CN107758614B - Method and equipment for producing hydrogen by solar energy thermochemical decomposition of water - Google Patents

Method and equipment for producing hydrogen by solar energy thermochemical decomposition of water Download PDF

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CN107758614B
CN107758614B CN201610687450.1A CN201610687450A CN107758614B CN 107758614 B CN107758614 B CN 107758614B CN 201610687450 A CN201610687450 A CN 201610687450A CN 107758614 B CN107758614 B CN 107758614B
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CN107758614A (en
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高为鑫
桂宝桃
王彬
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Jiangsu Tianyi Micro Metal Powder Co Ltd
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    • 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
    • C01B3/12—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 carbon monoxide
    • C01B3/14—Handling of heat and steam
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/06—Ferric oxide [Fe2O3]
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/08—Ferroso-ferric oxide [Fe3O4]
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    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/133—Renewable energy sources, e.g. sunlight

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Abstract

The invention relates to a method and equipment for producing hydrogen by utilizing solar energy to perform thermochemical decomposition on water. The invention takes a solar energy light-gathering heat collector as a heat source and takes water, Carbonyl (CO) or carbonyl metal complex as raw materials; water and CO or one or more carbonyl metal complexes are put into a solar vacuum high-temperature heat absorption tube (tank), the solar vacuum high-temperature heat absorption tube (tank) absorbs the solar energy gathered by the solar concentrating collector, the temperature rises to the critical temperature of the water, and the pressure also rises to the critical pressure of the water along with the temperature rise. The water in critical state is subjected to reduction reaction with CO or carbonyl metal complex in a solar vacuum high-temperature heat absorption tube (tank) to prepare hydrogen, metal or oxide micro-nano particles thereof, carbon dioxide or carbonic acid compounds (calcium carbonate, sodium carbonate, ammonium bicarbonate and the like). Is a low-cost solar hydrogen production poly-generation technology and equipment.

Description

Method and equipment for producing hydrogen by solar energy thermochemical decomposition of water
Technical Field
The invention relates to a method and equipment for producing hydrogen by utilizing solar energy to thermochemically decompose water, belonging to the field of new energy. Specifically, the invention relates to a poly-generation technology and equipment for preparing hydrogen, metal or oxide micro-nano particles thereof and carbon dioxide by heating water to a critical state by using a solar concentrating collector and carrying out reduction reaction on critical water and Carbonyl (CO) or carbonyl metal complex.
Background
With the development of human society, the practical role and strategic importance of energy sources are self-evident. The search for continuous and rich clean energy is the foundation of human society survival and development. Even if the greenhouse effect caused by the emission of carbon dioxide is not considered, the limited and non-renewable properties of fossil energy are enough to force human beings to search for alternative energy sources. The sustainable energy of the earth is solar energy, the most abundant water is stored, and a new alternative energy is searched, so that the solar energy is researched and developed from the two aspects, has the widest prospect and is sustainable and clean in the true sense.
The hydrogen production by utilizing the solar light thermochemical cycle to decompose the water is a good combination of the hydrogen energy production by utilizing the solar light heat.
There are many reported thermochemical hydrogen production methods, and there are several types in the following representative and classical meanings.
The Ispra research institute in Italy at the beginning of the 70 th century proposed a Mark 1 cycle, the reaction process of which is as follows:
（1）CaBr2(s)+2H2O(g)
Figure DEST_PATH_IMAGE001
Ca(OH)2+2HBr(g)
（2）Hg(i)+2HBr(g)
Figure DEST_PATH_IMAGE002
HgBr2(s)+H2(g)
（3）HgBr2+Ca(OH)2(s)
Figure DEST_PATH_IMAGE003
CaBr2+HgO(s)+H2O(g)
（4）HgO(s)
Figure DEST_PATH_IMAGE004
Hg(g)+1/2O2
the hydrogen production efficiency of the cyclic reaction reaches 40-60%, and is generally 50%.
In 1976, DeYonkov, Hetsukamur research institute of Sumitomo Seisakuwa, Japan, proposed a practical two-stage cycle.
Fe2O3+H2O+2SO2
Figure DEST_PATH_IMAGE005
2FeSO4+H2
2FeSO4
Figure DEST_PATH_IMAGE006
Fe2O3+2SO2+1/2O2
The secondary circulation is characterized by less unit operation, is the simplest circulation and therefore has lower cost, and researchers develop three-stage, four-stage or even multi-stage circulation reaction systems in order to reduce reaction temperature and search for reaction systems with higher energy conversion efficiency. In thermochemical hydrogen production, different chemical reactions have different compounds, such as compounds of sulfur, bismuth, calcium, bromine, mercury, iron, iodine, magnesium, copper, chlorine, nickel, potassium, lithium, etc., as intermediate reactants, and the reaction temperature is typically eight nine hundred degrees celsius, which is high by only a few thousand degrees celsius. After the reaction is finished, the amount of chemicals is not reduced, the chemicals can be recycled, only water is consumed, and the water is decomposed into hydrogen and oxygen.
UT-1, UT-2 and UT-3 cyclic reactions are proposed in the Guishan Xiuxiong of the university of Tokyo, Japan, wherein the UT-3 reaction is a solid-gas four-stage cyclic reaction, and the process is as follows:
（1） CaBr2(s)+H2O(g)
Figure DEST_PATH_IMAGE007
CaO(s)+2HBr(g)
（2）CaO(s)+Br2(g)
Figure DEST_PATH_IMAGE008
CaBr2(s)+12O2(g)
（3）Fe3O4(s)+8HBr(s)
Figure DEST_PATH_IMAGE009
3FeBr2(s)+4H2O(g)+Br2(g)
（4）3FeBr2+4H2O(g)
Figure DEST_PATH_IMAGE010
Fe3O4(s)+6HBr(g)+H2(g)
the hydrogen production efficiency of the circular reaction is more than or equal to 40 percent.
The U.S. chemists proposed sulfur-iodine thermochemical cycle, copper chloride cycle, lithium iodide cycle, and sulfidation cycle reactions. The reaction process of the thermochemical cycle reaction of sulfur-iodine is as follows:
（1） 2HI(g)
Figure DEST_PATH_IMAGE011
H2(g)+I2(g)
（2） SO2(g)+2H2O(l)+I2(g)
Figure DEST_PATH_IMAGE012
H2SO4(aq)+2HI(aq)
（3） H2SO4(l)
Figure DEST_PATH_IMAGE013
SO2(g)+1/2O2(g)+H2O(g)
the reaction process of the copper chloride circulation reaction is as follows:
（1） 2Cu(s)+2HCl(l)
Figure DEST_PATH_IMAGE014
2CuCl(s)+H2(g)
（2）4CuCl
Figure DEST_PATH_IMAGE015
2CuCl2(s)+2Cu(s)
（3）2CuCl2(s)
Figure DEST_PATH_IMAGE016
2CuCl(s)+Cl2(g)
（4）Cl2(g)+Mg(OH)2(s)
Figure DEST_PATH_IMAGE017
MgCl2(aq)+H2O(g)+12O2(g)
（5）MgCl2(aq)+2H2O(g)
Figure DEST_PATH_IMAGE018
Mg(OH)2(s)+2HCl(g)
the hydrogen production efficiency of this cyclic reaction was 55%.
The iodine lithium cycle reaction process is as follows:
（1）3I2(l)+6LiOH(aq)
Figure DEST_PATH_IMAGE019
5LiI(s)+LiIO3(s)+3H2O(g)
（2）LiIO3(aq)+KI(aq)
Figure DEST_PATH_IMAGE020
KIO3(aq)+LiI(aq)
（3）KIO3(s)
Figure DEST_PATH_IMAGE021
KI(aq)+3/2O2(g)
（4）6LiI(l)+6H2(g)
Figure DEST_PATH_IMAGE022
6HI(g)+6LiOH(l)
（5）6HI+3Ni(s)
Figure DEST_PATH_IMAGE023
3NiI2(aq)+3H2(g)
（6）3NiI2(s)
Figure DEST_PATH_IMAGE024
Ni(s)+3I2(g)
the hydrogen production efficiency of this cyclic reaction was 64%.
The vulcanization cycle (or Mark 2) reaction process is as follows:
（1）2H2O(l)+SO2(g)
Figure DEST_PATH_IMAGE025
H2SO4(aq)+H2(g) (Electrolysis 0.17V)
（2）H2SO4(aq)
Figure DEST_PATH_IMAGE026
H2O(g)+SO2+12O2(g)
The hydrogen production efficiency of the circular reaction reaches 40-50%.
More rapid thermochemical cycle technologies have been developed in recent years, spanning the step of hydrogen and oxygen separation. The specific process is that, in the first step, a high-temperature heat source is utilized to decompose metal oxide into a metal simple substance and oxygen; the second step is that the metal simple substance reacts with high-temperature steam to generate metal oxide and hydrogen. The oxides reported in the literature that can be used in this thermochemical cycle are ZnO, FeO, TiO, CoO, etc. For example, the thermochemical cycle constructed by the ZnO/Zn redox reaction can solve the explosion problem possibly generated by the contact of hydrogen and oxygen of a high-temperature heat source. The reaction process is as follows.
ZnO(s)
Figure DEST_PATH_IMAGE027
Zn(g)+1/2O2
Zn(l)+H2O
Figure DEST_PATH_IMAGE028
ZnO(s)+H2
The first step is an endothermic reaction, at 2300K, solid ZnO(s) decomposes into Zn (g) and O2(ii) a The second step is an exothermic reaction, in which Zn reacts with water at 700K to produce hydrogen and ZnO in solid form. The solid ZnO separated in the second step is recycled in the first step, and oxygen and hydrogen are respectively obtained in the reaction process, so that the step of separating gas at high temperature is avoided. The utility model 200320127837.X designs a hydrogen production device aiming at the thermochemical cycle formed by ZnO reduction reported by foreign documents.
The hydrogen production method has high reaction temperature and low hydrogen yield.
Disclosure of Invention
The invention aims to provide a method and equipment for producing hydrogen by solar photo-thermal chemical decomposition of water, which have the advantages of low reaction temperature, easily obtained and cheap raw materials, simple process and high hydrogen yield and can simultaneously co-produce micro-nano particles of metal or oxide thereof and high-purity carbon dioxide or carbonic acid compounds.
The invention is realized by the following method:
according to the volume of the solar vacuum high-temperature heat absorption reactor, the pressure in a vacuum high-temperature heat absorption pipe or container at 374.3 ℃ is more than 20.5Mpa (the temperature and the pressure are critical conditions of water) and less than 30 Mpa; adding water (the adding amount of the water can be slightly higher than a calculated value in order to ensure that the reaction is sufficient) and Carbonyl (CO) or a carbonyl metal complex into a solar vacuum high-temperature endothermic reactor according to a reaction proportion, sealing the vacuum high-temperature endothermic reactor, and heating the water and the CO or the carbonyl metal complex in the vacuum high-temperature endothermic reactor to the critical temperature (374.3 ℃, namely 647.3K) of the water by using a solar focusing heat collector, wherein the pressure in the vacuum high-temperature endothermic reactor is more than 20.5MPa, the water is in a critical state, and the CO reacts with oxygen in the critical water; or the carbonyl metal complex is completely decomposed at the temperature, and carbon monoxide and metal atoms which are decomposed are reduced to critical water to generate hydrogen, micro-nano particles of metal or oxide thereof and carbon dioxide.
Chemical reaction equation using CO as the reducing agent: CO + H2O——CO2+H2；
Chemical equation using iron pentacarbonyl as the reducing agent:
2Fe（CO）5＋13H2O——Fe2O3+10CO2+13H2- (1) or
3Fe（CO）5＋19H2O——Fe3O4+15CO2+19H2————（2）。
The solar focusing heat collector used by the invention can be a trough type solar focusing heat collector, a tower type solar focusing heat collector or a dish type solar focusing heat collector.
The solar vacuum high-temperature endothermic reactor used in the invention can be a tubular or a pot high-pressure container, and the form of the reactor is matched with the selected solar focusing heat collector; the material for manufacturing the vacuum high-temperature endothermic reactor can be carbon steel or stainless steel, and is selected according to the requirements of the manufacturing specifications of the high-pressure vessel.
The Carbonyl (CO) used as the reducing agent in the invention can be CO in industrial exhaust gas; the metal carbonyl complex may be one or a combination of two or more kinds of metal carbonyl complexes such as iron pentacarbonyl, nickel tetracarbonyl, tungsten hexacarbonyl, chromium hexacarbonyl, molybdenum hexacarbonyl, dicobalt octacarbonyl, dimanganese decacarbonyl, and the like. Iron pentacarbonyl and nickel tetracarbonyl are preferred, and iron pentacarbonyl is more preferred.
Different reducing agents are selected, the reaction proportion of the reducing agents and water is different, and the obtained micro-nano particles of the metal or the oxide thereof are also different. Such as:
selecting iron pentacarbonyl as a reducing agent, and collecting ferric oxide or ferric oxide micro-nano particles, hydrogen and carbon dioxide;
selecting nickel tetracarbonyl as a reducing agent, and collecting metal nickel micro-nano particles, hydrogen and carbon dioxide;
depending on whether or under what conditions the metal atom contained in the metal carbonyl complex is easily oxidized.
The invention has the advantages that:
the process is clean and environment-friendly, no energy consumption is caused, and the output is free from emission;
the reaction is simple, the hydrogen production and reaction conditions are relatively mild, the temperature is low, and the method is easy to realize;
the weather adaptability is strong, and the heating can be accumulated in each reaction period until the reaction condition is obtained;
the hydrogen yield is high, and the actual test shows that the hydrogen yield reaches more than 90 percent;
the reaction product is easy to separate, and the products of the reaction of CO and critical water are only hydrogen and carbon dioxide, so that the separation is very easy (see the following description); in the reaction product of the carbonyl metal complex and the critical water, the solid phase is metal or oxide micro-nano particles thereof, the gas phase is hydrogen and carbon dioxide, and the solid-gas separation is very easy; the gas phase hydrogen and carbon dioxide are safely mixed together, and the hydrogen and the carbon dioxide can be easily separated by using a physical method (a pressure swing adsorption method or a cryogenic method) or a chemical method to obtain pure hydrogen and carbon dioxide or carbonic acid compounds (calcium carbonate, sodium carbonate, ammonium bicarbonate and the like).
Low raw material cost, multiple output and good economic benefit. CO in the industrial waste gas is used as a reducing agent, and flare combustion is changed into waste utilization, so that the method is environment-friendly; taking cheap pentacarbonyl iron as a reducing agent as an example, only one output of the micro-nano ferric oxide or ferroferric oxide can sufficiently make up for all expenses.
Drawings
FIG. 1 is a schematic diagram of an apparatus for producing hydrogen by solar thermochemical decomposition of water, which is composed of a tubular solar vacuum high-temperature endothermic reactor and a trough solar focusing collector. In the drawings
1 is a trough type solar focusing mirror;
2 is a tubular solar vacuum high-temperature endothermic reactor.
FIG. 2 is a device for producing hydrogen by solar energy photo-thermal chemical decomposition of water, which consists of a tank-type solar vacuum high-temperature endothermic reactor and a dish-type solar focusing heat collector. In the drawings
1 is a dish type solar focusing mirror;
2 is a pot-type solar vacuum high-temperature endothermic reactor.
FIG. 3 is a device for producing hydrogen by solar energy photo-thermal chemical decomposition of water, which consists of a tank type solar vacuum high-temperature endothermic reactor and a tower type solar focusing heat collector. In the drawings
1 is a solar focusing mirror;
2 is a pot-type solar vacuum high-temperature endothermic reaction tower.
Examples
1. 20mol of water is added into a 4000ml tank type solar vacuum high-temperature endothermic reactor, 20mol of carbon monoxide is compressed into the tank type solar vacuum high-temperature endothermic reactor, a dish type solar focusing heat collector is utilized to heat the vacuum high-temperature endothermic reactor to 380 ℃, and the pressure of the vacuum high-temperature endothermic reactor is 26 Mpa. At this point the reaction is complete.
And (3) removing or closing the solar focusing heat collector, discharging a reaction product in the solar vacuum high-temperature endothermic reactor into another closed vacuum container, and cooling and separating to obtain 19.6mol of hydrogen and 19.7gmol of carbon dioxide.
2. 320g of iron pentacarbonyl and 200g of water are added into a vacuum high-temperature heat absorption pipe with the volume of 2600ml, and the vacuum high-temperature heat absorption reactor is heated to 380 ℃ by using a trough type solar focusing heat collector, wherein the pressure of the vacuum high-temperature heat absorption pipe is 24 Mpa. At this point the reaction is complete.
And (3) removing or closing the solar focusing heat collector, discharging a reaction product in the solar vacuum high-temperature endothermic reactor into another closed vacuum container, and cooling, settling and separating to obtain 21g (about 233L) of hydrogen, 369g (about 187L) of carbon dioxide gas and 126g of ferroferric oxide with the average particle size of 3.6 microns.

Claims (4)

1. A method for producing hydrogen by utilizing solar energy to perform thermochemical decomposition on water is characterized in that a solar energy light-gathering heat collector is used as a heat source, and water and a carbonyl metal complex are used as raw materials; water and one or more carbonyl metal complexes are added into a solar vacuum high-temperature heat absorption device, the solar vacuum high-temperature heat absorption device absorbs solar energy gathered by a solar light-gathering heat collector, the temperature rises to the critical temperature of the water, the pressure also rises to the critical pressure of the water along with the temperature rise, the critical water and the carbonyl metal complexes are subjected to reduction reaction in the solar vacuum high-temperature heat absorption device, and hydrogen, metal or oxide micro-nano particles thereof, carbon dioxide or carbonic acid compounds are prepared.
2. The method for producing hydrogen by solar thermochemical decomposition of water according to claim 1, wherein the solar concentrator collector comprises a trough solar collector, a tower solar collector, a dish solar collector, or a combination thereof.
3. The method for producing hydrogen by solar thermochemical decomposition of water according to claim 1, wherein said solar vacuum high temperature heat sink is a tubular or can high pressure vessel, the form of which is adapted to the selected solar thermal collector; the material for manufacturing the solar vacuum high-temperature heat absorbing device is carbon steel or stainless steel and is selected according to the requirements of the manufacturing specifications of the high-pressure container.
4. The method of claim 1, wherein the metal carbonyl complex is selected from one or more of iron pentacarbonyl and its derivatives, nickel tetracarbonyl, tungsten hexacarbonyl, chromium hexacarbonyl, molybdenum hexacarbonyl, cobaltosic octacarbonyl, and dimanganese decacarbonyl.
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