the method has a number of advantages: it is continuous, only water and aluminum take part in the reactions, which ensures the purity of the products obtained (hydroxides and oxides of aluminum, as well as hydrogen), changes in temperature and pressure conditions determine the type of products obtained.
  • the necessary pressure and temperature ranges in the reactor with this method are supported by the continuous removal of steam and gas and a suspension of aluminum hydroxide.
  • This support is a serious technical problem, since the ratio between the pressure, temperature, and mass of vented gas and a suspension of aluminum hydroxide is determined by a rather complex formula that takes into account the partial pressures of saturated water vapor and hydrogen, the mass of introduced aluminum, the temperature in the reactor, and the free volume of the reactor.
  • the dynamic change of these factors makes it insufficient as a regulatory factor only to divert the reaction products from the reactor, and it does not provide the necessary accuracy of maintaining the regimes in
  • the aim of the proposed method is to provide the necessary process parameters for guaranteed receipt of output products of specified types and purity.
  • Such technical problems as increasing the reliability of the reactor and its stability are being solved.
  • the essence of the proposed method is to obtain hydroxides or oxides of aluminum and hydrogen from a suspension of finely divided aluminum powder in water, including preparing a suspension of finely divided aluminum powder in water, creating saturated water vapor pressure in the reactor, spraying the suspension into a high pressure reactor, and withdrawing a mixture of water vapor from the reactor and hydrogen, as well as the output from the reactor of aluminum hydroxide or aluminum oxide to the receiving device, measuring the temperature T in the reactor, measuring yes P Lenia gas mixture in the reactor. (The following are the distinguishing features of the method).
  • the partial pressure of saturated water vapor PH 2 O is determined.
  • the partial pressure of hydrogen ⁇ is determined, and the
  • R is the universal gas constant (8.317-j / moltrad)
  • the essence of the proposed device for producing hydroxides or oxides of aluminum and hydrogen is that it contains a source of suspension of fine powdered aluminum with water with a mixer, a reactor, a condenser, a receiving device, an adjustable valve to remove a mixture of water vapor and hydrogen, an adjustable valve to remove hydroxides or oxides aluminum, a temperature sensor in the reactor, a pressure sensor at the inlet of the slurry supply to the reactor, a pressure sensor at the outlet of the gas-vapor mixture, and a pressure sensor in front of the steam inlet call mixture into the capacitor.
  • the proposed device contains an adjustable means of supplying a suspension to the reactor and a control controller with input and output, the source of the suspension containing an adjustable means of supplying water and an adjustable means of supplying aluminum powder, the input of the controller is connected to a temperature sensor in the reactor and the indicated pressure sensors, and the controller output is connected to a suspension source controlled by a means for supplying a suspension of finely divided aluminum powder with water into the reactor OP, an adjustable valve for discharging a mixture of water vapor and hydrogen and an adjustable valve for removing hydroxides or aluminum oxides.
  • an adjustable means for supplying a suspension of finely divided aluminum powder in water comprises a high pressure pump and an adjustable valve.
  • an adjustable means for supplying a suspension of finely divided aluminum powder in water comprises an adjustable high pressure pump.
  • the controller can be part of an automatic process control and management system and is connected to the top-level machine by an interface.
  • FIG. 1 shows a block diagram of a device.
  • FIG. 2 shows a functional diagram of the controller.
  • FIG. 3 shows a functional diagram of a top-level machine.
  • processor module MVU
  • FIG. 1 shows an installation comprising a source of a suspension of finely divided aluminum powder with water 1, a reactor 8, a receiver (suspension settler) 10, a condenser 9, an adjustable means for supplying the specified suspension to the reactor 4, a control controller 7.
  • the source of the suspension 1 contains an adjustable means for feeding aluminum powder 2, which is a screw device with an adjustable drive; adjustable means of water supply 3 - a flow regulator of the company ⁇ rkhophorst Hi-Tech BV, Aluminum powder and water are sent to the mixer 20 - a vessel made of stainless steel and equipped with a mixing device.
  • Source mixture 1 is connected with adjustable means ⁇ slurry feed to reactor 4, which comprises a high pressure membrane type pump company URACA 5 and valve 6 firm LH Automation.
  • reactor 4 comprises a high pressure membrane type pump company URACA 5 and valve 6 firm LH Automation.
  • the suspension of aluminum powder with water is fed into the reactor 8, which is a high-pressure apparatus equipped with a nozzle that atomizes a suspension of powdered aluminum in water to a droplet diameter of not more than 100 ⁇ m.
  • the reactor is equipped with an internal temperature sensor 16, a temperature sensor 17 is installed on the reactor shell, a pressure sensor 11 is connected at the inlet of the suspension supply, a pressure sensor 12 is connected at the outlet of the gas-vapor mixture 12.
  • the mixture of water and hydrogen vapors is discharged through an adjustable valve 14 to the condenser 9 where the separation of water vapor from hydrogen takes place.
  • a pressure sensor 13 is installed in front of the condenser entrance. Hydroxides and aluminum oxides are discharged from the lower part of the reactor through an adjustable valve 15 to the collection 10. Adjustable valves 14, 15 manufactured by LG Automation. Metran sensors are used to measure pressures and temperatures. Controller 7
  • SUBSTITUTE SHEET (RULE 26) has a control input 18 and a control output 19, in addition, it is connected to a upper level computer (hereinafter referred to as a machine), in FIG. 1 not shown.
  • FIG. 2 shows a functional diagram of controller 7.
  • the processor module of controller 27 is connected to input modules of discrete signals 23 and input modules of analog signals 24, which, in turn, are connected to the control input of controller 18.
  • the processor module of controller 27 is connected to output modules of discrete signals 25 and output modules of analog signals 26, which, in turn, are connected to the control output of the controller 19.
  • the processor module of the controller 27 is connected via network adapters 28 and 29 to the computer M WU 22 (see. Fig. 2 and 3).
  • Controller 7 for example, type CM 1820M KP2.14 provides the input of 128 discrete signals of the “contact contact” type with the power of these contacts from an internal (12 V) power source, the output of 64 discrete signals via normally open relay contacts 10 A, 220 V AC 50 Hz, input of 64 analog 4 ⁇ 20 mA signals and 4 analog output signals 4 ⁇ 20 mA.
  • Discrete signals are inputted by 4 discrete input modules 23 - MDB4.3 (32 channels per module) and 8 MKDB / B1.1 discrete I / O cross modules (16 channels per module), discrete signals are output by 2 modules 25 discrete output MDByw.4 and 4 modules cross relay MKRZ.l, input / output of analog signals is provided by 4 modules 26 MABl.8 and 4 modules cross analog input MKAB2.7.
  • the processor module 27 MPZ.l has an integrated channel RS232 / 485 22 to provide communication with the machine 22 of the upper level at speeds up to 115200 bps.
  • FIG. 3 shows a functional diagram of the machine of the upper level 22.
  • the processor module 30 of the MVU is connected via the network adapter 29 of the MVU to the controller 7.
  • the module 30 is connected to the software module for process control 31, which, in turn, is connected to the database of initial parameters 32.
  • the source data database 32 is also connected to the software module for editing the source parameters database 33.
  • SUBSTITUTE SHEET (RULE 26) it is necessary to provide fine atomization of a suspension of aluminum powder with water into a reactor in which water and its vapors are present at a temperature of 250 - 400 C and a pressure of 10 - 20 MPa, and the ratio of the suspension fed to the reactor to water and its vapors in the reactor should be 1 : 50-100 parts by weight In this case, the size of the droplets of the injected suspension should be no more than 100 microns.
  • water is preliminarily supplied to reactor 8, it is heated to create saturated water vapor to a temperature of 250 - 400 C and a pressure of 10 - 20 MPa.
  • an adjustable feeding means 4 the suspension of finely dispersed aluminum powder with a given ⁇ -consumption and the ratio of Al and H 2 O is fed into the reactor 8.
  • Hydrogen in the composition of combined-cycle gas about 25 wt.% Hydrogen and about 75 wt.% Water
  • aluminum hydroxides (oxides) in the form of an aqueous suspension 25-35 wt.% Hydroxides (oxides) are removed from the reactor to the separation stage.
  • ASKU 21 introduces the set mass flow rates of the obtained hydroxides and hydrogen, the ratio of Al and H 2 O in the suspension, which determines the type of hydroxides produced, and the calculated values of pressure and temperature in the reactor.
  • the controller 7 provides the appropriate control signals to the means 2 and 3 of the supply of aluminum powder and distilled water, setting their nominal costs.
  • control signals are supplied to the adjustable valves 14, 15 installed on the corresponding lines, determining their cross-section, control signals to the means for supplying the suspension 4 to the reactor (pump and adjustable valve).
  • Mendeleev which is true in these conditions: m n is the mass of hydrogen released per unit time, ⁇ Hi is the molar mass,
  • R is the universal gas constant (8.317-J / moltrad)
  • T 1 is the temperature in the reactor
  • V a ⁇ is the free volume of the reactor.
  • the free volume of the reactor V m is a part of the geometric volume of the reactor Vp, minus the volume that the water initially filled in (adjusted for expansion at a given temperature) V 11 o ⁇ r and the volume of suspension of aluminum powder with water that entered the reactor before stationary mode of hydrogen evolution V cya ⁇
  • V cll V p - V th0ITr - V cyc ⁇ (3)
  • equation (2) takes the following form:
  • m Al is the mass of aluminum entering the reactor per unit time.
  • the controller compares the readings of the pressure sensor P 12 with the selected optimal value of P and, in the case of deviation of these values, generates control signals for the aluminum feed means according to formula (5), adjusting the mass of aluminum supplied to the reactor.
  • the temperature sensor on the reactor shell 17 serves to prevent accidents associated with overheating of the reactor.
  • purified water is used, for example, distilled, but the method also allows the use of ordinary water.
  • the resulting method is characterized by non-waste, manufacturability and high productivity, as well as environmental safety.
  • the installation was created mainly on the basis of commercially available elements; the reactor vessel with the necessary input and output lines of the processed products was specially manufactured.
  • the corresponding software for automated control systems was developed.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

L'invention concerne un procédé et un dispositif de fabrication d'hydroxydes ou d'oxydes d'aluminium à partir d'aluminium métallique par oxydation dans un milieu aqueux, notamment de production d'hydroxydes d'aluminium de forme boehmite ou bayerite. De plus, l'invention concerne un procédé de fabrication d'hydrogène par l'interaction d'eau et d'aluminium. A la différence des procédés connus, le procédé proposé prévoit l'utilisation d'eau et d'aluminium uniquement, la réaction entre lesquels s'écoule dans des proportions prédéterminées d'une suspension de poudre d'aluminium finement dispersée et d'eau, alimentée dans le réacteur, le réglage de fonctionnement du réacteur s'effectuant par la modification de la quantité de suspension de poudre d'aluminium dans d'eau, alimentée par unité de temps, ou par celle de la quantité de poudre d'aluminium introduite dans la suspension par unité de temps dans les limites prédéterminées, le rapport entre l'alumine et l'eau dans la suspension déterminant la forme de l'hydroxyde ou d'oxyde d'aluminium obtenu à la sortie. Pour assurer le régime prédéterminé de déroulement de l'opération et obtenir le produit sous la forme désirée, on utilise un système de gestion automatisé sur la base d'un contrôleur de type SM 1820M KP2.14.
PCT/RU2006/000353 2005-07-11 2006-07-06 Procede et dispositif de fabrication d'hydroxydes ou d'oxydes d'aluminium et d'hydrogene WO2007008115A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2005121562/15A RU2278077C1 (ru) 2005-07-11 2005-07-11 Способ получения гидроксидов или оксидов алюминия и водорода и устройство для его осуществления
RU2005121562 2005-07-11

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WO2007008115A1 true WO2007008115A1 (fr) 2007-01-18
WO2007008115A8 WO2007008115A8 (fr) 2007-08-16

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103494918A (zh) * 2013-10-11 2014-01-08 哈尔滨欧替药业有限公司 参芪温阳阴道膨胀栓及其制备方法和检测方法
CN104291268A (zh) * 2014-05-26 2015-01-21 上海东科凯乔能源科技有限公司 一种用湿化学法制备产氢材料改性铝粉体的方法
CN104787794A (zh) * 2015-03-26 2015-07-22 昆明理工大学 一种制备高纯氧化铝的自吸式水解反应装置及应用
CN112624167A (zh) * 2020-12-21 2021-04-09 中氢能源科技发展(内蒙古)有限公司 一种拟薄水铝石的制备方法
WO2023178430A1 (fr) * 2022-03-22 2023-09-28 Gh Power Inc. Système à réacteur à hydrogène pour la production en continu d'hydrogène et d'alumine avec régulation et commande de pression et de température

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2519450C1 (ru) * 2012-12-11 2014-06-10 Федеральное государственное бюджетное учреждение науки Объединенный институт высоких температур Российской академии наук (ОИВТ РАН) Способ получения корунда высокой чистоты
RU173853U1 (ru) * 2016-10-28 2017-09-14 Общество с ограниченной ответственностью "Технологии алюмоэнергетики" (ООО "Технологии алюмоэнергетики") Установка для получения оксидов алюминия высокой чистоты

Citations (4)

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US4543246A (en) * 1984-10-04 1985-09-24 Houser Clifford F Hydrogen generator
SU1623946A1 (ru) * 1986-05-13 1991-01-30 С А Юрченко А С Можин и Р Ф.Прозпрова Установка дл получени водорода
US20030118505A1 (en) * 2000-07-20 2003-06-26 Andersen Erling Reidar Energy production method and apparatus
RU2223221C1 (ru) * 2003-02-11 2004-02-10 Закрытое акционерное общество "Фирма Риком СПб" Способ получения гидроксидов или оксидов алюминия и водорода

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4543246A (en) * 1984-10-04 1985-09-24 Houser Clifford F Hydrogen generator
SU1623946A1 (ru) * 1986-05-13 1991-01-30 С А Юрченко А С Можин и Р Ф.Прозпрова Установка дл получени водорода
US20030118505A1 (en) * 2000-07-20 2003-06-26 Andersen Erling Reidar Energy production method and apparatus
RU2223221C1 (ru) * 2003-02-11 2004-02-10 Закрытое акционерное общество "Фирма Риком СПб" Способ получения гидроксидов или оксидов алюминия и водорода

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103494918A (zh) * 2013-10-11 2014-01-08 哈尔滨欧替药业有限公司 参芪温阳阴道膨胀栓及其制备方法和检测方法
CN104291268A (zh) * 2014-05-26 2015-01-21 上海东科凯乔能源科技有限公司 一种用湿化学法制备产氢材料改性铝粉体的方法
CN104787794A (zh) * 2015-03-26 2015-07-22 昆明理工大学 一种制备高纯氧化铝的自吸式水解反应装置及应用
CN112624167A (zh) * 2020-12-21 2021-04-09 中氢能源科技发展(内蒙古)有限公司 一种拟薄水铝石的制备方法
CN112624167B (zh) * 2020-12-21 2023-02-21 中氢能源科技发展(内蒙古)有限公司 一种拟薄水铝石的制备方法
WO2023178430A1 (fr) * 2022-03-22 2023-09-28 Gh Power Inc. Système à réacteur à hydrogène pour la production en continu d'hydrogène et d'alumine avec régulation et commande de pression et de température

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WO2007008115A8 (fr) 2007-08-16

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