CN102925667B - Independent container for producing rich-titanium material and preparation method of rich-titanium material with independent container - Google Patents
Independent container for producing rich-titanium material and preparation method of rich-titanium material with independent container Download PDFInfo
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- CN102925667B CN102925667B CN201210462480.4A CN201210462480A CN102925667B CN 102925667 B CN102925667 B CN 102925667B CN 201210462480 A CN201210462480 A CN 201210462480A CN 102925667 B CN102925667 B CN 102925667B
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Abstract
The invention discloses an independent container for producing a rich-titanium material, and a preparation method of the rich-titanium material with the independent container. The independent container consists of two parts, namely a tray and an upper cover, wherein the tray comprises a bottom plate for placing ilmenite briquettes, a lower part heat-preservation sleeve wrapped on the bottom plate, and a support plate connected with the bottom part of the lower part heat-preservation sleeve; the upper cover comprises a container liner which is placed on the bottom plate and can cover the ilmenite briquettes, an upper part heat-preservation sleeve that is wrapped on the container liner, and brackets which penetrate through the upper part heat-preservation sleeve from outside to inside and are connected with the container liner; and high-temperature resistant wave-transparent coatings are arranged between the bottom plate and the lower part heat-preservation sleeve and between the container liner and the upper part heat-preservation sleeve. The independent container is wave-transparent, resists high temperature resistant and can preserve heat; and the preparation method of the rich-titanium material adopts a continuous microwave kiln and the independent container for producing the rich-titanium material, and also adopts a new reduction mechanism, so that the air pollution is less, and the energy consumption is low.
Description
Technical field
The present invention relates to a kind ofly prepare the container that rich titanium material is used, and apply the method that this container is prepared rich titanium material.
Background technology
Along with titanium industrial expansion, the natural rutile resource that titanium grade is higher is increasingly exhausted, and this just forces people to develop the abundant ilmenite resource of reserves.Because ilmenite titanium grade is low, be directly used in that titanium industrial production there will be that efficiency is low, long flow path, " three wastes " amount are large, high in cost of production problem, so generally all need preconcentration to become high-grade rich titanium material-titanium slag or artificial rutile, and then for titanium industrial production.Therefore, the ilmenite of research high-efficient energy-saving environment friendly is produced rich titanium material method and is had very important meaning for titanium industrial expansion.
The traditional method of producing rich titanium material is mostly to belong to carbothermic reduction reaction, first use traditional microwave kiln or high-power mineral hot furnace that ilmenite and various carbonaceous and binder mixtures are smelted into liquid, make the iron oxide reduction in ilmenite become molten iron, realize the separated of titanium and iron, thereby obtain rich titanium material.This method is because be high-temperature service, and need to add in a large number such as additives such as pitch cokes, so easily cause atmospheric pollution, simultaneously because energy consumption is too high, there is no enough market competitivenesss, the pressure and the national energy-saving that are subject at present environmental protection reduce discharging the urgent and on the verge of being replaced of policy.
Summary of the invention
The object of this invention is to provide a kind of autonomous container that rich titanium material uses and method of preparing rich titanium material thereof of producing, solve traditional technical problem that rich titanium preparation method for material is seriously polluted, energy consumption is high.
For achieving the above object, the present invention adopts following technical scheme: a kind ofly produce the autonomous container that rich titanium material is used, it is characterized in that: by pallet and upper cover two portions, formed, described pallet comprises places the base plate that ilmenite briquetting is used, wrap in the bottom muff on base plate, and the supporting plate that is connected to muff bottom, bottom, described upper cover comprises the container inner liner that is placed on base plate and can covers ilmenite briquetting, wrap in the top muff on container inner liner, and ecto-entad is through top muff the bracket that is connected with container inner liner, between described base plate and bottom muff, between container inner liner and top muff, be equipped with high temperature resistant wave-permeable coating.
The horizontal cross sectional geometry of described container inner liner and base plate can be square, and the length of side of the horizontal section of container inner liner is less than the length of side of the horizontal section of base plate.
The horizontal cross sectional geometry of described container inner liner and base plate also can be circle, and the diameter of the horizontal section of container inner liner is less than the diameter of the horizontal section of base plate.
The vertical cross-section shape of described container inner liner can be convex shape.
A kind ofly apply the method that autonomous container that the rich titanium material of above-mentioned production uses is produced rich titanium material, it is characterized in that step is as follows: step 1, ilmenite briquetting is placed in the autonomous container that the rich titanium material of the production of can wave transparent and can be incubated uses, then put into microwave kiln laser heating 80~120 minutes, and then being sent microwave kiln, described ilmenite briquetting is the mixture briquetting that contains ilmenite powder, coal dust, borax, NaCl, iron oxide red and iron powder.
The material of emitting in step 6, hydrolytic decomposition pot is separated and cleaning through six grades of cyclone separators, then dry, finally obtains rich titanium material.
Compared with prior art the present invention has following characteristics and beneficial effect: container of the present invention is microwave reduction container, and its feature is, and 1, adopted rational design, shared the burden of the resistance to material of traditional kiln, break the whole up into parts; 2, maintenance service only relates to the autonomous container that the rich titanium material of production is used, so become very simple; 3, the most important thing is, produce autonomous container wave transparent, high temperature resistant, insulation that rich titanium material is used, especially there is good heat-insulating property, so producing the capacity usage ratio of the autonomous container inside that rich titanium material uses improves greatly, not only energy-conservation, can realize and being rapidly heated, guarantee best metallurgical atmosphere, for obtaining desirable rich titanium material, lay a good foundation simultaneously.
The method of the invention is a kind of titanium dioxide process of enriching, also can make microwave method solid state reduction produce rutile technique, with respect to traditional pyrogenic process, wet method, has larger difference.The method of the invention, from reduction mechanism, belongs to early stage (700 ℃) and relies on pyrolysis gas to comprise the reduction of hydrogen, alkanes (uncombined carbon and hydrogen that alkanes cracking produces), just there will be the direct-reduction of carbon latter stage.Not take the direct-reduction of carbon as main, compare with the carbothermic reduction in conventional art, in principle, have essential distinction.
The method of the invention has been utilized microwave kiln and has been produced the autonomous container that rich titanium material is used, and has avoided dexterously the mode of traditional kiln indirect heating, makes the resistance to material of kiln and heat preservation method become very simple.
The method of the invention has been utilized microwave kiln and has been produced the autonomous container that rich titanium material is used, and has also adopted new reduction mechanism simultaneously, so not only atmospheric pollution is little, and energy consumption is low.
The ultimate principle of the method for the invention is, the ilmenite briquetting that contains ilmenite powder is placed in the autonomous container that the rich titanium material of the production of can wave transparent and can be incubated uses, then by the microwave kiln of continuous operation, make ilmenite briquetting be given energy by microwave, make full use of the strong wave absorbtion of ilmenite and the wave transparent heat-insulating property of the autonomous container that the rich titanium material of production is used simultaneously, by microwave energy maximum using, and build best metallurgical reduction gas atmosphere, realize continuous microwave kiln autonomous container internal solid reduced ilmenite briquetting, finally utilize hydrolysis method to remove the fe in (restoring) ilmenite briquetting, realize ferrotianium separation and obtain rich titanium material, or even artificial rutile (needing further roasting to obtain).
From integrated artistic, the operational path of the method for the invention also has essential distinction with traditional preparation method.The present invention is a kind of airtight operation of producing the autonomous container that rich titanium material uses of having applied, its step is the Microwave Heating ilmenite briquetting (whole process is to carry out on continuous rollgang) that in the autonomous container of first using at the rich titanium material of production, (having sealed thermal insulating environment), dependence are come in thoroughly, after heating, ilmenite briquetting falls fe wherein through magnetic separation and in the internal corrosion of hydrolysis separating tank again, last residuum is rich titanium material (by after the further roasting of rich titanium material, can also obtain artificial rutile).
The method of the invention does not need huge pelletizing manufacturing system (being again pelletizing sintering system), does not need additional carbon element to supplement yet, but has adopted ilmenite briquetting.The formula of ilmenite briquetting and shape and pressing process, all be essentially different with traditional pelletizing, so the method for the invention has been avoided the huge pelletizing manufacturing system (being pelletizing sintering system) of setting up in order to improve metallurgical performance in traditional technology, has simplified production process.
The method of the invention adopts microwave kiln to replace traditional high-power mineral hot furnace, and microwave kiln is heated to be leading with internal tank, take full advantage of micro-wave energy.
The method of the invention has adopted ilmenite briquetting, because metallurgy environment and the atmosphere of ilmenite briquetting inside are good.Ilmenite briquetting is continuous production, and must in microwave kiln, could meet processing requirement by continuous operation.
The mineral of the ilmenite the present invention is directed to are not limited, can use all sea sand ore deposits.
That the microwave kiln furnitures of mentioning in the present invention have is easy to maintenance, can continuous operation and the high feature of microwave energy rate of utilization, especially the microwave source of kiln body both sides multiple spot dense distribution and the rollgang of loop line form (can transport ilmenite briquetting continuously, realized automatic production, for the expansion in future of the present invention provides space) not only realized the optimum coupling of microwave in big-length kiln chamber, and eliminated thermal runaway, guaranteed homogeneity and the stability of product quality.Transformer in microwave kiln and attached electric elements are arranged on the kiln body support frame of kiln body both sides, avoid the detrimentally affect that furnace gas temperature because producing continuously causes to transformer and attached electric elements, greatly simplified the thermal insulation fire-resistant system of microwave kiln bulky complex.
Furnace gas temperature in the kiln of the microwave kiln of mentioning in the present invention probably only has 100 ℃ of left and right, and (furnace gas temperature in traditional microwave kiln kiln probably has 1200 ℃~1300 ℃, smelting temperature in traditional high-power mineral hot furnace is up to 1700 ℃), the outer temperature near kiln body of kiln probably only has 50 ℃ of left and right, so while utilizing the present invention to produce rich titanium material, whole power consumption is only equivalent to use 40%~50% of traditional method.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention will be further described in detail.
Fig. 1 is the main TV structure schematic diagram of microwave kiln.
Fig. 2 is that schematic diagram is looked on the right side of Fig. 1.
Fig. 3 is the schematic diagram that rollgang coordinates with kiln body.
Fig. 4 is that the master who produces the autonomous container that rich titanium material uses looks schematic diagram.
Fig. 5 is the schematic top plan view of Fig. 4.
Fig. 6 is the schematic diagram of A-A section in Fig. 4.
Reference numeral: 1-kiln body, 2-magnetron, 3-opening for feed, 4-discharge port, 5-rollgang, 6-roller-way drive-motor, 7-heat preservation protective layer, 8-water-cooling sandwich, 9-kiln body support frame, 10-transformer and attached electric elements, 11-smoke discharging pipe, 12-produces the autonomous container that rich titanium material is used, 13-ilmenite briquetting, 14-base plate, 15-bottom muff, 16-high temperature resistant wave-permeable coating, 17-supporting plate, 18-container inner liner, 19-top muff, 20-bracket.
Embodiment
Referring to Fig. 4-6, in the present embodiment, producing the autonomous container 12 that rich titanium material uses is comprised of pallet and upper cover two portions, described pallet comprises places the base plate 14 that ilmenite briquetting is used, wrap in the bottom muff 15 on base plate 14, and the supporting plate 17 that is connected to muff bottom, bottom, described upper cover comprises the container inner liner 18 that is placed on base plate 14 and can covers ilmenite briquetting 13, wrap in the top muff 19 on container inner liner 18, and ecto-entad is through top muff 19 bracket 20 that is connected with container inner liner 18, between described base plate 14 and bottom muff 15, between container inner liner 18 and top muff 19, be equipped with high temperature resistant wave-permeable coating 16.In the present embodiment, the vertical cross-section of container inner liner 18 is shaped as convex shape.
In the present embodiment, the horizontal cross sectional geometry of container inner liner 18 and base plate 14 is square, and the length of side of the horizontal section of container inner liner 18 is less than the length of side of the horizontal section of base plate 14.In other embodiments, can also be that the horizontal cross sectional geometry of container inner liner 18 and base plate 14 is circle, and the diameter of the horizontal section of container inner liner 18 be less than the diameter of the horizontal section of base plate 14.
The autonomous container that the rich titanium material of described production is used is particular design, and its design is most important, and it is the separate unit of production line cocycle.First, produce autonomous container employing is high temperature resistant and wave transparent is very capable material making container inner liner 18 and base plate 14 that rich titanium material is used, container inner liner 18 and base plate 14 can be used as the protective layer that bears temperature of reaction, secondly, outside container inner liner 18 and base plate 14, brushed one deck protective cover, it is high temperature resistant wave-permeable coating 16, at the certain thickness top of the outer covering of high temperature resistant wave-permeable coating 16 muff 19 and bottom muff 15(, by lagging materials such as rock wools, made again), this structure makes ilmenite briquetting fully after microwave energy absorbing, reduce as much as possible scattering and disappearing of energy just, greatly improved the utilization ratio of energy, described high temperature resistant wave-permeable coating 16 can prevent that container inner liner 18 from damaging top muff 19 because temperature is too high, prevent that base plate 14 from damaging bottom muff 15 because temperature is too high, finally, use the bracket 20(of integrated steel also can be framework) container inner liner 18 and top muff 19 are connected into a set of independently individual, mechanical manipulator by designed, designed coordinates bracket 20 taking and placing container inner liners 18, can realize automated handling material, forms continuously and produces.
Referring to Fig. 1, produce autonomous container 12 wave transparents that rich titanium material uses, high temperature resistant, insulation, produce autonomous container 12 ISNs that rich titanium material uses and be placed with ilmenite briquetting 13, each produce autonomous container 12 that rich titanium material uses be independently individual, complete independently reduction reaction.Produce the autonomous container 12 that rich titanium material uses and be placed on rollgang 5, according to desin speed operation, autonomous container 12 can keep reasonable distance continuous operation under the driving of rollgang 5.
The method that the autonomous container that the rich titanium material of the above-mentioned production of this application is used is produced rich titanium material, its step is as follows.
In step 1, in the early stage of heating, in ilmenite briquetting, can there is following principal reaction: C
2h
6→ C
2h
4+ H
2, C
2h
4→ CH
4+ C, CH
4→ C+2H
2, FeO+n
2h
2→ Fe+H
2o+ (n
2-1) H
2; In the later stage of heating, in ilmenite briquetting, can there is Fe
xo
ythe reaction of+C (cracking carbon) → Fe+CO.
The material of emitting in step 6, hydrolytic decomposition pot is separated and clean through six grades of cyclone separators, then dry, finally obtains iron-holder≤1%(weight percent) rich titanium material.
In the present embodiment, ilmenite briquetting 13 mainly forms (total amount is 100%) by following raw materials by weight.
Ilmenite powder 78.5%~82.5%(determines according to all iron content in ilmenite, and content is high to be removed the limit, the low capping of content); Coal dust 10%~14%(determines according to all iron content in ilmenite, the high capping of content, content is low to be removed the limit); Borax 3%~4%(requires can not deliquescence, caking or weathering); NaCl0.5%~1.5%(requires can not deliquescence, caking or weathering); Iron oxide red 1.0%~1.5%; Iron powder 0.5%; In above-mentioned weight percent, the weight percent of the weight percent+coal dust of ilmenite powder also needs to guarantee between 92.5%~95%, and the weight percent of the weight percent+iron powder of weight percent+iron oxide red of the weight percent+NaCl of borax also needs to guarantee between 5.0%~7.5%.
Described coal dust is reductive agent, and borax, NaCl, iron oxide red and iron powder are additive.
In the present embodiment, the granularity of ilmenite is 70 order~200 orders, moisture content≤0.5%.Fe in iron oxide red
2o
3content>=97%, moisture content < 1%.The content > 98% of the iron in iron powder, non-corroding caking, granularity is 100 order~200 orders.
The generation of above proportioning comes from the molten brazing of oxygen common in production, people are accustomed to using the mixture of borax and salt to be sprinkling upon the molten metal surface of high temperature, make the metallic surface of high-temperature fusion remain clean and not oxidized, this is very great for the fe effect restoring in the solid state reduction process in the present invention, can keep its surfactivity, for occurring that as early as possible the complete diffusion reaction of iron crystal stock and ore particle inside provides assurance, avoided causing metallurgical atmosphere variation because of the covering of selective oxidation and impurity.
Following table is the result that the proportioning of different embodiment records in laboratory.In table, data are weight percentage.Result described in table be ilmenite briquetting after above-mentioned steps one to four, use 10% salt acid soak 10 minutes, then dry the TiO that chemical examination obtains
2content (because above-mentioned steps five and step 6 are the steps of large-scale industrial production, so in order to record TiO in laboratory
2content, need to adopt 10% salt acid soak 10 minutes, the method for then drying chemical examination is surveyed TiO
2content, this experimental technique is substantially the same with the effect of above-mentioned steps five and step 6).
The making step of described ilmenite briquetting 13 is as follows: a, ilmenite powder and reductive agent (coal dust), additive (borax, NaCl, iron oxide red and iron powder) are mixed in proportion to resulting mixture, add again amount of the mixture 5%(weight percent) water, then in stirrer, stir 5~15 minutes; B, the material of mixing is pressed under pressing machine (such as the pressing machine of 30Mpa) to the briquetting (thickness of briquetting and the penetrativity of microwave match, can guarantee that the sufficient reacting of briquetting inside is as the criterion completely) with certain thickness brick shape; C, at briquetting surface spraying water-based graphite coating, then under the condition of 80 ℃~120 ℃, dry 10~20 minutes.In order to make the process of suppressing briquetting become more easily better, make the forming effect of ilmenite briquetting better, can also in the mixture being mixed in proportion, add again micro-binding agent, such as wilkinite, but it is minimum that content should control to, guarantee the dry strength of briquetting.
Adopt the step of high pressure compacting and surface spraying water-based graphite coating, can make the inside of ilmenite briquetting there is good metallurgy environment and atmosphere, avoid the huge pelletizing sintering system of setting up in order to improve metallurgical performance in traditional technology, simplified production process.In addition, the ilmenite briquetting of standard geometrical shapes also in order to realize, produce continuously and the accumulating of material is provided convenience by mechanize.
Referring to Fig. 1-3, in the present embodiment, described microwave kiln includes kiln body 1, magnetron 2, rollgang 5, roller-way drive-motor 6 and transformer and attached electric elements 10, described kiln body 1 arranged transversely is also placed on kiln body support frame 9, one end, two ends of kiln body 1 is provided with opening for feed 3, the other end is provided with discharge port 4, the top of kiln body 1 is communicated with smoke discharging pipe 11, and the inwall of kiln body 1 is provided with heat preservation protective layer 7, and the outer wall of kiln body 1 is provided with water-cooling sandwich 8.
The structure of described kiln body 1 is by a large amount of experiments and produces checking: kiln body inwall brushing protective material (being heat preservation protective layer 7), the external wall of kiln is set up recirculated water cooling cover (being water-cooling sandwich 8).Described transformer and attached electric elements 10(comprise the elements such as high-tension transformer, electric capacity, diode etc.) be placed in that kiln is external, on the kiln body support frame 9 of the kiln body left and right sides, namely be designed into the position separated with kiln body 1, can avoid the interference of kiln temperature.Described magnetron 2 is arranged on that kiln is external, the left and right sides of kiln body, and magnetron 2 by opening for feed to discharge port direction multiple spot dense distribution, what magnetron 2 adopted is the form of small power multiple spot dense distribution, more satisfactory to whole reduction reaction.
Referring to Fig. 1, Fig. 3, the type of transmission of microwave kiln is rollgang 5(steel roller-way) adjustable speed operation, rollgang 5 is closed loops, rollgang 5 constantly turns round, can realize the mode of production of continuous reduced ilmenite, meanwhile, the discharge port end at kiln body 1 can arrange mechanical manipulator, the automatization of realization handling material.
Claims (2)
1. produce the autonomous container (12) that rich titanium material is used for one kind, it is characterized in that: by pallet and upper cover two portions, formed, described pallet comprises places the base plate (14) that ilmenite briquetting is used, wrap in the bottom muff (15) on base plate (14), and the supporting plate (17) that is connected to muff bottom, bottom, described upper cover comprises the container inner liner (18) that is placed on base plate (14) above and can covers ilmenite briquetting, wrap in the top muff (19) on container inner liner (18), and ecto-entad is through top muff (19) the bracket (20) that is connected with container inner liner (18), between described base plate (14) and bottom muff (15), between container inner liner (18) and top muff (19), be equipped with high temperature resistant wave-permeable coating (16),
The vertical cross-section of described container inner liner (18) is shaped as convex shape;
The horizontal cross sectional geometry of described container inner liner (18) and base plate (14) is square, and the length of side of the horizontal section of container inner liner (18) is less than the length of side of the horizontal section of base plate (14);
Or the horizontal cross sectional geometry of described container inner liner (18) and base plate (14) is circle, and the diameter of the horizontal section of container inner liner (18) is less than the diameter of the horizontal section of base plate (14).
2. apply the method that autonomous container that the rich titanium material of production described in the claims 1 uses is produced rich titanium material, it is characterized in that step is as follows:
Step 1, ilmenite briquetting is placed in the autonomous container (12) that the rich titanium material of the production of can wave transparent and can be incubated uses, then put into microwave kiln laser heating 80~120 minutes, and then being sent microwave kiln, described ilmenite briquetting is the mixture briquetting that contains ilmenite powder, coal dust, borax, NaCl, iron oxide red and iron powder;
Step 2, open and produce the autonomous container that rich titanium material is used, the ilmenite briquetting of red heat is pushed in cooling and stirring device fast, make ilmenite briquetting become the pulverulent material of 180 ℃~220 ℃;
Step 3, pulverulent material is risen in air float separator, with air float separator, remove micro mist more than 200 orders in pulverulent material;
Step 4, by the pulverulent material after selection by winnowing again through three grades of magnetic separation, obtain Magnetic Materials;
Step 5, Magnetic Materials is joined in hydrolytic decomposition pot, in the salt solution of 40 ℃~70 ℃, do not stopped to stir, blast air simultaneously and be oxidized, make the fe particle on Magnetic Materials ore particle surface be oxidized to Fe
2o
3and proceed in the aqueous solution;
The material of emitting in step 6, hydrolytic decomposition pot is separated and cleaning through six grades of cyclone separators, then dry, finally obtains rich titanium material.
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