CN101538627B - Method for preparing direct reduced iron by bio-oil - Google Patents
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Abstract
The invention relates to a method for preparing a direct reduced iron by a gas base method, in particular to a technology for preparing the direct reduced iron by taking the bio-oil and iron ore powders as raw materials. The method comprises the following steps of firstly sending the bio-oil and water vapor into a water vapor reforming reactor, converting the carbon-hydrogen-oxygen-contained organic matter in the bio-oil into a mixed gas with principle components of hydrogen and carbon dioxide, obtaining a reduced gas with the hydrogen concentration of more than 90vol% by a tail gas purifying and collecting system, subsequently preheating the reduced gas to the temperature of 100-200 DEG C and sending the preheated gas into a reduction reactor containing the iron ore powders, starting a self-heating system and controlling the temperature in the reduction reactor within 650-900 DEG C and keeping the temperature for 1-2h so that the reduced gas and the ferric oxide in the iron ore generate an oxidation-reduction reaction to obtain the direct reduced iron. The method is characterized in that a coke or a natural gas is not needed and the reproducible bio-oil raw material is used and the method has the advantages of being friendly to environment, simple and quick process, low energy consumption, high metallization rate and high production cost.
Description
Technical field
The present invention relates to utilize the method for gas base legal system direct-reduced iron, being specifically related to bio oil and iron ore is the technology that raw material is produced direct-reduced iron.
Background technology
At present, the main smelting process of Iron and Steel Production comprises two kinds: the direct-reduced iron technology of blast furnace technology and use Sweet natural gas or coal, wherein blast furnace ironmaking is a main technique methods in the present Iron and Steel Production, account for 90% of Iron and Steel Production output greatly, it uses high-quality iron ore, coke and slag making solvent to be raw material, iron-smelting process is made up of coking, sintering, blast furnace operation, and the energy that is consumed accounts for more than 30% of Iron and Steel Production total energy consumption.And traditional Iron And Steel Industry is serious source of pollution.Another kind method is to use the direct-reduced iron technology of Sweet natural gas, accounts for 10% of Iron and Steel Production output greatly, and this technology is reducing gas (H with the Sweet natural gas high temperature shift earlier
2+ CO), utilize reducing gas that the iron ore raw material is reduced into direct-reduced iron again, utilizing electric furnace smelting method at last is high-quality product made from steel with direct-reduced iron production.
Direct-reduced iron claims sponge iron again, mainly as the raw material of electric furnace process refining high-quality steel and special steel, also can be used for direct production electrical pure iron, ferrite and industrial iron charge.Utilize the MIDREX method of Sweet natural gas to research and develop successfully since nineteen sixty-eight, direct-reduced iron is just developed rapidly, has adopted the short flow process iron and steel enterprise output of direct-reduction process since 1975, with 12.3% speed increment every year on average.According to the statistic data of U.S. Mead rex company, world's direct-reduced iron output increased 12.4% on year-on-year basis in 2007, reached 6,722 ten thousand tons.Direct-reduced iron develops odjective cause rapidly and comprises (1) world majority state famine coking coal, but there are high-quality abundant iron ore and natural gas source in wherein many countries, can put suitablely by the production of national resource development direct-reduced iron because of ground; (2) along with the development of electric furnace flow production line, electric steel output is growing, and continuous casting ratio increases rapidly in world's system steel production in recent years, and the self-produced high-quality steel scrap of Steel Complex reduces, the steel scrap quantity not sufficient comprises the developing country of China owing to certainly will develop direct-reduced iron; Developed country's coating steel consumption increases day by day, and makes to remove that detrimental impurity is anxious in returning increases, and must adopt to mix 30%～50% direct-reduced iron and dilute; (3) Iron And Steel Industry is subjected to the competition of macromolecular material and silicate material over past ten years, is that the fast development of the small-sized special steel plant of characteristic has promoted the direct-reduced iron demand with quality, performance and many kinds.
Present existing production direct-reduced iron technical point gas base method and coal-based method two classes.Can be divided into shaft furnace process, kiln process, rotary hearth furnace method, retort process making sponge iron, pot type oven process and fluidized bed process etc. by main equipment.At present, the direct-reduced iron more than 90% is to be that the gas base method of raw material is produced in order to Sweet natural gas in the world, but its turnout is subjected to the restriction in natural gas supply, price and zone.It is also ripe relatively technically to make reductive agent with coal, but requires high and some restriction such as technological deficiency that are difficult to overcome of starting material condition, causes direct-reduced iron production not developed rapidly in the whole world.The coal-based direct reduction iron work industrial scale of having gone into operation at present is all little, and major part all is to handle iron-containing waste.
As seen, mainly there are two problems in present existing production direct-reduced iron technology: making iron oxide reduction in (1) prior art is that the raw material and the fuel of metallic iron is coke or Sweet natural gas, this class raw material is non-renewable fossil feedstock, supplied easily, the restriction in price and zone, exist simultaneously and how to reduce obnoxious flavour (CO, NOx, SO
2) and greenhouse gases (CO
2) emission problem; (2) hydrogen-rich synthetic gas that needs the higher hydrogen carbon ratio in the direct-reduced iron technology is as reducing gas, but no matter is the synthetic gas that coal gas vaporization or gas renormalizing obtain, and wherein CO all occupies significant proportion.Obtain containing H
2The reducing gas of 90% above purity must be carried out the water vapour conversion of CO again, and the CO that must be obtained by the CO conversion
2Absorb and remove, so energy drops into height.
Bio oil is to comprise the C/H/O liquid organic mixture by what the reaction of the fast pyrolysis of biomass obtained, biomass are meant that all derive from the regenerated material of animal and plant energy in the organism, mainly comprise agricultural crop straw, agriculture and forestry product residual processing waste, fastgrowing trees, firewood forests, algae, excrement of animals, domestic refuse and organic industrial sewage etc.About 1,460 hundred million tons of annual in the world yield of biomass.China's biomass resource is also very abundant, and every year, only agricultural crop straw and agricultural-food husk etc. just had more than 1,000,000,000 ton, and many regional on-site incineration stalks not only waste energy, but also causes serious environmental to be polluted.Therefore bring into play the potentiality of biomass resource, optimization has great significance to national resources.
Liquid bio oil has easily collecting, the easily storage and the advantage of easily transportation aspect; Compare with the biomass direct gasification, bio oil easily obtains the hydrogen-rich synthetic gas of higher hydrogen carbon ratio by the water vapor catalytic reforming.In the prior art, the bio oil technology has obtained Preliminary Applications.For example, reported among the ZL 200710134707.1 that to be raw material with the bio oil prepare the method for hydrogen by the electrocatalysis water vapour recapitalization method, obtained containing the hydrogen of hydrogen concentration greater than 90vol%.Bio oil also can directly be burnt and is used for generating and heat supply (Michael
Angew.Chem.Int.Ed.2008,47,2-14).Behind bio oil process catalytic pyrolysis or the shortening, fuel quality is improved in addition, and the bio oil after the refining can be mixed with ordinary diesel oil by a certain percentage, as fuel (S.Czenrnik, A.V.Bridgwater, the Energy ﹠amp of diesel engine; Fuels 2004,18,590-598).Although cost is higher at present, bio oil is succeedd aspect power fuel experiments such as engine, turbine; " energy and fuel " the 21st phase in 2007 " biological oil properties and the application in Fischer-Tropsch is synthetic " (ZhaoxiangWang et al., Energy; Fuels 2007,21,2421-2432) in play-by-play use biological oil reforming synthetic gas as raw material, be used for the achievement in research of fischer-tropsch reaction synthin compound.But generally speaking, the application of at present relevant bio oil still is in development.
Up to now, find no the report that bio oil is applied to the reduced iron technical elements.Therefore, explore that to utilize aboundresources, environmental friendliness, reproducible bio oil be very significant for raw material system direct-reduced iron technology.
Goal of the invention
The objective of the invention is to, at deficiency of the prior art, providing a kind of is the method for feedstock production direct-reduced iron with bio oil and iron ore, thereby reduces the energy input, helps environment protection.
Summary of the invention
Purpose of the present invention is achieved through the following technical solutions.
The method of utilizing bio oil and iron ore for the feedstock production direct-reduced iron of the present invention, at first bio oil and water vapor are sent in the electrocatalysis water vapour recapitalization reactor that is filled with reforming catalyst, carrying out electrocatalysis water vapour recapitalization reaction and water gas shift reaction after the two mixing, the heating fast, is that main component is the gas mixture of hydrogen and carbonic acid gas with the carbon containing in the bio oil-hydrogen-oxygen organic matter transformation; It is characterized in that (1) is with reacted mixed gas process condenser, CO then
2It is reducing gas more than the 90vol% that chemical absorption device, moisture eliminator obtain to contain hydrogen concentration in interior tail gas purification gathering system; (2) reducing gas is preheated to 100-200 ℃; (3) reducing gas after will preheating is sent in the reduction reactor that is filled with iron ore, start simultaneously this reduction reactor from heating system, the interior temperature of control reduction reactor is in 650 ℃-900 ℃ and be incubated 1-2 hour, make the ferric oxide generation redox reaction in reducing gas and the iron ore obtain direct-reduced iron, wherein, the input flow rate of described reducing gas is 100-200ml/min, and the particle diameter of iron ore is 0.1mm-1mm, preferably 0.1-0.2mm.
In preparation process, ferric oxide generation redox reaction obtains the main chemical reactions of direct-reduced iron and is in described reducing gas and the iron ore: Fe
xO
y+ yH
2→ xFe+yH
2O, Fe
xO
y+ yCO → xFe+yCO
2
Bio oil raw material of the present invention is to carry out the carbon containing hydrogen-oxygen organic compound that fast pyrolysis produces, i.e. biomass cracked oil by using by various reproducible biomass (as rice husk, stalk, wood chip etc.) under anaerobic and medium temperature condition.
Iron ore of the present invention is by a kind of or mixed type iron ore powder in the various rhombohedral iron ore that contain ferric oxide, limonite, the magnetite.
The method of producing direct-reduced iron provided by the invention; the reducing gas that uses is abundant with storage, environmental friendliness, reproducible bio oil are raw material; realized the recycle of the sustainability of resource-environmental integration; not only help environment protection; compare and use non-renewable fossil resource such as coking coal and Sweet natural gas in the traditional method, also have the advantage cheap, that capacity usage ratio is high as starting material.CO content is low in the reducing gas that bio oil is produced, and need not to carry out the CO conversion again, and whole technological process is easy to operate, degree of metalization is high.Described bio oil is to comprise the C/H/O liquid organic mixture by what the reaction of the fast pyrolysis of biomass obtained, and contained carbon comes from Atmospheric Carbon Dioxide, after burning is used again the form with carbonic acid gas turn back to atmosphere, realize carbon dioxide zero discharge; The obnoxious flavour that is discharged is (as SO
2) only be equivalent to use about 1/10 of fossil feedstock, help environment protection.
According to measuring and calculating, the cost that utilizes the present invention to make direct-reduced iron is approximately 1180 yuan/ton, and the coal-based direct reduction iron international price is 318 dollars/ton at present, and Renminbi is approximately 2200 yuan/ton; And 381 dollars/ton of gas base directly reducing iron prices, Renminbi is approximately 2671 yuan/ton; Substitute products such as steel scrap price are 390-395 dollar/ton, and Renminbi is approximately 2730 yuan of/ton steel scraps.Compare with fat coal system direct-reduced iron with using Sweet natural gas,, therefore can save the about 25-30% of cost, have bigger comprehensive utilization potentiality because the bio oil prices of raw and semifnished materials that the present invention uses are lower and capacity usage ratio is high.
Description of drawings
Fig. 1 is that the bio oil that obtains with the quick cracking of wood chip and hematite powder are the XRD analysis spectrogram of the direct-reduced iron that makes of raw material.
Fig. 2 is that the bio oil that obtains with the quick cracking of rice husk and limonite powder are the XRD analysis spectrogram of the direct-reduced iron that makes of raw material.
Embodiment
Below by specific embodiment the present invention is described further.
Embodiment 1
Bio oil and hematite powder that present embodiment is investigated to be obtained by the quick cracking of wood chip are prepared using method system direct-reduced iron of the present invention effect.
The reaction unit that uses the electrocatalysis water vapour recapitalization biological oil hydrogen-manufacturing reactor conduct in the prior art (ZL 200710134707.1) to prepare by bio oil.Prepare the method for synthetic gas of reducing by bio oil: at first the commercial Ni series catalysts of routine is reduced in 500 ℃ of following hydrogen atmospheres be filled in after one hour around the built-in electric stove wire and with electric stove wire surface uniform contact, catalyst levels is by per hour bio oil inlet amount decision, catalyst levels is 5.5g in the present embodiment, connect preheating zone heat tape power supply then, the temperature that makes the preheating zone is at 180-200 ℃; Connection is used for the power supply of the Ni-Cr electric stove wire of internal heating, makes the electric current that feeds the Ni-Cr electric stove wire be fixed on 3.0A, by the power of conditioned reaction device externally heated oven, the temperature in the reforming reactor inner chamber is regulated in 500-550 ℃ of scope.Open the liquid sampling pump on the bio oil raw material storage tanks outlet pipe and the valve of steam generator at last, regulate the flow of bio oil and water vapor, the bio oil steam after preheating and the mixed gas of water vapor, bio oil scission reaction, the reaction of bio oil electrocatalysis water vapour recapitalization and water-gas reaction take place in the reforming reactor inner chamber, and the mixed gas that obtains main component and be hydrogen and carbonic acid gas carries out tail gas purification aftertreatment again.In the present embodiment, raw materials used bio oil for obtaining by the quick cracking of wood chip, when the reforming reaction temperature at 550 ℃, electric current is 3A, the water vapour flow is 50g/h, the bio oil flow is 18g/h, corresponding mol ratio is 7 o'clock, hydrogen yield and bio oil transformation efficiency are respectively 96.8% and 97.1%, after cooling off, comprise hydrogen (70.5vol%) in the mixed gas, carbonic acid gas (25.1vol%), carbon monoxide (3.7vol%) and methane (0.1vol%), eliminate carbonic acid gas in the gas mixture with conventional chemical absorption process (20%NaOH solution), obtain the higher-grade reduction synthetic gas of hydrogeneous 92.6vol% and carbon monoxide 4.8vol%.
Adopt the reaction unit of flow reactor of fixed bed as iron ore reduction: it comprises tubular fixed-bed reactor that have thermal insulation layer, and the reduction synthetic gas feeding pipeline and the reaction end gas output channel that are connected both ends.The method for preparing direct-reduced iron by the bio oil reducing gas: at first iron ore is pulverized for particle diameter be to be filled in the flow reactor of fixed bed heating zone behind the 0.1-0.2mm powder, the iron ore addition is determined by reduction reaction device heating zone size, the iron ore consumption is 20g in the present embodiment, the reduction synthetic gas is preheating to and is passed into after 120 ℃ in the flow reactor of fixed bed that is filled with iron ore, and reduction synthetic gas total flux is 120ml/min; The working pressure of described flow reactor of fixed bed is 1atm, utilize indirect heating stove heating flow reactor of fixed bed simultaneously, insulation makes the ferric oxide generation redox reaction in reducing gas and the iron ore obtain direct-reduced iron when the temperature in this reactor inner chamber reaches 650-850 ℃.For guaranteeing the experiment accuracy, present embodiment stops heating after making the temperature in the reactor inner chamber be incubated 1h respectively in the time of 650 ℃, 750 ℃, 850 ℃, takes out gained direct-reduced iron product after cooling and analyzes comparison.The detected result of different reduction reaction temperatures sees Table 2.Adopting total iron content in the present embodiment is 54.69% rhombohedral iron ore stone powder, and main component sees Table 1 in this iron ore raw material.The result shows: when reduction reaction temperature is 850 ℃, the reduction reaction time, degree of metalization reached 94.7% in the direct-reduced iron product when being 1h.Described total iron comprises simple substance Fe, divalence Fe and trivalent Fe, and total iron content is represented with TFe (Total Fe content) usually; Described metallic iron is simple substance Fe, and metal Ferrum content is represented degree of metalization with MFe (MetalFe content) expression with MFe/TFe usually.
In order further to analyze the composition and the structure of iron ore raw material and direct-reduced iron product, at room temperature utilize XRD (X-ray Diffraction) method respectively raw material in the foregoing description 1 and product to be carried out the crystal phase structure analysis, testing sample all grinds and is 200-300 order powder, XRD measures on Philips X ' Pert PRO SUPER type commentaries on classics target X-ray diffractometer and carries out, source of radiation is Cu-K α, λ=1.5418
, sweep angle 2 θ=10 °-90 °, scanning step is 0.017 °, tube current 100mA, range 2000 (CPS).Detected result as shown in Figure 1, among the figure, I: rhombohedral iron ore raw material; II: the direct-reduced iron product (reductive condition: 650 ℃, 1h); III: the direct-reduced iron product (reductive condition: 850 ℃, 1h).Find out by figure, when reduction reaction temperature is 850 ℃, the reduction reaction time, the ferric oxide in the XRD analysis proof rhombohedral iron ore stone raw material almost completely was reduced to metallic iron when being 1h.
Main component and content in the used iron ore raw material of table 1
Table 2 is a raw material system direct-reduced iron effect with bio oil and the hematite powder that the quick cracking of wood chip obtains
(data are the mean value of three experiments in the table)
Embodiment 2:
It is prepared using method system direct-reduced iron of the present invention effect that present embodiment is mainly investigated with bio oil that is obtained by the quick cracking of rice husk and limonite powder.
In the present embodiment, reaction unit and method by the reaction unit of bio oil system reduction synthetic gas and iron ore reduction are all identical with embodiment 1, the different bio oil and the limonite powder that are to use the quick cracking of rice husk to obtain are raw material system direct-reduced iron, when the biological oil reforming temperature of reaction at 548 ℃, electric current is 2.9A, the water vapour flow is 50g/h, the bio oil flow is 18g/h, the mol ratio of water vapour and bio oil correspondence is 7 o'clock, hydrogen yield and bio oil transformation efficiency are respectively 93.5% and 95.1%, comprise hydrogen (69.3vol%) in the mixed gas of cooling back, carbonic acid gas (24.8vol%), carbon monoxide (5.1vol%) and methane (0.2vol%), eliminate carbonic acid gas in the mixed gas with conventional chemical absorption process (20%NaOH solution), obtain to contain the higher-grade reducing gas of 91.4vol% hydrogen and 6.5vol% carbon monoxide.In the present embodiment, the employing iron-holder is 51.76% limonite ore powder (consumption: 20g, particle diameter: 0.1-0.2mm) with biological oil reforming reducing gas (hydrogen richness: 91.4vol%, carbon monoxide content: 6.5vol%, total flux: in the time of 150ml/min), send in the flow reactor of fixed bed after the biological oil reforming reducing gas preheated 180 ℃, the working pressure of described reactor is 1atm, and the detected result that changes reduction reaction temperature is as shown in table 3.The result shows: when reduction reaction temperature is 850 ℃, the reduction reaction time, degree of metalization reached 93.1% in the direct-reduced iron product when being 1h.The XRD of limonite raw material and direct-reduced iron product (XRD testing tool and condition all with embodiment 1 in identical) detected result as shown in Figure 2, wherein, I: limonite raw material; II: the direct-reduced iron product (reductive condition: 650 ℃, 1h); III: the direct-reduced iron product (reductive condition: 850 ℃, 1h).When reduction reaction temperature is 850 ℃, the reduction reaction time, the ferric oxide in the limonite raw material almost completely was reduced to metallic iron when being 1h.
Table 3 is a raw material system direct-reduced iron effect with bio oil and the limonite powder that the quick cracking of rice husk obtains
(data are the mean value of three experiments in the table)
Embodiment 3:
It is prepared using method system direct-reduced iron of the present invention effect that present embodiment is mainly investigated with bio oil that is obtained by the quick cracking of wood chip and magnetite powder.
In the present embodiment, reaction unit and method by the reaction unit of bio oil system reduction synthetic gas and iron ore reduction are all identical with embodiment 1, when the biological oil reforming temperature of reaction at 555 ℃, electric current is 3.1A, the water vapour flow is 50g/h, the bio oil flow is 18g/h, the mol ratio of water vapour and bio oil correspondence is 7 o'clock, hydrogen yield and bio oil transformation efficiency are respectively 97.2% and 98.9%, comprise hydrogen (70.8vol%) in the mixed gas of cooling back, carbonic acid gas (25.5vol%), carbon monoxide (3.5vol%) and methane (0.1vol%), eliminate carbonic acid gas in the mixed gas with conventional chemical absorption process (20%NaOH solution), acquisition contains the higher-grade reducing gas of 93.1vol% hydrogen and 4.5vol% carbon monoxide, and the total flux of reduction synthetic gas is 180ml/min.In the present embodiment, adopting iron-holder is that 53.69% magnetic iron ore powder diameter is two kinds of 0.1-0.2mm and 0.8-1.0mm; Every group of consumption is 20g, sends in the flow reactor of fixed bed after the biological oil reforming reducing gas is preheated 200 ℃, and the working pressure of described reactor is 1atm, changes the detected result such as the table 4 of reduction reaction temperature.In the table, the magnetic iron ore powder diameter that uses in the sequence number 1,2,3 is 0.1-0.2mm; The magnetic iron ore powder diameter that uses in the sequence number 4 is 0.8-1.0mm.The result shows: when reduction reaction temperature is that 850 ℃, reduction reaction time are 1h, when the magnetic iron ore powder diameter was 0.1-0.2mm, direct-reduced iron resultant metal rate reached 96.0%.When the magnetic iron ore powder diameter is 0.8-1.0mm, reduction reaction temperature is that 850 ℃, reduction reaction time are when being 2h, the direct-reduced iron resultant metal rate that obtains is 82.7%, and wherein total iron (TFe) content is 65.13%, and metallic iron (MFe) content reaches 53.86%.It can also be seen that by this table the size of magnetic iron ore powder diameter has a significant impact direct-reduced iron resultant metal rate.Under the identical situation of other technical qualification, when the magnetic iron ore powder diameter was 0.8-1.0mm, even prolong the recovery time, its degree of metalization still was lower than the situation that particle diameter is 0.1-0.2mm.
Table 4 is a raw material system direct-reduced iron effect with bio oil and the magnetite powder that the quick cracking of wood chip obtains
(data are the mean value of three experiments in the table)
Claims (3)
1. method of utilizing bio oil and iron ore for the feedstock production direct-reduced iron, at first bio oil and water vapor are sent in the electrocatalysis water vapour recapitalization reactor that is filled with reforming catalyst, carrying out electrocatalysis water vapour recapitalization reaction and water gas shift reaction after the two mixing, the heating fast, is that main component is the gas mixture of hydrogen and carbonic acid gas with the carbon containing in the bio oil-hydrogen-oxygen organic matter transformation; It is characterized in that (1) is with reacted gas mixture process condenser, CO then
2It is reducing gas more than the 90vol% that chemical absorption device, moisture eliminator obtain to contain hydrogen concentration in interior tail gas purification gathering system; (2) reducing gas is preheated to 100-200 ℃; (3) reducing gas after will preheating is sent in the reduction reactor that is filled with iron ore, start simultaneously this reduction reactor from heating system, temperature is in 650 ℃-900 ℃ and be incubated 1-2h in the control reduction reactor, make the ferric oxide generation redox reaction in reducing gas and the iron ore obtain direct-reduced iron, wherein, the input flow rate of described reducing gas is 100-200ml/min, and the particle diameter of iron ore is 0.1mm-1mm; Described bio oil is the biomass cracked oil by using that is carried out the carbon containing hydrogen-oxygen organic compound of fast pyrolysis generation by reproducible biomass.
2. bio oil and the iron ore utilized as claimed in claim 1 is characterized in that for the method for feedstock production direct-reduced iron the particle diameter of described iron ore is 0.1-0.2mm.
3. bio oil and the iron ore utilized as claimed in claim 1 is characterized in that for the method for feedstock production direct-reduced iron described iron ore is by a kind of or mixed type iron ore powder in the rhombohedral iron ore that contains ferric oxide, limonite, the magnetite.
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