CN105586463B - A kind of technique being reduced directly pellet using methanol - Google Patents
A kind of technique being reduced directly pellet using methanol Download PDFInfo
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- CN105586463B CN105586463B CN201610166685.6A CN201610166685A CN105586463B CN 105586463 B CN105586463 B CN 105586463B CN 201610166685 A CN201610166685 A CN 201610166685A CN 105586463 B CN105586463 B CN 105586463B
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/0073—Selection or treatment of the reducing gases
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- 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
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Abstract
A kind of technique using Reduction of methanol Pellet Iron Ore stone of the invention, utilize the impedance variations in impedance detection system testing reduction process in situ, heating vaporization is carried out using methanol liquid, it is mixed again with hydrogen, nitrogen, atmosphere reacting furnace mixed gas being passed through at 750 900 DEG C, methanol cracks at high temperature becomes reduction activation gas, carry out the reduction reaction of pellet jointly in conjunction with hydrogen, nitrogen mixed gas, the conducting wire for being connected in pelletizing both ends is connected in electrochemical detection device again, monitors the variation that mixed gas is passed through rear pelletizing impedance in real time.Present invention utilizes impedance test system in situ, can be realized with electro-chemical test system it is good couple, securely and reliably；Use hydrogen generator hydrogen manufacturing for hydrogen source, it is environmental-friendly, it can realize the efficient utilization of the energy.Hydrogen partial is separately replaced using methanol gas, escapable cost is easily operated, simple for process, and gas effciency is high, and practical value in the industrial production is larger.
Description
Technical field
The present invention relates to a kind of Reduction of methanol techniques of Pellet Iron Ore stone, and in particular to methanol is restored with hydrogen gas mixture
The technique of pellet.
Background technology
In recent years, with the rapid development of steel and iron industry, the total energy consumption of steel industry, greenhouse gases and each pollutant
Discharge, iron ore, the increasingly deficient of coke resource are increasingly paid close attention to by various circles of society, and metallurgy industry circular economy hair is accelerated
Exhibition process promotes the development of energy-saving and emission-reduction new theory, new method, new technology, new process, new material and new equipment, has been steel
The trend of the times of industry and inevitable choice.The direct-reduction technique of pellet is modern age refining as a non-blast furnace ironmaking technique
Important technological process in iron technology.Gas base directly reducing iron process is the Main way of current direct-reduction technique, and gas base is straight
It refers to being restored to miberal powder using gas under ore not yet fusion temperature, ferriferous oxide being directly reduced into gold to connect reduction
Belong to the process of iron.Common gas-based reduction gas is：H2, CO etc..
Hydrogen as high-energy fuel, reducibility gas, for the smeltings such as hydrogen-carbon fused reduction iron-smelting, hydrogen reduction blast furnace ironmaking
Golden collar domain, be cleaning, high efficiency extraction metallurgical technology important development direction, not only can fundamentally reduce coke usage amount,
Reduce CO2Discharge, and cast iron product has the advantages that low-carbon, phosphorus, sulfur content, the dynamics in reducing iron oxides and heat transfer
Aspect has apparent advantage.However, hydrogen metallurgical technology is faced with many problems, its development is limited：Hydrogen reduction iron first
Oxide is the endothermic reaction, and hydrogen plays the role of providing reaction heat and reducing agent in the reactor, however hydrogen is as physics
The utilization rate that heat causes Hydrogen Energy is low；In addition, hydrogen reduction ferriferous oxide acquisition lytic activity is big, easily cause material viscous under high temperature
Knot, leads to serious consequence, and cannot be satisfied reduction under low temperature and require；In addition, steel production scale is huge, the source of hydrogen with
And how to solve low energy consumption low cost hydrogen manufacturing and become the metallurgical major issue faced of hydrogen.
The ironmaking flow for being related to carbon reduction is CO in steel production2Primary discharge process, directly and associated emissions account for steel
90% or more of iron industry total release.High CO2Discharge capacity makes " hydrogen is metallurgical " based on hydrogen reduction to be increasingly subject to close extensively
Note.Therefore, low-carbon reduction technique can solve problem above, be smelted iron currently with Hydrogen Energy, and CO is reduced2That discharges is feasible
Property scheme.
Traditional carbon reducing process needs natural gas as reduction air source, and limitation is fairly obvious, and it is necessary to have special
Regional superiority, with no doubt feasible in coal gas principle, but its cost of investment is huge.In addition, coal gas in fluidized-bed reactor
Utilization ratio is relatively low, and it is also uneconomic to make to recycle by pure also Primordial Qi.Therefore, exploitation non-natural gas reduction technique is one
A relative ideal and economic selection, it is that carbon restores industrialized key to develop reduction air source that is economic, cheap, stablizing.
Therefore the present invention sets and is mixed into the methanol gas that part is generated by methanol liquid vaporization in hydrogen gas, methanol is as one
Kind organic alcohols, boiling point is relatively low, is easy to vaporize, and can be cracked to form hydrogen and carbon monoxide etc. at a certain temperature also
Originality gas, one of source that not only can be as hydrogen can also provide part carbon source.The hydrogen reduction for realizing low-carbon, can drop
Low cost.Meanwhile impedance detection system in situ is reapplied in reduction process so that reduction process is realized with electro-chemical test system
Good coupling, in time reflect the impedance variations in reduction process, by the process of the variation control reaction of impedance,
Securely and reliably.
Invention content
An object of the present invention is to provide one kind and being directed to hydrogen reducing pellet, and hydrogen is replaced using part methanol, real
The direct-reduction technique of existing low-carbon reduction can not only reduce cost to solve the deficiency that existing pellet is reduced directly technique, have
There is good economy；The second purpose is that reduction process uses electrochemical in-situ impedance detection, can be by electrochemistry and non-blast furnace
Ironmaking is combined, and can reflect pellet impedance variations in time, and operating procedure is simple, and practical value is big.
The present invention is achieved by the following technical solutions：A kind of technique being reduced directly pellet using methanol, including
Following steps：The technique first vaporizes methanol liquid, then is passed through the nitrogen of certain pressure, and nitrogen takes methanol gas and hydrogen out of
The produced hydrogen of gas generator is mixed according to suitable ratio uniform, then mixed gas is passed through to having warmed up up to reduction temperature
In high temperature process furnances, the reduction reaction under high temperature is carried out with the pellet that processing was transformed, is detected in reduction process every 20min
The impedance variations of pelletizing stop gas supply, wait for that temperature is down to room temperature after pelletizing impedance value stabilization, and obtained reduzate is Fe
Or Fe3C takes the pellet surface layer powder after reduction several, with mortar grinder after screening, takes a certain amount of carry out XRD analysis.
Further, the hydrogen with the ratio of nitrogen methanol mixed gas between 1:9 to 9:Between 1.
The pressure for further providing for nitrogen is 5-13MPa.
Further, the pellet reforming technology is as follows：Pellet to be restored is polished into two planes, and is put down at two
Holes is got on face, quality record is weighed and gets off, screw is screwed into holes, and screw connects two conducting wires and then sets pellet
In in porcelain boat, be put into the alundum tube of tube furnace, porcelain boat pushed away to the center of alundum tube with stove hook, by aluminium oxide stove plug in
Suitable position keeps two conducting wires not contact, and is drawn from one end, is connected to VMP-2 electrochemical workstations.
Further, the technique of the methanol liquid vaporization is：Methanol liquid is heated to by temperature using constant temperature blender with magnetic force
Degree is 67-80 DEG C, methanol liquid vaporization.
Further, the hydrogen is produced using hydrogen generator electrolysis water, and the flow that hydrogen generates is in 10-500ml/min
Between.
Further, institute's reduction temperature is 750-900 DEG C.
Further, the electrochemical test system uses VMP-2 electrochemical workstations, and exchange resistance is carried out with three-electrode system
Anti- test.
It is a further object of the present invention to provide the reduction apparatus of above-mentioned reducing process, which includes：Nitrogen cylinder, No. 1 stream
Gauge, hydrogen generator, No. 2 flowmeters, methyl alcohol vaporizing device, No. 3 flowmeters, Gas mixing valve, No. 4 flowmeters, tube-type atmosphere furnaces
With VMP-2 electrochemical workstations；
Wherein, the hydrogen generator is connected to by No. 2 flowmeters with described Gas mixing valve one end, and the nitrogen cylinder passes through 1
Number flowmeter is connected to one end of the methyl alcohol vaporizing device, and the other end of the methyl alcohol vaporizing device passes through No. 3 flows
Meter is connected to described Gas mixing valve one end, and the other end of the Gas mixing valve is connected by the air inlet of No. 4 flowmeters and tube-type atmosphere furnace
Logical, the VMP-2 electrochemical workstations pass through cable and the tube-type atmosphere furnace data connection.
Further, the methyl alcohol vaporizing device is made of constant temperature blender with magnetic force and sealing container.
The present invention develops a kind of direct-reduction technique using Reduction of methanol pellet, and the technique is first by methanol liquid
Vaporization, then it is passed through the nitrogen of certain pressure, nitrogen takes methanol gas with the produced hydrogen of hydrogen generator according to suitable out of
Ratio uniform mixes, then mixed gas is passed through to having warmed up up in 750-900 DEG C of high temperature process furnances, is transformed with processing
Pellet carries out the reduction reaction under high temperature, and the recovery time is then fixed on pellet both sides according to the quality control of pellet
Conducting wire is connected with electrochemical workstation, and then realizes the impedance variations of in situ detection pellet.
Advantage of the present invention：
The advantage of the invention is that with hydrogen generator hydrogen manufacturing, the renewable energies such as nuclear power, water power, wind-force and underground heat can be used
Source converts electric energy hydrogen manufacturing；Hydrogen partial can be replaced with methanol, reduce hydrogen use ratio during hydrogen reducing pellet, realize
Low-carbon restores；It can realize in situ detection, realize the variation of the impedance of monitoring reduction in time.
The present invention is using the CO and H for cracking generation after methyl alcohol vaporizing at high temperature2It is simple for process as reducibility gas,
Invest, consume it is less.Meanwhile needed for being replenished in time by adding quantity of methyl alcohol by the way of methanol liquid heating vaporization
Reducibility gas, process is convenient simple, it can be achieved that thoroughly reduction.
Description of the drawings
Fig. 1 is a kind of technique being reduced directly pellet using methanol of the present invention, and is applied to when reduction
Impedance detection system schematic in situ.
Fig. 2 is the wiring diagram of pellet transformation processing.
Fig. 3 is that pellet leads to impedance value and change curve after hydrogen, methanol.
Fig. 4 is that pellet leads to the XRD curves after hydrogen reduction.
Fig. 5 is that pellet leads to the XRD curves after hydrogen, Reduction of methanol.
Fig. 6 is a kind of direct-reduction process flow chart using Reduction of methanol pellet of the invention.
In figure:1, nitrogen cylinder；2, No. 1 flowmeter；3, hydrogen generator；4, No. 2 flowmeters；5, methyl alcohol vaporizing device；6、3
Number flowmeter；7, Gas mixing valve；8, No. 4 flowmeters；9, tube-type atmosphere furnace；10, electrochemical workstation；11, screw；12 pellets.
Specific implementation mode
In order to be better understood by present disclosure, feature, advantage, below in conjunction with attached drawing and example to present invention process into
Row detailed description, particular content are as follows：
Embodiment 1：
Combined with Figure 1 and Figure 2, the present embodiment it is a kind of using methanol be reduced directly pellet process system by nitrogen cylinder 1,
7, No. 4 No. 1 flowmeter 2,3, No. 2 flowmeters 4 of hydrogen generator, 5, No. 3 flowmeters 6 of methyl alcohol vaporizing device, Gas mixing valve flowmeters
8, the compositions such as tube-type atmosphere furnace 9 and impedance detection system.
Pellet is polished into two planes, and gets holes on two planar, quality is weighed and is denoted as 3.659g, two
Screw is screwed into hole, screw connects two conducting wires.Then, pellet is placed in porcelain boat, is put into the alundum tube of tube furnace, use stove
Hook pushes away porcelain boat to the center of alundum tube, and aluminium oxide stove is plugged in suitable position, keeps two conducting wires not contact, draws from one end
Go out, is connected to VMP-2 electrochemical workstations.When tube furnace heating is reached predetermined temperature, its impedance value is detected.Then QL is opened
Hydrogen generator, nitrogen cylinder pressure reducing valve are passed through hydrogen and nitrogen, control hydrogen, nitrogen ratios 1:9, using VMP-2 electrochemistry
Work station detects the impedance variations of pelletizing in reduction process every 20min, and after pelletizing impedance value stabilization, controlled atmosphere furnace is in hydrogen
Natural cooling under gas, nitrogen atmosphere waits for that temperature is down to room temperature, and it is 3.409g to take out pellet and weigh, and negates the pellet after answering
Surface layer powder is several, with mortar grinder after screening, takes a certain amount of carry out XRD analysis.
Schematically patent of the present invention and embodiments thereof are described above, description is not limiting, attached drawing
Shown in also be patent of the present invention one of embodiment, actual structure is not limited to this.So if this field
Those of ordinary skill indicated by it, in the case of not departing from patent of the present invention and creating objective, not inventively design
Frame mode similar with the technical solution and embodiment, should all belong to the protection domain of patent of the present invention.
Embodiment 2：
Combined with Figure 1 and Figure 2, the present embodiment it is a kind of using methanol be reduced directly pellet process system by nitrogen cylinder 1,
7, No. 4 No. 1 flowmeter 2,3, No. 2 flowmeters 4 of hydrogen generator, 5, No. 3 flowmeters 6 of methyl alcohol vaporizing device, Gas mixing valve flowmeters
8, the compositions such as tube-type atmosphere furnace 9 and impedance detection system.
Pellet is polished into two planes and is punched, and gets holes on two planar, quality is weighed and is denoted as
3.796g, is screwed into screw in holes, and screw connects two conducting wires.Then, pellet is placed in porcelain boat, is put into the rigid of tube furnace
In beautiful pipe, porcelain boat is pushed away to the center of alundum tube with stove hook, aluminium oxide stove is plugged in suitable position, two conducting wires is kept not connect
It touches, is drawn from one end, be connected to VMP-2 electrochemical workstations.When tube furnace heating is reached predetermined temperature, its impedance is detected
Value.Then QL hydrogen generators, nitrogen cylinder pressure reducing valve are opened, hydrogen and nitrogen, control hydrogen, nitrogen ratios 1 are passed through:9, and
And the constant temperature blender with magnetic force device for making methyl alcohol vaporizing is opened, the liquid methanol amount in sealing container that controls is 80ml, vaporization temperature
Degree is 67 DEG C, detects the impedance variations of pelletizing in reduction process every 20min using VMP-2 electrochemical workstations, waits for that pelletizing hinders
After anti-value stabilization, controlled atmosphere furnace natural cooling under hydrogen, nitrogen atmosphere waits for that temperature is down to room temperature, takes out pellet and weighs
For 3.426g, it is several to negate the pellet surface layer powder after answering, and with mortar grinder after screening, takes a certain amount of carry out XRD analysis.
Schematically patent of the present invention and embodiments thereof are described above, description is not limiting, attached drawing
Shown in also be patent of the present invention one of embodiment, actual structure is not limited to this.So if this field
Those of ordinary skill indicated by it, in the case of not departing from patent of the present invention and creating objective, not inventively design
Frame mode similar with the technical solution and embodiment, should all belong to the protection domain of patent of the present invention.
Embodiment 3：
Combined with Figure 1 and Figure 2, the present embodiment it is a kind of using methanol be reduced directly pellet process system by nitrogen cylinder 1,
7, No. 4 No. 1 flowmeter 2,3, No. 2 flowmeters 4 of hydrogen generator, 5, No. 3 flowmeters 6 of methyl alcohol vaporizing device, Gas mixing valve flowmeters
8, the compositions such as tube-type atmosphere furnace 9 and impedance detection system.
Pellet is polished into two planes and is punched, and gets holes on two planar, quality is weighed and is denoted as
3.574g, is screwed into screw in holes, and screw connects two conducting wires.Then, pellet is placed in porcelain boat, is put into the rigid of tube furnace
In beautiful pipe, porcelain boat is pushed away to the center of alundum tube with stove hook, aluminium oxide stove is plugged in suitable position, two conducting wires is kept not connect
It touches, is drawn from one end, be connected to VMP-2 electrochemical workstations.When tube furnace heating is reached predetermined temperature, its impedance is detected
Value.Then QL hydrogen generators, nitrogen cylinder pressure reducing valve are opened, hydrogen and nitrogen, control hydrogen, nitrogen ratios 1 are passed through:9, and
And the constant temperature blender with magnetic force device for making methyl alcohol vaporizing is opened, the liquid methanol amount in sealing container that controls is 80ml, vaporization temperature
Degree is 67 DEG C, detects the impedance variations of pelletizing in reduction process every 20min using VMP-2 electrochemical workstations, waits for that pelletizing hinders
After anti-value stabilization, controlled atmosphere furnace natural cooling under hydrogen, nitrogen atmosphere waits for that temperature is down to room temperature, takes out pellet and weighs
For 3.256g, it is several to negate the pellet surface layer powder after answering, and with mortar grinder after screening, takes a certain amount of carry out XRD analysis.
Schematically patent of the present invention and embodiments thereof are described above, description is not limiting, attached drawing
Shown in also be patent of the present invention one of embodiment, actual structure is not limited to this.So if this field
Those of ordinary skill indicated by it, in the case of not departing from patent of the present invention and creating objective, not inventively design
Frame mode similar with the technical solution and embodiment, should all belong to the protection domain of patent of the present invention.
XRD analysis the result shows that, reduzate be Fe and Fe3C, when single-pass hydrogen reducing, reduzate Fe leads to hydrogen
Product after being restored with methanol mixed gas is Fe and Fe3C.Through material phase analysis, in the product of embodiment 2, Fe3C accounts for 73%, and
Fe accounts for 27%.
Table 1 is the variation that pellet leads to the impedance value after hydrogen, methanol under different flow, as follows：
Table 1.
Claims (6)
1. a kind of technique being reduced directly pellet using methanol, which is characterized in that include the following steps：The technique is first by first
Alcohol liquid vaporizes, then is passed through the nitrogen of 5-13Mpa, and nitrogen takes methanol gas with the produced hydrogen of hydrogen generator according to 1 out of:
9 to 9:Between 1 ratio uniform mixing, hydrogen generate flow between 10-500ml/min, then by mixed gas be passed through to
It has warmed up and reaches in the high temperature process furnances that reduction temperature is 750-900 DEG C, carried out under high temperature with the pellet that processing was transformed
Reduction reaction detects the impedance variations of pelletizing in reduction process every 20min, after pelletizing impedance value stabilization, stops gas supply, waits for
Temperature is down to room temperature, and obtained reduzate is Fe and Fe3C takes the pellet surface layer powder after reduction several, uses mortar grinder
After screening, a certain amount of carry out XRD analysis is taken.
2. technique according to claim 1, which is characterized in that the pellet reforming technology is as follows：By pelletizing to be restored
Mine polish two planes, and gets holes on two planar, weighs quality record and gets off, and screw, spiral shell are screwed into holes
Then pellet is placed in porcelain boat by nail two conducting wires of connection, be put into the alundum tube of tube furnace, porcelain boat is pushed away to corundum with stove hook
Aluminium oxide stove is plugged in suitable position, two conducting wires is kept not contact, drawn from one end, be connected to VMP-2 by the center of pipe
Electrochemical workstation.
3. technique according to claim 1, which is characterized in that the technique of methanol liquid vaporization is：Using constant temperature magnetic
It is 67-80 DEG C that methanol liquid is heated to temperature by power blender, methanol liquid vaporization.
4. technique according to claim 1, it is characterised in that：Electrochemical test system uses VMP-2 electrochemical workstations,
Ac impedance measurement is carried out with three-electrode system.
5. a kind of reduction apparatus of technique as described in claim 1-4 any one, which is characterized in that the device includes：Nitrogen
Gas cylinder（1）, No. 1 flowmeter（2）, hydrogen generator（3）, No. 2 flowmeters（4）, methyl alcohol vaporizing device（5）, No. 3 flowmeters（6）、
Gas mixing valve（7）, No. 4 flowmeters（8）, tube-type atmosphere furnace（9）With VMP-2 electrochemical workstations（10 ）；
Wherein, the hydrogen generator（3）Pass through No. 2 flowmeters（4）With the Gas mixing valve（7）One end is connected to, the nitrogen cylinder
（1）Pass through No. 1 flowmeter（2）With the methyl alcohol vaporizing device（5）One end connection, the methyl alcohol vaporizing device（5）It is another
End passes through No. 3 flowmeters（6）With the Gas mixing valve（7）One end is connected to, the Gas mixing valve（7）The other end pass through No. 4 stream
Gauge（8）With tube-type atmosphere furnace（9）Air inlet connection, the VMP-2 electrochemical workstations（10 ）Pass through cable and the pipe
Formula atmosphere furnace（9）Data connection.
6. device according to claim 5, which is characterized in that the methyl alcohol vaporizing device（5）By constant temperature blender with magnetic force
It is formed with sealing container.
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| CN106521074B (en) * | 2017-01-13 | 2018-03-30 | 刘冬冬 | A kind of equipment and technique that DRI is produced using methanol decomposition |
| CN107082428B (en) * | 2017-04-28 | 2019-03-26 | 苏州大学 | A method of cementite is prepared using more metal sulfate slags |
| CN107737943B (en) * | 2017-11-03 | 2019-08-02 | 重庆大学 | A kind of method that Reduction of methanol prepares tungsten carbide or/and tungsten powder |
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| US5221369A (en) * | 1991-07-08 | 1993-06-22 | Air Products And Chemicals, Inc. | In-situ generation of heat treating atmospheres using non-cryogenically produced nitrogen |
| US5259893A (en) * | 1991-07-08 | 1993-11-09 | Air Products And Chemicals, Inc. | In-situ generation of heat treating atmospheres using a mixture of non-cryogenically produced nitrogen and a hydrocarbon gas |
| JP2948771B2 (en) * | 1997-02-28 | 1999-09-13 | 川崎重工業株式会社 | Manufacturing method of iron carbide |
| CN101538627B (en) * | 2009-03-27 | 2010-09-08 | 中国科学技术大学 | Method for preparing direct reduced iron by bio-oil |
| CN102605133A (en) * | 2012-01-13 | 2012-07-25 | 中冶赛迪工程技术股份有限公司 | Direct reduction method for producing sponge iron by aid of coke oven gas |
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