CN101117665A - Fluid-bed reactor for oxido-reduction sintering of high calcium magnesium titanium slag - Google Patents
Fluid-bed reactor for oxido-reduction sintering of high calcium magnesium titanium slag Download PDFInfo
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- CN101117665A CN101117665A CNA200610089104XA CN200610089104A CN101117665A CN 101117665 A CN101117665 A CN 101117665A CN A200610089104X A CNA200610089104X A CN A200610089104XA CN 200610089104 A CN200610089104 A CN 200610089104A CN 101117665 A CN101117665 A CN 101117665A
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Abstract
The present invention relates to a fluidized bed reactor used for oxidizing and deoxidizing and baking high calcium magnesium titanium slag to remove calcium for improving the titanium inert solid grade, and comprises a cylindrical column material settlement section, a cylindrical column material reaction section, and a coniform column air preheating section. The main body of the cylindrical fluidized bed reactor is the cylindrical column material reaction section, and the top part is of a horn mouth shape, the top part of the horn mouth column body is connected with the cylindrical column material settlement section, the bottom end of the reaction is connected with the air preheating section. The upper part of the air preheating section is provided with a material feeding port, and the bottom part is arranged with an air distribution plate under which an air inlet is provided. The lower part of the material reaction is provided with a material discharging port, and the top part is provided with an air outlet. More than one baffle with holes is arranged in the material reaction. The present invention can make the residence time of particles of the high calcium magnesium titanium slag prolong following the increase of the grain size to satisfy the requirements of the reaction time of different grain sizes of particles.
Description
Technical field
The invention belongs to gas-solid phase processing reactor field, particularly be used for the fluidized-bed reactor that oxidation-reduction roasting high calcium magnesium titanium slag calcium-magnesium removing improves titanium ore material grade.
Background technology
China is titanium resource big country, and wherein the reserves in Flos Bombacis Malabarici western part account for more than 1/4 of world's total amount.At present, the utilization of titanium resource is to obtain titanium tetrachloride by chlorination process in the titaniferous ore, and producing titaniums such as titanium white and titanium sponge by titanium tetrachloride then is goods.Yet climb calcium-magnesium content height in the western titanium ore, smart titanium ore material (the claiming high calcium magnesium titanium slag again) quality that obtains behind the process electrosmelting is lower, wherein TiO
2Content has only 70%～80%, and calcium magnesium (CaO+MgO) foreign matter content is but up to 7%～11%, and advanced chloridization process is very harsh to ingredient requirement, and its CaO and MgO content must be controlled at below the 1.5wt%.Calcium-magnesium content is too high to cause the liquid phase after the chlorination to be separated out, and very easily causes the bed bonding, thereby chlorination process can't be carried out.The calcium-magnesium content height becomes climbs the main difficult problem that western titanium resource utilizes, and reduces calcium, the Mg content of climbing in the western smelting titanium slag, and promoting its quality is that it is able to key for high-efficient use.
U.S. Pat 5830420 has been introduced redox-hydrochloric acid leaching technology and has been promoted the quality of high calcium magnesium titanium slag, the core of this technology is calcium magnesium in the high calcium magnesium titanium slag to be formed be easy to the thing phase that is leached by hydrochloric acid by the oxidation-reduction calcination process, removes calcium magnesium by hydrochloric acid leaching then.Fluidized-bed reactor because have that gas-solid well contacts, input and output material advantages such as control easily, and be used to the reactor of oxidation-reduction roasting high calcium magnesium titanium slag calcium-magnesium removing.But this patent is just mentioned the employing fluidized-bed reactor, and does not specifically disclose the structure of fluidized-bed reactor.During common fluidized-bed roasting high calcium magnesium titanium slag material because the residence time distributes comparatively homogeneous, cause long and coarse particles reaction times deficiency of fine particle reaction times, the production efficiency of oxidation-reduction roasting high calcium magnesium titanium slag descends.Simultaneously, according to Geldart particle classification, climb western high calcium magnesium titanium slag particle and belong to the category-B particle.When adopting the normal stream fluidized bed reactor to handle this type of material, the bed expansion rate is lower, occurs bubble in the fluid mapper process mutually with mutually close, and gas exchange rate is very low between the two-phase, causes the gas-solid contact efficiency to reduce; Fluidization pressure drop instability can form joint and unstable operational stage such as gush, and air pocket is difficult for broken, and the gas-solid contact efficiency is descended, directly the transformation efficiency that reacts of influence and the productive rate of product etc.
Summary of the invention
The objective of the invention is to overcome the above-mentioned technical problem that existing fluidized-bed reactor exists, provide a kind of under hot conditions, the high calcium magnesium titanium slag particle fully contacts with oxidizing gas or reducing gas physical efficiency, the residence time of high calcium magnesium titanium slag particle in fluidized-bed of different-grain diameter can be controlled by fluidizing gas velocity and feed rate, and can carry out the fluidized-bed reactor of quantity-produced oxidation-reduction roasting high calcium magnesium titanium slag.
Principle of work of the present invention is: gas from bottom to top is by the dispersion of band foraminous baffle plate, and air pocket is able to fragmentation or division, makes gas-solid fully to contact; By multiwalled band foraminous baffle plate is installed, can make to have a plurality of concentrated phase sections in the fluidized-bed, both made full use of the bed space, reduced the axial backmixing of gas-solid phase again, improve the distribution of the solid phase residence time; Gu employing gas-and flow to upward operation, material adds from reactor lower part, under the effect of air-flow, move up step by step, because the different-grain diameter particle is subjected to the difference that influences of fluidizing gas velocity, make the contain rate of the little particle of particle diameter in bed be lower than the rate that contains in raw material, thereby obtain the short residence time, and the contain rate of the big particle of particle diameter in bed is higher than containing rate and can obtain the long residence time in raw material, helps satisfying the demand of different-grain diameter particle to the reaction times.
Technical scheme of the present invention is that existing fluidized-bed reactor is improved, in the intravital columniform cylinder material reaction section of fluidized-bed reactor, have and be connected with a bed body and be with the foraminous baffle plate, its connection is that band foraminous baffle plate is fixedlyed connected with the bed body by flange, or band foraminous baffle plate is fixedly connected on anchor and the tubing string that the bed body is connected, is being with unpowered drive unit on the foraminous baffle plate.
The object of the present invention is achieved like this: the fluidized-bed reactor of oxidation-reduction roasting high calcium magnesium titanium slag mainly is made of columniform cylinder material settling section, columniform cylinder material reaction section and conical cylinder gas preheating section;
The main body of one cylindrical stream fluidized bed reactor is columniform cylinder material reaction section, its top is the hydraucone shape, connect a columniform cylinder material settling section at the top of hydraucone cylinder, connect a conical cylinder gas preheating section in the bottom of columniform cylinder material reaction section;
Have the material opening for feed on the wall on the top, junction of columniform cylinder material reaction section and conical cylinder gas preheating section, the bottom in conical cylinder gas preheating section is equipped with gas distribution grid, and the grid distributor below is gas feed;
On the cylinder wall below the hydraucone of columniform cylinder material reaction section, have the material discharge port, have pneumatic outlet at the top of columniform cylinder material settling section;
In columniform cylinder material reaction section the inside more than one band foraminous baffle plate is installed, the aperture is 1/50～1/8 with the internal diameter ratio of columniform cylinder material reaction section, and its perforate is not limit.
Tubing string more than one or one is installed in the described columniform cylinder material reaction section, and tubing string is fixed on the anchor, and anchor is fixed on the fluidized-bed reactor main body.
Described band foraminous baffle plate can be fixed on the wall of columniform cylinder material reaction section by flange, or on the fixed tubing string.
Described material discharge port is out the position when columniform cylinder material reaction section begins to become the hydraucone cylinder.
Spacing between the described band foraminous baffle plate is 1/5～2/1 with the internal diameter ratio of columniform cylinder material reaction section.
The bottom of fluidized-bed reactor of the present invention is that taper shape can guarantee that processed high calcium magnesium titanium slag particle still is in fluidized state in the gas warm, and top is that the material settling section of expanding reach can prevent that the small-particle in the high calcium magnesium titanium slag particle from being taken out of by air-flow.Described band foraminous baffle spacing is 1/5～2/1 with the internal diameter ratio of columniform cylinder conversion zone, and the aperture of band foraminous baffle plate is 1/50～1/8 with the internal diameter ratio of columniform cylinder material reaction section, can guarantee effectively that the residence time of fine particle in fluidized-bed reactor shortens, and the residence time of coarse particles in fluidized-bed reactor prolongs, and satisfies the needs of different-grain diameter particle to the reaction times.
The fluidized-bed reactor of oxidation-reduction roasting high calcium magnesium titanium slag of the present invention is when work, the high calcium magnesium titanium slag raw material is joined in the fluidized-bed reactor by opening for feed, reacted high calcium magnesium titanium slag is discharged by discharge port, oxidizing gas or reducing gas disperse the laggard fluidized-bed reactor of going into by gas feed through gas distribution grid, under sandwich tape foraminous baffle effect, fully contact with the high calcium magnesium titanium slag particle, the fine particle of taking out of the sedimentation of slowing down in expanding reach, reacted gas is discharged by pneumatic outlet.
The fluidized-bed reactor of the oxidation-reduction roasting high calcium magnesium titanium slag calcium-magnesium removing of gas-solid of the present invention and stream contact sandwich tape foraminous baffle plate, can effectively avoid in the normal stream fluidized bed reactor particle residence time homogeneous comparatively, cause long and insufficient shortcoming of coarse particles reaction times of fine particle reaction times; The interior high calcium magnesium titanium slag particulate residence time of fluidized-bed reactor is increased with particle diameter prolong, satisfy the demand of different-grain diameter particle the reaction times; And the residence time of particle in bed effectively improved the reaction efficiency of oxidation-reduction roasting high calcium magnesium titanium slag calcium-magnesium removing by feed rate and the stable control of fluidizing gas velocity.High calcium magnesium titanium slag after the oxidation-reduction roasting can be used for existing chloridization process requirement behind hydrochloric acid leaching.
Fluidizing agent is for containing O under the described oxidizing condition
2Gas, service temperature is 700 ℃～1000 ℃.
Fluidizing agent is CO gas, H under the described reductive condition
2The mixed gas of gas, reformation Sweet natural gas mixed gas or above-mentioned gas, service temperature are 700 ℃～900 ℃.
The fluidizing gas velocity of described oxidizing gas and reducing gas is 0.05m/s～0.50m/s.
Described feed rate is directly proportional per unit m with the horizontal interfacial area of fluidized-bed reactor conversion zone
2Feed rate on the horizontal interface is 318.5kg/h～3185kg/h.
The present invention compared with prior art has following advantage:
(1) in single fluidised bed, adopts multiwalled band foraminous baffle plate, both effectively utilized the space of fluidized-bed reactor, saved investment, can suppress the particulate axial backmixing again, the material that guarantees different-grain diameter has the corresponding residence time in fluidized-bed reactor, and the residence time is controlled easily.
(2) solid since taked gas-and the flow direction on operator scheme, the effect of distribution again through sandwich tape foraminous baffle plate, the contain rate of the big titanium slag particle of particle diameter in bed is higher than the rate that contains in the raw material, can obtain the long residence time, and the contain rate of the little titanium slag particle of particle diameter in bed is lower than the rate that contains in the raw material, then obtain the short residence time, thereby satisfied the required reaction times of different-grain diameter particle.
(3) add suitable band foraminous baffle plate after, eliminated joint and emerged in large numbers and resembling, bed has stable fluidization pressure drop.
(4) need not power-equipment, easy and simple to handle, the equipment life cycle is long, and technology is easy to amplify.
Description of drawings
Fig. 1. the fluidized-bed reactor vertical profile synoptic diagram (flange is fixed) of a kind of sandwich tape foraminous baffle plate of the present invention.
Fig. 2. the fluidized-bed reactor vertical profile synoptic diagram (tubing string is fixed) of another kind of sandwich tape foraminous baffle plate of the present invention.
Reference numeral
1. material settling section 2. material reaction sections 3. gas preheating sections
4. opening for feed 5. flanges 6. are with the foraminous baffle plates
7. gas feed 8. gas distribution grids 9. discharge ports
10. pneumatic outlet 11. anchors 12. tubing strings
Embodiment
Further specify fluidized-bed reactor of the present invention below in conjunction with embodiment and be used for oxidation-reduction roasting high calcium magnesium titanium slag calcium-magnesium removing.
See also Fig. 1.One is high for 1800mm, internal diameter are the fluidized-bed reactor of the oxidation-reduction roasting high calcium magnesium titanium slag of 86mm, and it mainly is made of columniform cylinder material settling section 1, columniform cylinder material reaction section 2 and conical cylinder gas preheating section 3.
The top of one columniform cylinder material reaction section 2 is the hydraucone shape, connect a columniform cylinder material settling section 1 at the top of hydraucone cylinder, connect a conical cylinder gas preheating section 3 in the bottom of columniform cylinder material reaction section, in columniform cylinder material reaction section 2 the insides, by a plurality of flanges 5 a plurality of band foraminous baffle plates 6 are fixed on the wall of columniform cylinder material reaction section, the aperture of band foraminous baffle plate 6 is 2.5mm, and is 100mm with the spacing between the foraminous baffle plate 6 in twos;
Have material opening for feed 4 on the wall on columniform cylinder material reaction section 2 and the top, junction of conical cylinder gas preheating section 3, in the bottom of 3 li of conical cylinder gas preheating sections gas distribution grid 8 is installed, the grid distributor below is gas feed 7;
On the cylinder wall below the hydraucone of columniform cylinder material reaction section 2, and be that position when columniform cylinder material reaction section 2 begins to become the hydraucone cylinder has material discharge port 9, have pneumatic outlet 10 at the top of columniform cylinder material settling section 1.
The high calcium magnesium titanium slag particle is added in the fluidized-bed reactor through opening for feed 4 by screw feeder, and reaction back high calcium magnesium titanium slag is collected by hopper after discharge port 9 is discharged.In the oxidising process, service temperature is 850 ℃, and oxidizing gas is for containing O
2Air, fluidizing gas velocity is 0.106m/s; In the reduction process, service temperature is 800 ℃, and reducing gas is a CO gas, and fluidizing gas velocity is 0.106m/s.Feed rate is 5.0kg/h.Experiment finds that titanium slag is grain fluidized evenly, and the phenomenon that joint gushes disappears, and bed pressure drop is stable, can realize the input and output material of continous-stable.When the mean residence time of oxidation and reduction process was 90min, the high calcium magnesium titanium slag after the oxidation was through X-ray diffractometer (XRD) analysis revealed, except Ti
3+Be converted into Ti
4+And Fe
2+Be converted into Fe
3+Cenotype CaSiO is arranged outward, in the product
3Generate.To the high calcium magnesium titanium slag after the reduction of above-mentioned material through X-ray diffractometer (XRD) analysis revealed, Ti
4+And Fe
3+All be reduced to initial valence state, and have cenotype geikielite structure to generate.Calucium Silicate powder and geikielite that CaO and MgO form respectively in the oxidation-reduction process all can be removed by hydrochloric acid leaching, can satisfy the requirement of existing chloridization process.
See also Fig. 2.One is high for 1500mm, internal diameter are the fluidized-bed reactor of the oxidation-reduction roasting high calcium magnesium titanium slag of 86mm, and it mainly is made of columniform cylinder material settling section 1, columniform cylinder material reaction section 2 and conical cylinder gas preheating section 3.
The top of one columniform cylinder material reaction section 2 is the hydraucone shape, connect a columniform cylinder material settling section 1 at the top of hydraucone cylinder, connect a conical cylinder gas preheating section 3 in the bottom of columniform cylinder material reaction section, in columniform cylinder material reaction section 2 the insides 3 endowels 12 are installed, and being equilateral triangle distributes, tubing string 12 is fixed on the anchor 11, and anchor is fixed on the fluidized-bed reactor main body; A plurality of band foraminous baffle plates 6 are fixed on this tubing string, and the aperture of band foraminous baffle plate 6 is 10mm, and is 150mm with the spacing between the foraminous baffle plate 6 in twos;
Have material opening for feed 4 on the wall on columniform cylinder material reaction section 2 and the top, junction of conical cylinder gas preheating section 3, in the bottom of 3 li of conical cylinder gas preheating sections gas distribution grid 8 is installed, the grid distributor below is gas feed 7;
On the cylinder wall below the hydraucone of columniform cylinder material reaction section 2, and be that position when columniform cylinder material reaction section 2 begins to become the hydraucone cylinder has material discharge port 9, have pneumatic outlet 10 at the top of columniform cylinder material settling section 1.
The high calcium magnesium titanium slag particle adds fluidized-bed reactor by screw feeder through opening for feed 4, and reaction back high calcium magnesium titanium slag is collected by hopper after discharge port 9 is discharged.In the oxidising process, service temperature is 700 ℃, and oxidizing gas is for containing O
2Air; In the reduction process, service temperature is 700 ℃, and reducing gas is H
2Gas.Fluidizing gas velocity is 0.087～0.164m/s, and feed rate is 5.0kg/h and 7.2kg/h.The mean residence time of high calcium magnesium titanium slag particle in fluidized-bed can be by fluidizing gas velocity and feed rate control, and mean residence time (t/h) is subjected to fluidizing gas velocity (U/ms
-1) and feed rate (F/kgh
-1) influence as shown in Table 1.
Table one fluidized gas speed and feed rate are to the influence of mean residence time
The contrast of table one data shows that fluidizing gas velocity increases, and mean residence time reduces; And feed rate increases, and mean residence time reduces.As seen, the mean residence time of high calcium magnesium titanium slag particle roasting in the fluidized-bed reactor of sandwich tape foraminous baffle plate can be by fluidizing gas velocity and the stable control of feed rate.
See also Fig. 2.One is high for 1800mm, internal diameter are the fluidized-bed reactor of the oxidation-reduction roasting high calcium magnesium titanium slag of 100mm, and it mainly is made of columniform cylinder material settling section 1, columniform cylinder material reaction section 2 and conical cylinder gas preheating section 3.
The top of one columniform cylinder material reaction section 2 is the hydraucone shape, connect a columniform cylinder material settling section 1 at the top of hydraucone cylinder, connect a conical cylinder gas preheating section 3 in the bottom of columniform cylinder material reaction section, in columniform cylinder material reaction section 2 the insides 3 endowels 12 are installed, and being equilateral triangle distributes, tubing string 12 is fixed on the anchor 11, and anchor is fixed on the fluidized-bed reactor main body; A plurality of band foraminous baffle plates 6 are fixed on this tubing string, and the aperture of band foraminous baffle plate 6 is 8.5mm, and is 100mm with the spacing between the foraminous baffle plate 6 in twos;
Have material opening for feed 4 on the wall on columniform cylinder material reaction section 2 and the top, junction of conical cylinder gas preheating section 3, in the bottom of 3 li of conical cylinder gas preheating sections gas distribution grid 8 is installed, the grid distributor below is gas feed 7;
On the cylinder wall below the hydraucone of columniform cylinder material reaction section 2, and be that position when columniform cylinder material reaction section 2 begins to become the hydraucone cylinder has material discharge port 9, have pneumatic outlet 10 at the top of columniform cylinder material settling section 1.
The high calcium magnesium titanium slag particle adds fluidized-bed reactor by screw feeder through opening for feed 4, and reaction back high calcium magnesium titanium slag is collected by hopper after discharge port 9 is discharged.In the oxidising process, service temperature is 1000 ℃, and oxidizing gas is for containing O
2Air; In the reduction process, service temperature is 900 ℃, and reducing gas is a CO gas.Fluidizing gas velocity is 0.104m/s～0.140m/s, and feed rate is 7.2kg/h.Different-grain diameter (d
p/ μ m) (t/h) is subjected to fluidizing gas velocity (U/ms the particulate residence time
-1) influence as shown in Table 2.
The table two different-grain diameter high calcium magnesium titanium slag particulate residence time is subjected to the influence of fluidizing gas velocity
Show that by the contrast of table two data for different fluidizing gas velocities, the increase of the high calcium magnesium titanium slag particulate residence time with its particle diameter prolongs.The reaction times of particle in fluidized-bed that particle diameter is little is shorter, and the big reaction times of particle in fluidized-bed of particle diameter is longer.Therefore, the fluidized-bed reactor of sandwich tape foraminous baffle plate can satisfy the demand of different-grain diameter titanium slag particle to the reaction times.
Claims (8)
1. the fluidized-bed reactor of an oxidation-reduction roasting high calcium magnesium titanium slag mainly is made of columniform cylinder material settling section, columniform cylinder material reaction section and conical cylinder gas preheating section; It is characterized in that:
The main body of one cylindrical stream fluidized bed reactor is columniform cylinder material reaction section, its top is the hydraucone shape, connect a columniform cylinder material settling section at the top of hydraucone cylinder, connect a conical cylinder gas preheating section in the bottom of columniform cylinder material reaction section;
Have the material opening for feed on the wall on the top, junction of columniform cylinder material reaction section and conical cylinder gas preheating section, the bottom in conical cylinder gas preheating section is equipped with gas distribution grid, and the grid distributor below is gas feed;
On the cylinder wall below the hydraucone of columniform cylinder material reaction section, have the material discharge port, have pneumatic outlet at the top of columniform cylinder material settling section;
In columniform cylinder material reaction section the inside more than one band foraminous baffle plate is installed.
2. fluidized-bed reactor according to claim 1 is characterized in that: described material discharge port is out the position when columniform cylinder material reaction section begins to become the hydraucone cylinder.
3. fluidized-bed reactor according to claim 1 is characterized in that: the spacing between the described band foraminous baffle plate is 1/5～2/1 with the internal diameter ratio of columniform cylinder material reaction section.
4. according to claim 1 or 3 described fluidized-bed reactors, it is characterized in that: the aperture of described band foraminous baffle plate is 1/50～1/8 with the internal diameter ratio of columniform cylinder material reaction section.
5. according to claim 1 or 3 described fluidized-bed reactors, it is characterized in that: described band foraminous baffle plate is fixed on the wall of columniform cylinder material reaction section by flange.
6. fluidized-bed reactor according to claim 4 is characterized in that: described band foraminous baffle plate is fixed on the wall of columniform cylinder material reaction section by flange.
7. according to claim 1 or 3 described fluidized-bed reactors, it is characterized in that: described band foraminous baffle plate is fixed on columniform cylinder material reaction Duan Zhongyi root or the tubing string more than, this tubing string is fixed on the anchor, and anchor is fixed on the fluidized-bed reactor main body.
8. fluidized-bed reactor according to claim 4, it is characterized in that: described band foraminous baffle plate is fixed on columniform cylinder material reaction Duan Zhongyi root or the tubing string more than, this tubing string is fixed on the anchor, and anchor is fixed on the fluidized-bed reactor main body.
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104099482A (en) * | 2014-07-22 | 2014-10-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Ilmenite concentrate fluidization reaction device and ilmenite concentrate fluidization reaction method |
| CN114752772A (en) * | 2022-03-16 | 2022-07-15 | 中南大学 | Method for preparing fluidized chlorination furnace charge by upgrading titanium slag |
-
2006
- 2006-08-03 CN CNA200610089104XA patent/CN101117665A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104099482A (en) * | 2014-07-22 | 2014-10-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Ilmenite concentrate fluidization reaction device and ilmenite concentrate fluidization reaction method |
| CN104099482B (en) * | 2014-07-22 | 2017-01-18 | 攀钢集团攀枝花钢铁研究院有限公司 | Ilmenite concentrate fluidization reaction device and ilmenite concentrate fluidization reaction method |
| CN114752772A (en) * | 2022-03-16 | 2022-07-15 | 中南大学 | Method for preparing fluidized chlorination furnace charge by upgrading titanium slag |
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