CN102534264A - Technique for producing and reducing ilmenite in industrial microwave kiln - Google Patents
Technique for producing and reducing ilmenite in industrial microwave kiln Download PDFInfo
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- CN102534264A CN102534264A CN2012100441081A CN201210044108A CN102534264A CN 102534264 A CN102534264 A CN 102534264A CN 2012100441081 A CN2012100441081 A CN 2012100441081A CN 201210044108 A CN201210044108 A CN 201210044108A CN 102534264 A CN102534264 A CN 102534264A
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Abstract
The invention provides a method for reducing ilmenite, which comprises the following steps: sending ilmenite, a reducer and a desulfurizer, which serve as raw materials, into a microwave high-temperature kiln; sequentially preheating, sintering and cooling; and sequentially pulverizing, screening, carrying out magnetic separation, and carrying out jet mil blending, wherein in the sintering process, microwaves of which the frequency is 2450MHz are emitted to the raw materials until the reduction temperature of the sintering belt in the kiln reaches 600-800 DEG C. In the sintering step, the microwaves of which the frequency is 2450MHz are emitted to the raw materials, so that the raw materials quickly absorb microwave energy from inside to outside, thereby ensuring the integral heating uniformity of the material, enhancing the heating uniformity of the raw materials, enabling the ilmenite to sufficiently participate into the reducing reaction, and being beneficial to enhancing the grade of the product; the microwave heating speed is high, so that the time for reaching the temperature required by the generation of the reducing reaction is shortened, thereby shortening the production cycle and lowering the energy consumption. Therefore, the ilmenite prepared by the method provided by the invention has the characteristics of high product yield and low energy consumption.
Description
Technical field
The present invention relates to the preparation of ore field, particularly a kind of industrial microwave kiln is produced the process method of reduced ilmenite.
Background technology
Ilmenite is the oxide mineral of iron and titanium, and it is the main ore that refines titanium.China's titanium aboundresources, reserves reach 10,000,000,000 tons approximately, account for 80% of world's titanium ore resource, and wherein rutile and anatase octahedrite account for 20%.The characteristics of China's titanium ore are: high-grade natural rutile is relatively poorer, and low-grade compound mineral intergrowth reserves are bigger.In recent years, along with the titanium industrial expansion, the natural rutile resource is exhausted day by day, therefore the development and use of storing abundant ilmenite resource is more and more received people's attention.
Though the ilmenite reserves are abundant, the titanium grade is lower, if use directly that it carries out that the titanium industrial production exists that efficient is low, long flow path, " three wastes " amount is big and problem such as cost height.Therefore, ilmenite generally all need carry out enrichment in advance.From metallurgical angle; The method of enrichment ilmenite has a lot; Prior art adopts the sintering synthesis method mostly, adopts carbothermic method enrichment ilmenite usually, and concrete is main reduction apparatus as adopting tunnel or dome kiln; Ilmenite and reductive agent and sweetening agent are added thermal reduction, get through cooling pulverizing, screening, magnetic separation again.But it is restive to adopt aforesaid device to have temperature, shortcomings such as production efficiency.
In order to address the above problem; Prior art adopts kiln to carry out the reduction of reduced ilmenite in addition; This method is that it is to be thermal source with oil gas; Perhaps resistive heating sintering roller kiln add thermal reduction with ilmenite and reductive agent and sweetening agent, get through cooling pulverizing, screening, magnetic separation, airflow milling blending again.For example application number is that 200410015172.2 Chinese patent discloses the method that a kind of rotary kiln is produced reduced ilmenite; This method is that raw material is sent in the kiln; Under the reduction atmosphere, add thermal reduction; Thermal zone heating reductive temperature is 1050 ℃～1180 ℃, and reduction is after cooling, screening, magnetic separation, bump selection by winnowing, blending and get.
Though adopt existing kiln to come reduced ilmenite can improve the continuous performance of production to a certain extent, but still deposit the problem of following two aspects: the first, material is heated inhomogeneous, unstable product quality, yield rate is lower; The second, the kiln operating power is higher, need reach 250KWh, and it is more higher to consume energy.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of method of reducing of ilmenite, and this method yield rate is high, and it is low to consume energy.
In view of this, the present invention provides a kind of method of reducing of ilmenite, may further comprise the steps:
With ilmenite, reductive agent and sweetening agent is raw material, said raw material is sent into carried out preheating, sintering and cooling in the microwave high-temperature kiln successively, pulverizes successively then, screening, magnetic separation and airflow milling blending;
Be that microwave reduction temperature of sintering zone to the said microwave high-temperature kiln of 2450MHz is 600 ℃～800 ℃ to the raw material transmitting frequency in the sintering process.
Preferably, the reduction temperature of sintering zone is 700 ℃～800 ℃ in the said microwave high-temperature kiln.
Preferably, the said agglomerating time is 1h～3h.
Preferably, the power of said sintering zone microwave is 9KW/h.
Preferably, the weight ratio of said ilmenite and reductive agent is 1: (0.4～1).
Preferably, the weight ratio of said sweetening agent and reductive agent is (0.04～0.1): 1.
Preferably; Said sintering is specially: the raw material after the preheating is sent into the sintered heat insulating district; Said sintered heat insulating district is provided with microwave channel; Said microwave channel links to each other with magnetron, and in the sintering process, magnetron is that the reduction temperature in microwave to the sintered heat insulating district of 2450MHz is 600 ℃～800 ℃ through microwave channel to the raw material transmitting frequency in sintered heat insulating district.
Preferably, said preheating is specially: said raw material is sent into preheating zone and heating zone successively, and the temperature of said preheating zone is 200 ℃～400 ℃, and the temperature of heating zone is 400 ℃～600 ℃.
Preferably, said refrigerative mode is a water-cooled.
The present invention provides a kind of method of reducing of ilmenite; This method adopts the microwave high-temperature kiln; In sintering process, being the microwave of 2450MHz to the raw material transmitting frequency, can be that the microwave of 2450MHz is coupled with frequency because ilmenite raw material is good absorbing material and its.Therefore under the effect of above-mentioned microwave, raw material can be rapidly rapid absorption microwave energy from inside to outside, guarantee the heating of material monolithic homogeneous, improved the homogeneity that raw material is heated, make ilmenite fully participate in reduction reaction, help improving the grade of product; In addition, this kind type of heating can make raw material in short-term, reach the required temperature of reduction reaction, and then shortening has reduced energy consumption in the time of the production cycle.Therefore, adopt method provided by the invention to prepare ilmenite and have finished product rate height, characteristic of low energy consumption.Experiment showed, and adopt method reduced ilmenite provided by the invention can save electric energy 50%～70%, the finished product rate reaches more than 90%.
Description of drawings
The microwave high-temperature furnace construction synoptic diagram that Fig. 1 adopts for the embodiment of the invention.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, describe just to further specifying feature and advantage of the present invention but should be appreciated that these, rather than to the restriction of claim of the present invention.
The embodiment of the invention discloses a kind of method of reducing of ilmenite, comprise the steps:
With ilmenite, reductive agent and sweetening agent is raw material, said raw material is sent in the microwave high-temperature kiln heat successively, sintering and cooling, pulverize successively then, screening, magnetic separation and airflow milling blending;
Be that microwave reduction temperature of sintering zone to the said microwave high-temperature kiln of 2450MHz is 600 ℃～800 ℃ to the raw material transmitting frequency in the sintering process.
The present invention considers with the reduction apparatus of microwave high-temperature kiln as ilmenite in order to improve the homogeneity that material is heated, adopts the mode of microwave heating to provide reduction reaction required heat energy.The present invention adopts the reason of microwave heating specifically to be: at first, ilmenite and charcoal all are good suction ripple materials, are suitable for carrying out microwave heating; Secondly; With respect to the mode of existing dependence heating element transmission through convection current, conduction or radiation delivery heat energy; Microwave heating is the coupling that utilizes the basal body structure of the microwave of specific band and material, makes heating object rapid absorption microwave energy from inside to outside, guarantees the heating of material monolithic homogeneous; Help ilmenite and fully participate in reduction reaction, improve product grade; At last, microwave heating speed is fast, and it is temperature required to make raw material in short-term, reach reduction reaction, and then shortening has reduced energy consumption in the time of the production cycle.
The raw material that aforesaid method uses comprises ilmenite, reductive agent and sweetening agent.Wherein, the weight ratio of ilmenite and reductive agent is preferably 1: (0.4～1), more preferably 1: (0.6～0.9).Reductive agent can adopt material well known to those skilled in the art, and is concrete like coal ash.The amount ratio of sweetening agent and reductive agent is preferably (0.04～0.1): 1, more preferably (0.07～0.8): 1.Sweetening agent can adopt material well known to those skilled in the art, and is concrete like lime.
The aforesaid method first-selection is carried out preheating earlier with raw material, and the purpose of preheating is to remove the moisture in the raw material, improves the porosity of ilmenite, and is convenient to carry out follow-up reduction step.The temperature of heating is preferably 200 ℃～600 ℃, and the time is preferably 0.5h～2h.As preferred version, preheating is carried out according to following mode: said raw material is sent into preheating zone and heating zone successively, and the temperature of preheating zone is 200 ℃～400 ℃, and the temperature of heating zone is 400 ℃～600 ℃.
Material after the preheating is proceeded the agglomerating step, and this step is the operation of ilmenite generation reduction reaction.Need to the raw material transmitting frequency microwave of 2450MHz also simultaneously; The microwave of this frequency can be coupled with raw material; Make raw material be heated to temperature required 600 ℃～800 ℃ of reduction reaction from the inside to the outside rapidly, the reduction temperature that preferably is heated to sintering zone in the microwave high-temperature kiln is 700 ℃～800 ℃.Because the aforesaid method rate of heating is fast, can obviously improve the reducing power of reductive agent, and raw material is heated evenly, so sintering time of the present invention is shorter, preferably is controlled to be 1h～3h.The power of sintering zone microwave is preferably 9KW/h.
Sintering step of the present invention is excellent to carry out according to following mode:
Raw material after the preheating is sent into the sintered heat insulating district; Sintered heat insulating is provided with microwave channel in the district; Microwave channel links to each other with magnetron; In the sintering process, magnetron is that the reduction temperature in microwave to the sintered heat insulating district of 2450MHz is 600 ℃～800 ℃ through microwave channel to the raw material transmitting frequency in sintered heat insulating district.
The work in-process that will reduce behind the sintering reaction cool off, and preferably adopt the type of cooling of water-cooled.As those skilled in the art's known content, the ilmenite after reduction is oxidized once more, and above-mentioned preheating, sintering and cooling are all carried out under reduction protection atmosphere, and the kiln internal gas pressure preferably is made as 0.5atm～0.5atm+300pa.
After the cooling with material pulverize successively, screening, magnetic separation and airflow milling blending, just obtain the ilmenite reduction product.Pulverizing, screening, magnetic separation and airflow milling blending can be carried out according to mode well known to those skilled in the art, and the present invention does not have special restriction to this.
The present invention preferably adopts microwave high-temperature kiln as shown in Figure 1, comprising:
Body of heater, body of heater is provided with preheating zone 101, heating zone 102, sintered heat insulating district 103 and cooling zone 104 successively from feeding mouth 11 to discharge port 12;
Be provided with vacuum fan 2 in the heating zone 102;
Sintered heat insulating district 103 is provided with microwave wave source passage 131, and the porthole the other end links to each other with magnetron 3;
Be equipped with thermopair 5 in preheating zone 101, heating zone 102, the sintered heat insulating district 103;
Screw thruster 4 is used to promote raw material;
Electrical control system (not marking in the drawings) is used to control burner hearth temperature inside and magnetron 3.
Whole piece kiln body is streamlined, adds circulation, cooling water-cooled overcoat; The total specified power of magnetron is 75 ± 10KW, uses lagging material to be the aluminosilicate glass fiber between roller-way and the kiln body.During work, adopt reducing atmosphere in the stove.
Adopt the technology of above-mentioned microwave high-temperature kiln reduced ilmenite to be specially:
Ilmenite, reductive agent and sweetening agent proportionally mixed obtain raw material.
Be placed on the load bearing board after raw material put into saggar, under the angle of rake promotion of screw, raw material gets into the preheating zone heating with the road, and control preheating zone temperature is 200 ℃～400 ℃.
Raw material gets into the heating zone heating with roller-way, and control heating zone temperature is 400 ℃～600 ℃.
Raw material gets into the heating of sintered heat insulating district with roller-way, is the microwave of 2450MHz with control magnetron transmitting frequency in the sintered heat insulating district, and microwave power is made as 9KW/h, and the temperature in control sintered heat insulating district is 600 ℃～800 ℃,
Raw material gets into the cooling zone cooling with roller-way.
Raw material is seen the kiln sintering line off by the screw thruster, gets into outer circulation, and taking-up is removed rough coal grain, magnetic separation, airflow milling removal free buckwheat coal and coal dust, blending through pulverizing, screening then.
Can know by foregoing; Existing for existing ilmenite reduction method, be the microwave of 2450MHz to the raw material transmitting frequency in the sintering circuit of the present invention, raw material is the rapid absorption microwave energy from inside to outside; Guarantee the heating of material monolithic homogeneous; Improve the homogeneity that raw material is heated, made ilmenite fully participate in reduction reaction, helped improving the grade of product; In addition,, shortened the temperature required time of raw material generation reduction reaction thus, and then shortening has reduced energy consumption in the time of the production cycle because microwave heating speed is fast.Therefore, adopt method provided by the invention to prepare ilmenite and have finished product rate height, characteristic of low energy consumption.
In order further to understand the present invention, ilmenite reduction method provided by the invention is described below in conjunction with embodiment.Protection scope of the present invention is not limited by the following examples.
Following examples all adopt microwave high-temperature kiln as shown in Figure 1, and roller-way is the mullite rectangle.Reductive agent is coal dust, and sweetening agent is lime.
Embodiment 1
The raw material that this enforcement is used comprises ilmenite, reductive agent and sweetening agent, and the weight ratio of ilmenite and reductive agent is 1: 0.5, and the amount ratio of reductive agent and sweetening agent is 1: 0.07.
1, be placed on load bearing board after raw material is put into saggar, under the angle of rake promotion of screw, raw material gets into preheating zone heating 1 hour with the road, and control preheating zone temperature is 300 ℃.
2, raw material gets into heating zone heating 1 hour with roller-way, and control heating zone temperature is 500 ℃, opens vacuum fan, extracts obnoxious flavour and powder impurity out.
3, raw material gets into sintered heat insulating district heating 1 hour with roller-way, is the microwave of 2450MHz with control magnetron transmitting frequency in the sintered heat insulating district, and microwave power is made as 9KW/h, and the temperature in control sintered heat insulating district is 750 ℃.
4, raw material gets into cooling zone cooling 3 hours with roller-way, to being cooled to 100 ℃.
5, raw material is seen the kiln sintering line off by the screw thruster, gets into outer circulation, and whole process adopts the control of reducing atmosphere under meter.
6, the material taking-up is removed rough coal grain, magnetic separation, airflow milling removal free buckwheat coal and coal dust, blending through pulverizing, screening.
The ability 24h of this production line * 10 plates * 6KG=1440kg/ day, rated consumption electric energy 75KW * 24h=1800KWh, the total electric energy 50KWh of actual consumption practices thrift power consumption 50%～70%, and yield rate is about 95%.
The difference of present embodiment and embodiment 1 is:
The weight ratio of iron ore and reductive agent is 1: 0.4 in the raw material, and the amount ratio of reductive agent and sweetening agent is 1: 0.05;
The preheating zone temperature is 250 ℃;
The heating zone temperature is 400 ℃;
Sintered heat insulating district temperature is 600 ℃.
The finished product rate that present embodiment makes is 92%.
The difference of present embodiment and embodiment 1 is:
The weight ratio of iron ore and reductive agent is 1: 0.8 in the raw material, and the amount ratio of reductive agent and sweetening agent is 1: 0.06;
The preheating zone temperature is 40 ℃;
The heating zone temperature is 600 ℃;
Sintered heat insulating district temperature is 800 ℃.
The finished product rate that present embodiment makes is 94%.
Can know that by The above results with respect to existing ilmenite production technique, method energy consumption provided by the invention is low practices thrift power consumption 50%～70%, and the finished product rate is higher, surpasses 90%.
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments among this paper.Therefore, the present invention will can not be restricted to these embodiment shown in this paper, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (9)
1. the method for reducing of an ilmenite is characterized in that, may further comprise the steps:
With ilmenite, reductive agent and sweetening agent is raw material, said raw material is sent into carried out preheating, sintering and cooling in the microwave high-temperature kiln successively, pulverizes successively then, screening, magnetic separation and airflow milling blending;
Be that microwave reduction temperature of sintering zone to the said microwave high-temperature kiln of 2450MHz is 600 ℃～800 ℃ to the raw material transmitting frequency in the sintering process.
2. method of reducing according to claim 1 is characterized in that, the reduction temperature of sintering zone is 700 ℃～800 ℃ in the said microwave high-temperature kiln.
3. method of reducing according to claim 1 is characterized in that, the said agglomerating time is 1h～3h.
4. method of reducing according to claim 1 is characterized in that, the power of microwave is 9KW/h in the said sintering zone.
5. method of reducing according to claim 1 is characterized in that, the weight ratio of said ilmenite and reductive agent is 1: (0.4～1).
6. method of reducing according to claim 1 is characterized in that, the weight ratio of said sweetening agent and reductive agent is (0.04～0.1): 1.
7. method of reducing according to claim 1; It is characterized in that; Said sintering is specially: the raw material after the preheating is sent into the sintered heat insulating district, and said sintered heat insulating district is provided with microwave channel, and said microwave channel links to each other with magnetron; In the sintering process, magnetron is that the reduction temperature in microwave to the sintered heat insulating district of 2450MHz is 600 ℃～800 ℃ through microwave channel to the raw material transmitting frequency in sintered heat insulating district.
8. method of reducing according to claim 1 is characterized in that, said preheating is specially: said raw material is sent into preheating zone and heating zone successively, and the temperature of said preheating zone is 200 ℃～400 ℃, and the temperature of heating zone is 400 ℃～600 ℃.
9. method of reducing according to claim 1 is characterized in that, said refrigerative mode is a water-cooled.
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| CN103447148B (en) * | 2013-08-08 | 2016-02-17 | 内蒙古科技大学 | Microwave reduction is utilized to contain concentration equipment and the magnetic selection method of bloodstone material |
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| CN108239688A (en) * | 2018-03-30 | 2018-07-03 | 胡俊旭 | A kind of microwave reduction shaft kiln and its restoring method |
| CN108715930A (en) * | 2018-06-25 | 2018-10-30 | 中南大学 | A kind of discarded desulfurizing agent is applied to the processing method of sintering |
| CN108796215A (en) * | 2018-06-25 | 2018-11-13 | 中南大学 | A kind of processing method of discarded desulfurizing agent |
| CN114686687A (en) * | 2022-03-09 | 2022-07-01 | 山东产研绿洲环境产业技术研究院有限公司 | Ilmenite microwave titanium enrichment device and method |
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Application publication date: 20120704 |